A sealing device for the transfer of easily oxidized materials and its application method

Abstract

This invention discloses a sealing device for transferring easily oxidizable materials and its usage method. The sealing device includes a ball valve, a rubber gasket, a KF clamp, a vacuum interface, and an ampoule. The ball valve and the vacuum interface are sealed together by the KF clamp and the rubber gasket, forming a detachable transitional sealing structure. In use, the uniformly mixed raw materials are first loaded into the ampoule inside a glove box, and after placing the tube stopper, the vacuum interface and ball valve are installed sequentially, keeping the valve closed. After transferring the material outside the glove box, a vacuum sealing machine is connected through the outer interface of the ball valve. The vacuum is evacuated to a predetermined vacuum level and kept closed. Finally, the ampoule is sealed using a flame torch to complete the encapsulation. This invention achieves continuous atmospheric isolation of the material during the transfer process through a detachable sealing structure, effectively preventing easily oxidizable materials from contacting air, and providing reliable encapsulation and operational assurance for the synthesis of materials with low air stability.

Description

Technical Field

[0001] This invention relates to the field of inorganic material preparation technology, specifically to a sealing device for the transfer of easily oxidized materials and its usage method. Background Technology

[0002] In the solid-phase synthesis of inorganic functional materials, especially those prone to oxidation or with low air stability, the transfer and encapsulation of raw materials and intermediates are crucial steps determining the quality of the synthesis. Traditional synthesis methods typically involve mixing the raw materials in a glove box, directly transferring them to an open or simply sealed container, transferring them outside the glove box, and then vacuum-sealing them. This method presents high exposure risks, is cumbersome and uncontrollable, and lacks reliable encapsulation. In recent years, with the urgent demand for high-purity, specific-valence functional materials in fields such as new energy materials, superconducting materials, and thermoelectric materials, higher requirements have been placed on the protective atmosphere control of synthesis technologies.

[0003] To address this, various improved technologies have been developed, such as using glove boxes equipped with transition chambers and employing fully enclosed material transfer systems. However, these systems are often complex and costly, or still have exposure windows at the connection between continuous vacuuming and final sealing. Furthermore, for material systems such as sulfides and selenides, which are extremely sensitive to oxygen and water and may be corrosive, traditional transfer devices containing numerous rubber / plastic seals are prone to aging, contamination, or seal failure during long-term use, making it difficult to meet the experimental requirements of high vacuum and high cleanliness. Especially in the process of high-quality single-crystal growth or high-purity material preparation, even higher requirements are placed on the vacuum and cleanliness of the system before encapsulation. Therefore, there is an urgent need for a material transfer and encapsulation device that can achieve high sealing levels, high vacuum compatibility, and good corrosion resistance. Summary of the Invention

[0004] Purpose of the invention: The purpose of this invention is to provide a sealing device for the transfer of easily oxidized materials and its method of use, aiming to solve the oxidation problem caused by transfer exposure during the synthesis of materials with low air stability.

[0005] Technical Solution: The sealing device for transferring easily oxidized materials according to the present invention includes a ball valve, a rubber gasket, a vacuum interface, a KF clamp, and an ampoule. The ball valve has KF interfaces at both ends. The vacuum interface includes a KF adapter, a rubber ring, a metal gasket, and an ampoule adapter. The ampoule includes a quartz tube and a quartz tube stopper. The ball valve and the vacuum interface are sealed together by the rubber gasket and the KF clamp, forming a detachable transition seal structure. This structure is compatible with standard vacuum systems and molecular pump systems, enabling a high-vacuum pumping environment and reducing the risk of contamination from organic sealing materials.

[0006] Furthermore, the KF interfaces on both sides of the ball valve are standard KF16 interfaces.

[0007] Furthermore, the rubber gasket consists of an outer rubber layer and an inner metal ring, the outer diameter of which matches the inner diameter of the KF interface.

[0008] Furthermore, the dimensions of the ampoule adapter are matched to the dimensions of the ampoule opening.

[0009] Furthermore, the dimensions of the KF clamp are matched with the KF interface of the ball valve and the KF interface of the vacuum interface.

[0010] Furthermore, the quartz tube has a length of 190-210mm, an outer diameter of 20-22mm, an inner diameter of 16-18mm, and a waist-narrowing structure at a distance of 90-100mm from one end, with an outer diameter of 16-18mm and an inner diameter of 12-14mm at the waist-narrowing section.

[0011] Furthermore, the quartz tube has a length of 200mm, an outer diameter of 20mm, an inner diameter of 17mm, and a waist-narrowing structure at a distance of 95mm from one end, with an outer diameter of 16mm and an inner diameter of 13mm at the waist-narrowing point.

[0012] Furthermore, the quartz tube plug has a height of 15-20 mm and a diameter of 14-16 mm.

[0013] Furthermore, the quartz tube plug has a height of 15mm and a diameter of 15mm.

[0014] The method for transferring easily oxidizable material raw materials using a sealing device according to the present invention includes the following steps: S1. Inside the glove box, the evenly mixed raw materials are loaded into the quartz tube, and a tube plug is placed; S2. Place the rubber ring and metal washer on the mouth of the ampoule, and insert the ampoule adapter from below the ampoule. Then tighten the ampoule adapter and KF adapter. S3. Connect the ball valve to the vacuum port tightly using rubber gaskets and KF clamps, and keep the ball valve in the closed position; S4. Transfer the assembled device outside the glove box, connect the vacuum sealing machine through the KF interface on the outside of the ball valve, evacuate to the predetermined pressure, open the ball valve, and evacuate to the predetermined pressure again; S5. Use a flame torch to seal the ampoules, completing the sealing process.

[0015] Beneficial effects: Compared with the prior art, the present invention has the following significant advantages: (1) The present invention adopts an all-metal vacuum connection structure with ball valve and KF interface as the core, which significantly reduces the risk of volatilization and pollution of organic materials while ensuring structural strength. Compared with traditional rubber plug or vacuum grease sealing method, it has higher cleanliness and long-term stability.

[0016] (2) The device can be directly connected to standard vacuum systems and molecular pump systems to achieve excellent sealing performance, and the ultimate vacuum of the system can reach 10. -6 The Torr-level significantly improves the degassing capacity of the raw material system before sealing, providing conditions for the synthesis of high-purity materials.

[0017] (3) Since the sealing structure is mainly composed of metal parts, it avoids the failure problem of organic sealing materials in corrosive environments, and is particularly suitable for material systems with corrosive or highly reactive properties such as sulfides, selenides, and phosphides.

[0018] (4) By constructing a reliable transition sealing structure between the glove box and the vacuum sealing system, the sample loading, vacuuming and sealing process can be completed under conditions of no air exposure throughout the process, thereby significantly reducing the pollution of oxygen and water to the reaction system, which is beneficial to obtaining high-purity powder and high-quality single crystal materials.

[0019] (5) The device has a compact structure and small size. All components use standardized interfaces, which can quickly connect with the glove box outlet and vacuum system to achieve seamless connection between operation inside the box and sealing outside the box. Its overall size has been optimized to fully adapt to the internal space requirements of common glove box transition compartments, which facilitates safe transfer.

[0020] (6) The device is lightweight and has a straight axis. The overall weight is controlled to meet the upper limit of the load of mainstream vacuum tube sealing machines. Its straight cylindrical shape design ensures the stability when rotating dynamically on the tube sealing machine's rotating frame, without shaking or eccentricity, thereby ensuring the airtightness, consistency and operational safety of the sealing process.

[0021] This device, with its simple and ingenious design and readily available materials, achieves low-cost, high-efficiency end-to-end atmosphere protection. It not only simplifies the operation process but also significantly improves encapsulation success rate and material preservation quality. It can be widely used in the preparation of high-end materials sensitive to atmosphere, such as high-purity powders, battery materials, organometallic compounds, and single-crystal synthesis, and has significant practical application value. Attached Figure Description

[0022] Figure 1 This is a disassembly diagram of the sealing device in Embodiment 1 of the present invention.

[0023] Figure 2 This is a schematic diagram of the connection of the sealing device in Embodiment 1 of the present invention.

[0024] Figure 3 This is a schematic diagram of the ball valve in Embodiment 1 of the present invention.

[0025] Figure 4 This is a schematic diagram of the rubber gasket in Embodiment 1 of the present invention.

[0026] Figure 5 This is a schematic diagram of the quartz tube and quartz tube plug used to provide a vacuum environment in Embodiment 1 of the present invention.

[0027] Figure 6 This is a flowchart of the vacuum sealing operation in Embodiment 1 of the present invention.

[0028] Figure 7 This is an optical photograph of the BaTiS3 crystal synthesized in Example 1 of this invention.

[0029] Figure 8 This is a comparison chart of the synthesized BaTiS3 in Example 1 of the present invention and the theoretically calculated XRD data.

[0030] Figure 9 This is an optical photograph of the BaTiS3 crystal synthesized in Example 2 of this invention.

[0031] Figure label: 1-Ball valve; 11-Valve; 12-KF interface; 121-KF disc; 122-Interface inner diameter; 2-Rubber washer; 21-Rubber layer; 22-Metal ring; 3-Vacuum connector; 31-KF adapter; 32-Rubber ring; 33-Metal washer; 34-Ampoule adapter; 4-KF clamps; 5-Ampoule; 51-Quartz tube; 52-Quartz tube stopper. Detailed Implementation

[0032] The technical solution of the present invention will be further described below with reference to the accompanying drawings and embodiments.

[0033] Example 1

[0034] like Figure 1 As shown, the present invention provides a sealing device for transferring easily oxidized materials (such as inorganic compounds sensitive to air and moisture), including a ball valve 1, a rubber gasket 2, a vacuum interface 3, a KF clamp 4, and an ampoule 5. The two ends of the ball valve 1 are KF interfaces 12; the vacuum interface 3 includes a KF adapter 31, a rubber ring 32, a metal gasket 33, and an ampoule adapter 34; the ampoule 5 includes a quartz tube 51 and a quartz tube plug 52; the ball valve 1 and the vacuum interface 3 are sealed together by the rubber gasket 2 and the KF clamp 4, forming a detachable transition sealing structure.

[0035] like Figure 3 The KF ports 12 on both sides of the ball valve 1 shown are standard KF16 ports, ensuring compatibility with other sealing devices.

[0036] like Figure 4 The rubber gasket 2 shown consists of an outer rubber layer 21 and an inner metal ring 22. The outer diameter of the metal ring 22 matches the inner diameter 121 of the KF interface 12 to ensure sealing and enhance the mechanical strength and positioning accuracy of the gasket.

[0037] One end of the KF adapter 31 of the vacuum interface 3 is a KF interface 311, which is fastened to the KF interface 12 of the ball valve by a KF clamp 4; the other end is an ampoule adapter 34, the size of which matches the outer diameter of the ampoule 5. The ampoule adapter 34 and the KF adapter 31 are connected by a threaded connection, and a rubber ring 32 and a metal washer 33 are arranged between them in sequence, which can achieve axial compression and sealing of the ampoule mouth during tightening.

[0038] The dimensions of the KF clamp 4 are matched with the KF interface 12 of the ball valve and the KF interface 311 of the KF adapter 31. The clamp's locking force presses the rubber gasket 2 firmly between the mating end faces, forming a detachable, highly sealed connection.

[0039] like Figure 5 The quartz tube 51 shown has dimensions of 200 mm in length, 20 mm in outer diameter, and 17 mm in inner diameter. It has a waist-shaped structure 95 mm from one end, with an outer diameter of 16 mm and an inner diameter of 13 mm at the waist. This structure has excellent chemical inertness and thermal stability, and facilitates the isolation of the raw material area during the loading process, which is convenient for subsequent sealing operations.

[0040] The quartz tube stopper 52 has a height of 15mm and a diameter of 15mm. The appropriate stopper size ensures that the stopper can be smoothly inserted into the ampoule without falling into the raw material area, and can be directly fused with the quartz tube during the sealing process to form a vacuum-tight seal.

[0041] Taking the preparation of BaTiS3 crystals by chemical vapor transport as an example, according to Figure 6 The procedure shown begins by accurately weighing 0.1694 g of barium sulfide (BaS), 0.1120 g of titanium disulfide (TiS2), and 0.0256 g of elemental sulfur (S) in a glove box. The excess elemental sulfur is used to compensate for any sulfur loss during synthesis. The mixture is then ground in a mortar for 30 minutes to obtain a uniform precursor powder.

[0042] Load the well-mixed precursor powder into Figure 5 After inserting the quartz tube 51 as shown, insert the tube plug 52 into the quartz tube 51. Then... Figure 2The rubber ring 32 and metal washer 33 shown are placed on the mouth of the ampoule 5, and the ampoule adapter 34 is inserted from below the ampoule 5. The ampoule adapter 34 is then screwed tightly onto the KF adapter 31. Figure 2 As shown.

[0043] Connect ball valve 1 to vacuum port 3 via Figure 4 The rubber gasket 2 and KF clamp 4 shown are tightly connected, keeping the ball valve 11 in the closed state, as follows. Figure 3 As shown.

[0044] After transferring the sealing device outside the glove box, the ball valve 1 is tightly connected to the vacuum sealing machine using KF clamp 4 and rubber gasket 2, and the vacuum level is evacuated to the predetermined level. Then, the ball valve 11 is opened, and the vacuum level is evacuated again to the predetermined level, sealing the quartz tube 51 and the tube plug 52 to form a complete vacuum seal structure. Subsequently, the quartz tube containing the raw material is placed in a tube furnace for heat treatment.

[0045] To confirm the sealing performance of the sealing device, the prepared BaTiS3 material was removed. An optical photograph of the synthesized BaTiS3 crystal is shown below. Figure 7 As shown.

[0046] The remaining powder in the tube was ground and XRD analysis was performed, then compared with the standard peak positions. Figure 8 The peak positions corresponded accurately and without significant shift, confirming that the material was not oxidized.

[0047] This embodiment demonstrates that the sealing device and transfer packaging method provided by this invention can effectively isolate air and prevent easily oxidized materials from oxidizing during the critical process of transferring them from the glove box to the vacuum sealing machine. XRD characterization confirmed the high quality and oxidation-free state of the obtained material in terms of phase purity, verifying the reliability and effectiveness of this method in the synthesis of protective atmosphere-sensitive materials.

[0048] Example 2

[0049] In this embodiment, a quartz tube with a length of 190 mm, an outer diameter of 20 mm, and an inner diameter of 16 mm is used, as well as a tube plug with a height of 20 mm and a diameter of 14 mm. The remaining process parameters are set in accordance with those in Example 1, including the raw material ratio, packaging method, protective atmosphere, and heat treatment regime.

[0050] The quartz tube containing the raw material was sealed and the reaction was carried out under the set heat treatment conditions. After the reaction was completed, the sample was removed, and BaTiS3 crystals were obtained. An optical photograph of the obtained crystal is shown below. Figure 9 As shown.

[0051] As can be seen from the figure, the prepared BaTiS3 crystals have smooth surfaces and uniform morphology, and no obvious oxidation phenomenon was observed, indicating that this method can achieve stable synthesis of air-sensitive sulfide materials under conditions of effective isolation from the external environment.

[0052] Example 3

[0053] In this embodiment, a quartz tube with a length of 210 mm, an outer diameter of 22 mm, and an inner diameter of 18 mm is used, as well as a tube plug with a height of 20 mm and a diameter of 16 mm. The remaining process parameters are set in accordance with those in Example 1, including the raw material ratio, packaging method, protective atmosphere, and heat treatment regime.

[0054] The upper limit of the quartz tube length is set at 210 mm because when the quartz tube length exceeds this size, the overall length of the sealing assembly will exceed the space limit of the glove box transition compartment, which is not conducive to loading and transfer operations, thus affecting the actual feasibility of the device.

[0055] The quartz tube containing the raw material was sealed and subjected to heat treatment. After the reaction was completed, the sample was removed. The obtained BaTiS3 material was characterized by XRD, and its diffraction peaks were in good agreement with the theoretical calculation results, indicating that the prepared sample has the expected crystal structure.

[0056] The above results demonstrate that the apparatus and process described in this embodiment can achieve stable synthesis of air-sensitive sulfide materials under conditions of effective isolation from external air, exhibiting good practicality and reliability.

Claims

1. A sealing device for the transfer of an oxidizable material, characterized in that, The utility model relates to a kind of vacuum sealing device, including ball valve (1), rubber washer (2), vacuum interface (3), KF clamp (4) and ampoule (5);The both ends of ball valve (1) are KF interface (12);Vacuum interface (3) includes KF adapter (31), rubber ring (32), metal washer (33) and ampoule adapter (34);Ampoule (5) includes quartz tube (51) and quartz tube plug (52);Ball valve (1) and vacuum interface (3) are sealedly connected by the rubber washer (2) and KF clamp (4) between, and constitute detachable transition sealing structure.

2. The sealing device according to claim 1, characterized in that The KF interface (12) of the ball valve (1) is a standard KF interface.

3. The sealing device of claim 1, wherein The rubber washer (2) is composed of an outer rubber layer (21) and an inner metal ring (22), and the outer diameter of the metal ring (22) matches the inner diameter of the KF interface (122).

4. The sealing device of claim 1, wherein The size of the ampoule adapter (34) matches the size of the ampoule (5).

5. The sealing device of claim 1, wherein, The size of the KF clamp (4) matches the KF disc (121) of the ball valve (1) and the KF disc (311) of the vacuum interface (3).

6. The sealing device of claim 1, wherein, The quartz tube (51) has a size of 190-210 mm in length, 20-22 mm in outer diameter, and 16-18 mm in inner diameter, and a tapered structure is provided at a distance of 90-100 mm from one end, with an outer diameter of 16-18 mm and an inner diameter of 12-14 mm.

7. The sealing device of claim 6, wherein The quartz tube (51) has a size of 200 mm in length, 20 mm in outer diameter, and 17 mm in inner diameter, and a tapered structure is provided at a distance of 95 mm from one end, with an outer diameter of 16 mm and an inner diameter of 13 mm.

8. The sealing device of claim 1, wherein, The quartz tube plug (52) has a size of 15-20 mm in height and 14-16 mm in diameter.

9. The sealing device of claim 8, wherein, The quartz tube plug (52) has a size of 15 mm in height and 15 mm in diameter.

10. A method for transferring a raw material of an oxidizable material using the sealing device according to claim 1, characterized by, The utility model includes the following steps: S1. In the glove box, the mixed raw materials are loaded into the quartz tube (51), and the tube plug (52) is placed; S2. The rubber ring (32) and the metal washer (33) are placed on the ampoule (5), and the ampoule adapter (34) is inserted from the bottom of the ampoule (5), and then the ampoule adapter (34) is screwed with the KF adapter (31); S3. The ball valve (1) and the vacuum interface (3) are tightly connected through the rubber washer (2) and the KF clamp (4), and the ball valve (1) is kept in the closed state; S4. The assembled device is transferred out of the glove box, and the vacuum sealing machine is connected through the KF interface (12) on the outside of the ball valve (1), and the valve (11) is opened after vacuuming to the predetermined pressure, and vacuuming to the predetermined pressure again; S5. The ampoule (5) is sealed by using a spray gun flame, and the packaging is completed.

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