Gas-phase transportation synthesis growth preparation combined device of vacuum atmosphere purification box

By designing a gas phase transport, synthesis and growth preparation combination device of vacuum air atmosphere purification box, the raw material loading, pipe sealing and gas phase transport and growth preparation of quartz crucible are directly completed in the glove box, solving the problems of pollution and performance degradation during material transfer. Efficient material synthesis and preparation are achieved.

CN222499462UActive Publication Date: 2025-02-18WUHAN SHIWEI OPTOELECTRONIC TECH CO LTD
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Patent Information

Application Number
CN202420444892.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-03-07
Publication Date
2025-02-18
Estimated Expiration
2034-03-07

AI Technical Summary

Technical Problem

During the process of material synthesis and growth, the existing technology requires frequent use of glove boxes to transfer materials, crucibles and raw materials, resulting in the material being easily contaminated and oxidized by moisture impurities in the atmosphere, degraded or failed in performance, and the overall preparation process is cumbersome, which wastes time .

Method used

Design a vacuum air-phase transportation, synthetic growth preparation device for gas-phase transportation, synthesis and growth preparation, including glove box, quartz tube, high-temperature growth furnace, magnetic coupled linear rotary inlet and sealing connector to realize the movement and sealing of quartz crucible in quartz tube Tube operation, and the raw material loading, pipe sealing, gas phase transport and growth preparation are completed directly in the glove box.

Benefits of technology

The one-time preparation of material synthesis, growth and transfer is realized, which reduces the cumbersome intermediate steps of material transfer, saves overall operating time, improves the preparation efficiency of material devices, and avoids material pollution and performance degradation.

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Abstract

The utility model discloses a vacuum atmosphere purification box gas phase transportation synthesis growth preparation combined device which comprises a glove box and a high-temperature growth furnace internally provided with a quartz tube, and one end of the quartz tube is communicated with the interior of the glove box through a connection transition bin; the magnetic coupling type linear rotation importer is arranged at the other end of the quartz tube, is connected with a quartz crucible through a sealing connecting piece, and drives the quartz crucible to move in the quartz tube; a tube sealing assembly is arranged in the glove box and is used for performing high-temperature plasma sintering and heat sealing on one end of the quartz crucible, and the tube sealing assembly is matched with a sealing connecting piece and is used for controlling the internal sealing of the quartz crucible; and growth preparation raw materials are filled in the quartz crucible. According to the utility model, raw material loading, tube sealing and transferring of the quartz crucible can be directly completed in the glove box for gas-phase transport growth preparation, crystal material obtaining and transferring and material device preparation operation, so that a large number of tedious intermediate steps are omitted, and the material device preparation efficiency is improved.
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Description

Technical Field

[0001] The utility model relates to the technical field of material synthesis growth preparation, in particular to a vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device. Background Art

[0002] Vapor transport is a common method for the synthetic growth and preparation of advanced materials. Generally, the growth raw materials are decomposed into gaseous components and then transported from one end of the container to the other end driven by the axial temperature gradient inside the closed crucible tube container, thereby synthesizing and growing the corresponding crystal materials. It is an important method for the synthetic growth and preparation of single crystal materials and material purification. It has the advantages of being direct, simple, effective, low-cost, easy to operate and control. The vacuum atmosphere purification glove box is a protective operating box. The interior of the box can provide an inert atmosphere environment without water and oxygen to prevent the material from being oxidized, contaminated, deteriorated and performance degraded, so as to facilitate the subsequent material device preparation and process treatment of the grown material.

[0003] Therefore, in the process of synthesizing growth materials using the existing raw materials using the vapor phase transport method, it is generally necessary to first seal the quartz tube containing the raw materials using a vacuum tube sealing machine, and then transfer the sealed quartz tube to a high-temperature furnace to complete the growth, and then move the grown crystal material to a glove box for subsequent material device preparation processes. During the multi-step transfer process, the material is extremely susceptible to contamination and oxidation by moisture, impurities, and materials in the atmosphere, resulting in performance degradation or failure.

[0004] In summary, in the overall preparation process of material devices, the transition chamber of the glove box needs to be frequently used to transfer materials, crucibles, and raw materials. The intermediate steps are cumbersome, which greatly wastes the overall preparation time of the material devices.

[0005] To this end, the present application specifically proposes a vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device to solve the above-mentioned technical problems, and the above-mentioned content is only used to assist in understanding the technical solution of the present application, and does not represent an admission that the above-mentioned content is the closest prior art. Utility Model Content

[0006] The main purpose of the utility model is to provide a vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device which can directly perform sealed tube transfer operations in a glove box and conveniently and quickly move the crucible containing raw materials to a specified position in a growth furnace for material gas phase transport synthesis growth operations.

[0007] In order to solve the above technical problems, the utility model provides a vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device, comprising:

[0008] A glove box and a high-temperature growth furnace with a quartz tube disposed therein, wherein one end of the quartz tube is connected to the interior of the glove box via a connecting transition chamber;

[0009] A magnetically coupled linear rotary introducer is arranged at the other end of the quartz tube and is connected to a quartz crucible via a sealing connector, driving the quartz crucible to move inside the quartz tube;

[0010] The glove box is provided with a sealing tube assembly for sealing one end of a quartz crucible by high-temperature plasma sintering, and the sealing tube assembly cooperates with a sealing connector to seal the quartz crucible;

[0011] The quartz crucible is filled with growth preparation raw materials. When the interior of the quartz crucible is sealed, the high-temperature growth furnace is used to control the gas phase transmission operation of the material inside the quartz crucible.

[0012] Furthermore, the glove box is also provided with a material transition chamber for transferring materials inside the glove box, a vacuum pump for vacuumizing the inside of the glove box, and an atmosphere access component for filling a protective atmosphere into the glove box.

[0013] Furthermore, a support frame is provided on one side of the high temperature growth furnace for supporting and installing the magnetically coupled linear rotary introducer.

[0014] Furthermore, the sealing connector includes a sliding plate sliding along the length direction of the quartz tube, a mounting block arranged on the sliding plate, and a sleeve arranged on the mounting block and sealed at one end, and the other end of the sleeve is open for mounting the quartz crucible.

[0015] Furthermore, a driving rod is provided on the magnetic coupling type linear rotary introducer, and the driving rod is connected to the sliding plate, and is used for the magnetic coupling type linear rotary introducer to drive the sliding plate to move in the quartz tube.

[0016] Furthermore, the sleeve rotates on the mounting block, and the sealing connector further comprises a limiting rotation ring arranged on the outer side of the sleeve, and the limiting rotation ring is used for limiting the rotation of the sleeve on the mounting block.

[0017] Furthermore, a threaded portion is provided on the outer side of one end of the quartz crucible, so as to enable the quartz crucible to be threadably rotatably installed in the sleeve.

[0018] Furthermore, the sealing tube assembly includes a high-temperature plasma sintering device for one end of the high-temperature sealing tube quartz crucible and a switch handle for electrically driving the high-temperature plasma sintering device to operate.

[0019] Furthermore, the sealing tube assembly also includes a sliding bracket arranged inside the glove box and a sliding block slidably arranged on the sliding bracket, the high-temperature plasma sintering device and the switch handle are both arranged on the sliding block, and the switch handle is used to manually drive the sliding block to move on the sliding bracket.

[0020] The beneficial effects of the utility model are embodied in:

[0021] 1. The utility model arranges a sealing tube assembly in a glove box, and arranges a quartz tube for connecting to the interior of the glove box body in a high-temperature growth furnace, and uses a magnetically coupled linear rotary introducer to control the movement of the quartz crucible in the quartz tube. It is convenient to directly complete the raw material loading, tube sealing, and transfer of the quartz crucible to the quartz tube for gas phase transport growth preparation, crystal material acquisition, and further material device preparation operations in the glove box, thereby realizing the one-time preparation of material synthesis growth and transfer, eliminating the tedious intermediate steps of material transfer, greatly saving the overall operation time, and improving the material device preparation efficiency.

[0022] 2. The utility model provides a sealing connector at the end of the driving rod of the magnetically coupled linear rotary introducer, and uses the sealing connector to install and seal one end of the quartz crucible, so that the raw materials in the quartz crucible can be quickly moved to the sealing tube assembly for sealing operation after loading, and moved to the high-temperature growth furnace for gas phase transport and growth of the materials. This not only facilitates the movement of materials to different positions in the quartz tube for operation, but also facilitates the rapid loading and unloading of materials during the growth preparation process in the quartz crucible, and is easy to use. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The drawings constituting part of the present application are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation on the present invention. In the drawings:

[0024] Figure 1 It is an overall three-dimensional view of the utility model;

[0025] Figure 2 It is a three-dimensional cross-sectional schematic diagram of the utility model quartz crucible in a sliding state inside a quartz tube;

[0026] Figure 3 It is a three-dimensional cross-sectional schematic diagram of the movable connection structure of the quartz crucible of the utility model;

[0027] Figure 4 for Figure 3 The enlarged view of point A in the middle;

[0028] Figure 5 The utility model is a schematic diagram of the structural connection of the sealing tube assembly in the glove box.

[0029] In the figure:

[0030] 1. Glove box; 11. Material transition chamber; 12. Vacuum pump; 13. Atmosphere access assembly; 14. Sealing tube assembly; 141. Sliding bracket; 142. Sliding block; 143. Switch handle; 144. High-temperature plasma sintering device; 2. Connecting transition chamber; 3. Quartz tube; 4. High-temperature growth furnace; 5. Support frame; 6. Magnetic coupling linear rotary introducer; 61. Driving rod; 7. Quartz crucible; 71. Threaded part; 8. Sealing connector; 81. Sliding plate; 82. Mounting block; 83. Sleeve; 84. Limit rotating ring. DETAILED DESCRIPTION

[0031] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. In the absence of conflict, the embodiments in this application and the features in the embodiments can be combined with each other. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the utility model.

[0032] In the embodiment, see Figures 1 to 5 .

[0033] like Figure 1 and Figure 2 As shown, the utility model provides a vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device, comprising:

[0034] A glove box 1 and a high-temperature growth furnace 4 with a quartz tube 3 disposed therein, one end of the quartz tube 3 being connected to the interior of the glove box 1 via a transition chamber 2;

[0035] A magnetically coupled linear rotary introducer 6 is provided at the other end of the quartz tube 3 and is connected to a quartz crucible 7 through a sealing connector 8, driving the quartz crucible 7 to move inside the quartz tube 3. At this time, a support frame 5 is provided on one side of the high-temperature growth furnace 4 for supporting and installing the magnetically coupled linear rotary introducer 6;

[0036] A sealing tube assembly 14 is provided in the glove box 1 . The sealing tube assembly 14 is used to seal one end of the quartz crucible 7 by high-temperature plasma sintering. The sealing tube assembly 14 cooperates with the sealing connector 8 to seal the inside of the quartz crucible 7 .

[0037] Therefore, further, the quartz crucible 7 is filled with growth preparation raw materials, and the interior of the quartz crucible 7 is in a sealed state. The high-temperature growth furnace 4 is used to control the gas phase transmission operation of the material inside the quartz crucible 7 .

[0038] In a specific implementation, by setting the sealing tube assembly 14 in the glove box 1, and setting a quartz tube 3 for connecting to the interior of the main body of the glove box 1 in the high-temperature growth furnace 4, and using a magnetically coupled linear rotary introducer 6 to control the movement of the quartz crucible 7 in the quartz tube 3, it is convenient to directly complete the raw material loading, tube sealing, and transfer of the quartz crucible 7 to the quartz tube 3 for gas phase transport growth preparation, crystal material acquisition, and further material device preparation operations in the glove box 1, thereby realizing a one-time preparation of material synthesis growth and transfer, eliminating the tedious intermediate steps of material transfer, greatly saving the overall operation time, and improving the material device preparation efficiency.

[0039] It should be noted that the magnetically coupled linear rotary introducer 6 here is a prior art, and the existing patent (a high-precision all-metal sealed vacuum linear drive with application number CN201922423040.8) can be used as a replacement structure, and it will not be described in detail here.

[0040] Specifically, the glove box 1 is also provided with a material transition chamber 11 for transferring materials inside the glove box 1 , a vacuum pump 12 for vacuumizing the inside of the glove box 1 , and an atmosphere access component 13 for filling a protective atmosphere into the glove box 1 .

[0041] Among them, the material transition chamber 11 is used to transfer the gas phase synthetic growth material to the glove box 1, the vacuum pump 12 is also a prior art, used to vacuum the inside of the glove box 1, and the atmosphere access component 13 is composed of an atmosphere interface set on the glove box 1 and a valve on the atmosphere interface, which is used to connect the corresponding atmosphere box to fill a certain amount of protective atmosphere into the glove box 1.

[0042] In a specific embodiment, if Figure 3 and Figure 4 As shown, the sealing connector 8 is composed of a sliding plate 81 that slides along the length direction of the quartz tube 3, a mounting block 82 disposed on the sliding plate 81, and a sleeve 83 that is disposed on the mounting block 82 and sealed at one end, wherein the other end of the sleeve 83 is open for mounting the quartz crucible 7.

[0043] Specifically, during the connection process of the quartz crucible 7 , a threaded portion 71 is disposed on the outer side of one end of the quartz crucible 7 , so as to enable the quartz crucible 7 to be threadably installed in the sleeve 83 .

[0044] Therefore, when the quartz crucible 7 is threadedly installed at the opening at the other end of the sleeve 83, it can also ensure that one end of the quartz crucible 7 is closed.

[0045] Furthermore, the sleeve 83 can also be rotated on the mounting block 82 , and at this time the sealing connector 8 also includes a limiting rotation ring 84 arranged on the outside of the sleeve 83 , and the limiting rotation ring 84 is used to limit the rotation of the sleeve 83 on the mounting block 82 .

[0046] It should be further explained here that a driving rod 61 is provided on the magnetic coupling linear rotary introducer 6 , and the driving rod 61 is connected to the sliding plate 81 , so that the magnetic coupling linear rotary introducer 6 drives the sliding plate 81 to move in the quartz tube 3 .

[0047] Therefore, by setting a sealing connector 8 at the end of the driving rod 61 of the magnetically coupled linear rotary introducer 6, and using the sealing connector 8 to install and seal one end of the quartz crucible 7, it is convenient to quickly move the raw materials in the quartz crucible 7 to the sealing tube assembly 14 for sealing operation after loading, and move it to the high-temperature growth furnace 4 for gas phase transport and growth of the materials. This not only facilitates the movement of materials to different positions in the quartz tube 3 for operation, but also facilitates the rapid loading and unloading of materials during the growth and preparation process in the quartz crucible 7, and is convenient for use.

[0048] In a specific embodiment, if Figure 5 As shown, the sealing tube assembly 14 includes a high-temperature plasma sintering device 144 for sealing one end of the high-temperature quartz crucible 7 and a switch handle 143 for electrically driving the high-temperature plasma sintering device 144 to operate.

[0049] When the magnetically coupled linear rotary introducer 6 uses the driving rod 61 to move the quartz crucible 7 to the end, the end of the quartz crucible 7 away from the sleeve 83 extends into the glove box 1 and is located at the sintering position of the high-temperature plasma sintering device 144. At this time, the switch handle 143 can be used to electrically drive the high-temperature plasma sintering device 144 to operate, completing the tube sealing operation at one end of the quartz crucible 7, thereby ensuring that the interior of the quartz crucible 7 is closed at this time.

[0050] It should be noted that, after the other end of the sealed tube end of the quartz crucible 7 is removed from the sleeve 83 , the other end of the sealed tube end of the quartz crucible 7 can be used for taking out and unloading the growth preparation material.

[0051] Furthermore, the sealing tube assembly 14 further includes a sliding bracket 141 disposed inside the glove box 1 and a sliding block 142 slidably disposed on the sliding bracket 141 .

[0052] During use, the high-temperature plasma sintering device 144 and the switch handle 143 are both arranged on the sliding block 142, and the switch handle 143 is used to manually drive the sliding block 142 to move on the sliding bracket 141, which can ensure that the quartz crucible 7 of different lengths can be sealed at one end after being installed using the sealing connector 8.

[0053] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

[0054] In addition, it should be noted that if the embodiments of the present invention involve directional indications (such as up, down, left, right, front, back...), the directional indications are only used to explain the relative position relationship, movement status, etc. between the components in a certain specific posture. If the specific posture changes, the directional indications will also change accordingly.

[0055] In addition, if there are descriptions involving "first", "second", etc. in the embodiments of the utility model, the descriptions of "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In addition, the meaning of "and / or" appearing in the full text includes three parallel schemes. Taking "A and / or B" as an example, it includes scheme A, or scheme B, or schemes that A and B meet at the same time. In addition, in the embodiments of the utility model, "multiple" refers to more than two. In addition, the technical solutions between the various embodiments can be combined with each other, but it must be based on the ability of ordinary technicians in this field to implement. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the utility model.

Claims

1. A vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device, characterized in that: include: A glove box (1) and a high-temperature growth furnace (4) having a quartz tube (3) disposed therein, wherein one end of the quartz tube (3) is connected to the interior of the glove box (1) via a transition chamber (2); A magnetically coupled linear rotary introducer (6) is arranged at the other end of the quartz tube (3) and is connected to the quartz crucible (7) via a sealing connector (8), driving the quartz crucible (7) to move inside the quartz tube (3); The glove box (1) is provided with a sealing tube assembly (14) for sealing one end of a quartz crucible (7) by high-temperature plasma sintering, and the sealing tube assembly (14) cooperates with a sealing connector (8) to seal the quartz crucible (7); The quartz crucible (7) contains growth preparation raw materials. When the interior of the quartz crucible (7) is sealed, the high-temperature growth furnace (4) is used to control the gas phase transmission operation of the material inside the quartz crucible (7).

2. The vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device as claimed in claim 1, characterized in that: The glove box (1) is also provided with a material transition chamber (11) for transferring materials inside the glove box (1), a vacuum pump (12) for vacuum treatment inside the glove box (1), and an atmosphere access component (13) for filling a protective atmosphere into the glove box (1).

3. The vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device as claimed in claim 1, characterized in that: A support frame (5) is provided on one side of the high temperature growth furnace (4) for supporting and installing a magnetic coupling type linear rotary introducer (6).

4. The vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device as claimed in claim 1, characterized in that: The sealing connection member (8) comprises a sliding plate (81) sliding along the length direction of the quartz tube (3), a mounting block (82) arranged on the sliding plate (81), and a sleeve (83) arranged on the mounting block (82) and sealed at one end, the other end of the sleeve (83) being open for mounting the quartz crucible (7); The magnetic coupling type linear rotary introducer (6) is provided with a driving rod (61), and the driving rod (61) is connected to a sliding plate (81) and is used for the magnetic coupling type linear rotary introducer (6) to drive the sliding plate (81) to move in the quartz tube (3).

5. The vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device as claimed in claim 4, characterized in that: The sleeve (83) rotates on the mounting block (82), and the sealing connector (8) further comprises a limiting rotation ring (84) arranged on the outside of the sleeve (83), wherein the limiting rotation ring (84) is used for limiting the rotation of the sleeve (83) on the mounting block (82).

6. The vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device as claimed in claim 4, characterized in that: A threaded portion (71) is provided on the outer side of one end of the quartz crucible (7) for threadably rotating the quartz crucible (7) in the sleeve (83).

7. The vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device as claimed in claim 1, characterized in that: The sealing tube assembly (14) comprises a high-temperature plasma sintering device (144) for one end of a high-temperature sealing tube quartz crucible (7) and a switch handle (143) for electrically driving the high-temperature plasma sintering device (144) to operate.

8. The vacuum atmosphere purification box gas phase transport synthesis growth preparation combined device as claimed in claim 7, characterized in that: The sealing tube assembly (14) further comprises a sliding bracket (141) arranged inside the glove box (1) and a sliding block (142) slidably arranged on the sliding bracket (141); The high-temperature plasma sintering device (144) and the switch handle (143) are both arranged on the sliding block (142), and the switch handle (143) is used to manually drive the sliding block (142) to move on the sliding bracket (141).

Citation Information

Patent Citations

  • High-precision all-metal sealing vacuum linear driver

    CN211693401U