A method for continuously preparing two-dimensional materials by an automated CVD device

Abstract

The present invention belongs to the field of two-dimensional material preparation, and specifically relates to a method for continuously preparing two-dimensional materials by an automated CVD device. The automated CVD device for continuously preparing two-dimensional materials includes a reaction furnace, a boat assembly, a linear movement mechanism, a material storage device, and a loading and unloading mechanism. The method for continuously preparing two-dimensional materials by the automated CVD device provided by the present invention completely abandons the cumbersome processes of traditional manual double-sided sample loading and bolt fixation, and innovatively adopts single-sided automated sample injection. Through the coordinated cooperation of various designed parts, the effect of immediate sealing after the boat assembly injects the sample is successfully achieved, simplifying the process and greatly improving work efficiency. In addition, by designing the loading and unloading mechanism, the problem of sample loading failure caused by the uneven surface of the loading tray is effectively overcome, and self-adaptive deviation correction for loading and unloading is realized, thereby realizing the automated progress of the entire preparation process and finally achieving 24-hour continuous automated experiments.

Description

Technical Field

[0001] The present invention belongs to the field of two-dimensional material preparation, and particularly relates to a method for continuously preparing two-dimensional materials by an automated CVD device. Background Art

[0002] In the field of two-dimensional material preparation, chemical vapor deposition (CVD) is one of the most commonly used methods for growing high-quality two-dimensional materials. Commercial miniaturized CVD equipment can quickly and flexibly perform small-batch preparation in a laboratory environment, precisely control process parameters, and help researchers deeply understand the material growth mechanism. Currently, the equipment for preparing two-dimensional materials by chemical vapor deposition includes a workbench, on which a displacement platform is provided for moving the reaction furnace body. The loading operation of the reaction furnace body needs to be carried out on both sides respectively. The loading operation is to fix the sample rod on the corresponding flange with three bolts respectively. However, the above process steps are cumbersome, and the manual operation of fixing with bolts greatly increases the time cost. Secondly, when the existing sample rod places the substrate, it is difficult to level, which directly leads to poor parallelism of the experiment. In addition, there are many process parameters affecting material growth, including temperature, gas flow rate, precursor quality, etc. Manual sample feeding will bring deviations in the placement positions of the substrate and precursor in the furnace. The repeatability of manual experiments is poor, and the efficiency of manual experiments is low and high-throughput experiments cannot be achieved. Summary of the Invention

[0003] The technical problem to be solved by the present invention is: to provide a method for continuously preparing two-dimensional materials by an automated CVD device, which can perform unilateral automatic loading and maintain the airtightness of the furnace body and the horizontality of the sample, shorten the time cost. At the same time, the automated and continuous operation can reduce manual experimental errors, improve the accuracy and parallelism of the experiment, and achieve 24-hour high-throughput experiments.

[0004] The present invention provides a method for continuously preparing two-dimensional materials by an automated CVD device, using the automated CVD device, and the automated CVD device includes a reaction furnace, a boat assembly, a linear movement mechanism, a material storage device, and a loading and unloading mechanism;

[0005] The reaction furnace includes a furnace body for performing vapor deposition, and a material inlet and outlet is provided on one side of the furnace body;

[0006] The boat assembly includes a boat and a boat rod arranged in sequence. The boat rod is arranged at the output end of the linear movement mechanism, and the linear movement mechanism is used to drive the boat assembly to enter the furnace body through the material inlet and outlet; when the boat assembly enters the furnace body, the boat rod and the material inlet and outlet are sealed by a seal ring on the boat rod;

[0007] The material storage device stores the substrate for vapor deposition and the crucible for storing the precursor;

[0008] The loading and unloading mechanism is used to transfer the substrate and the crucible on the material storage device to the porcelain boat for vapor deposition, and is also used to transfer the substrate and the crucible on the porcelain boat that have completed vapor deposition to the next station;

[0009] The method for continuously preparing two-dimensional materials using the automated CVD device is to perform continuous automated experiments using the automated CVD device.

[0010] Furthermore, the reaction furnace comprises a furnace body and a furnace tube placed in the furnace body;

[0011] A connecting flange is provided at one end of the furnace body, an air inlet / outlet cavity is provided on the connecting flange, an air inlet / outlet hole I connected to the furnace body is provided at one end of the air inlet / outlet cavity, a material inlet and outlet is provided at the other end, and an air inlet / outlet hole II connected to the outside of the furnace body is also provided on the air inlet / outlet cavity;

[0012] The furnace tube is hollow inside and has two openings at both ends, one of which is connected to the outside of the furnace body for air inlet / outlet, and the other is abutted against the end of the air inlet / outlet hole I away from the air inlet / outlet cavity;

[0013] One end of the porcelain boat assembly can extend into the furnace tube through the material inlet and outlet and the air inlet / outlet hole I in sequence. There is an air inlet / outlet gap between the outer wall of the porcelain boat rod and the air inlet / outlet hole I. The porcelain boat rod and the material inlet and outlet are sealed by the sealing ring on the porcelain boat rod.

[0014] Furthermore, the inlet / outlet air cavity comprises a side enclosure I, a fixed side wall I arranged at one end of the side enclosure I, and a sliding side wall I slidably arranged in the side enclosure I;

[0015] The inlet / outlet hole I is arranged on the sliding side wall I;

[0016] The material inlet and outlet are arranged on the fixed side wall I;

[0017] The air inlet / outlet II is arranged on the side wall I or the fixed side wall I;

[0018] A spring I is also provided between the sliding side wall I and the fixed side wall I, and the spring I pushes the sliding side wall I to abut against the furnace tube opening.

[0019] Furthermore, a sealing cylinder is provided on one side of the material inlet and outlet extending toward the sliding side wall I;

[0020] At least one sealing ring is arranged on the outer wall of the porcelain boat rod. When the porcelain boat rod is matched with the reaction furnace, the sealing ring is sealed and matched with the inner wall of the sealing tube.

[0021] Furthermore, an air inlet / outlet flange is provided at the other end of the furnace body;

[0022] The air inlet / outlet flange includes a side enclosure II, a fixed side wall II provided at one end of the side enclosure II, and a sliding side wall II slidably provided within the side enclosure II;

[0023] An air inlet / outlet port I connecting to the outside of the furnace body is provided on the side enclosure II or the fixed side wall II;

[0024] An air inlet / outlet port II communicating with the inside of the furnace body is provided on the sliding side wall II;

[0025] A spring II is further provided between the sliding side wall II and the fixed side wall II, and the spring II pushes the sliding side wall II to abut against the opening of the furnace tube.

[0026] Furthermore, the furnace tube is a rectangular quartz glass tube.

[0027] Furthermore, a rectangular groove with an upward opening is provided on the ceramic boat, and two limiting grooves are provided on the bottom wall of the rectangular groove. One of the limiting grooves is used to place the substrate, and the other limiting groove is used to place the crucible;

[0028] The material storage device includes a substrate storage tray for storing a plurality of substrates and a crucible storage tray for storing a plurality of crucibles. The number of substrates and crucibles arranged on the substrate storage tray and the crucible storage tray is the same and corresponds in groups, and the distance between each group of substrates and crucibles is the same;

[0029] The loading and unloading mechanism includes two clamping heads. One of the clamping heads is used to clamp the substrate, and the other clamping head is used to clamp the crucible;

[0030] The distance between the two limiting grooves, the distance between each group of substrates and crucibles, and the distance between the two clamping heads are all kept the same.

[0031] Furthermore, the clamping head for clamping the substrate is a suction cup;

[0032] The clamping head for clamping the crucible is a clamping jaw.

[0033] Furthermore, the loading and unloading mechanism further includes a manipulator, and the clamping head is provided at the output end of the manipulator.

[0034] Furthermore, the process of the suction cup sucking the substrate includes the following steps:

[0035] If the signal given during the process of the suction cup grasping the substrate is positive, the manipulator raises a certain distance, which is process one; read the signal of the suction cup again, which is process two;

[0036] Case 1: If the signal of Process 1 is positive and the signal of Process 2 is also positive, the manipulator will transfer the substrate and the crucible to the ceramic boat.

[0037] Case 2: If the signal of Process 1 is positive and the signal of Process 2 is negative, the manipulator will descend and repeat the suction cup grasping operation. When grasping, the horizontal height of the suction cup rises by 0.1 mm relative to the previous time, and the operation will be executed in a loop until it meets Case 1.

[0038] Case 3: If the signal of Process 1 is negative and the signal of Process 2 is negative, the manipulator will descend and repeat the suction cup grasping operation. When grasping, the horizontal height of the suction cup drops by 0.1 mm relative to the previous time, and continuous adjustment will be made until it meets Case 1.

[0039] The beneficial effects of the present invention are as follows. The method for continuously preparing two-dimensional materials by the automated CVD device provided by the present invention completely abandons the cumbersome processes of traditional manual double-sided sample loading and bolt fixation. It innovatively adopts single-sided automated sample injection. Through the coordinated cooperation of multiple designed parts, the effect of immediately sealing after the ceramic boat assembly is injected is successfully achieved, simplifying the process and greatly improving work efficiency. In addition, by designing the loading and unloading mechanism, the problem of sample loading failure caused by the uneven surface of the loading tray is effectively overcome, realizing self-adaptive deviation correction for loading and unloading, and then realizing the automation of the entire preparation process, and finally achieving 24-hour continuous automated experiments. Brief Description of the Drawings

[0040] Attached Figure 1 is a schematic structural diagram of the first angle of the present invention;

[0041] Attached Figure 2 is a schematic structural diagram of the second angle of the present invention;

[0042] Attached Figure 3 is for the present invention attached Figure 2 is a partial enlarged view of part A in the figure;

[0043] Attached Figure 4 is a schematic structural diagram of the ceramic boat assembly of the present invention located outside the reaction furnace;

[0044] Attached Figure 5 is a front cross-sectional view of the reaction furnace of the present invention;

[0045] Attached Figure 6 is a schematic structural diagram of the ceramic boat assembly of the present invention;

[0046] Attached Figure 7 is a schematic structural diagram of the ceramic boat assembly of the present invention located inside the reaction furnace;

[0047] Attached Figure 8 is a front cross-sectional view of the ceramic boat assembly of the present invention located inside the reaction furnace;

[0048] Attached Figure 9is an attachment Figure 8 The partial enlarged view at position B in

[0049] attachment Figure 10 is an attachment Figure 8 The partial enlarged view at position C in

[0050] attachment Figure 11 is an attachment Figure 8 The partial enlarged view at position D in

[0051] In the figure, 1 - reaction furnace; 11 - furnace body; 12 - furnace tube; 13 - connecting flange; 131 - inlet / outlet cavity; 1311 - side enclosure Ⅰ; 1312 - fixed side wall Ⅰ; 1313 - sliding side wall Ⅰ; 1314 - spring Ⅰ; 132 - inlet / outlet hole Ⅰ; 133 - material inlet / outlet; 134 - inlet / outlet hole Ⅱ; 135 - inlet / outlet interval; 136 - sealing cylinder; 14 - outlet / inlet flange; 141 - side enclosure Ⅱ; 142 - fixed side wall Ⅱ; 143 - sliding side wall Ⅱ; 144 - outlet / inlet port Ⅰ; 145 - outlet / inlet port Ⅱ; 146 - spring Ⅱ; 2 - boat assembly; 21 - boat; 211 - rectangular groove; 212 - limiting groove; 22 - boat rod; 221 - sealing ring; 3 - linear movement mechanism; 4 - material storage device; 41 - substrate storage tray; 42 - crucible storage tray; 5 - loading / unloading mechanism; 51 - manipulator; 52 - suction cup; 53 - clamping jaw; 6 - workbench. Detailed implementation manners

[0052] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention.

[0053] It should be noted that all the directional indications (such as up, down, left, right, front, back...) in the embodiments of the present invention are only used to explain the relative position relationship and movement conditions between components in a specific posture. If the specific posture changes, the directional indications will also change accordingly.

[0054] In addition, the descriptions such as "first" and "second" in the present invention are only for descriptive purposes, and cannot be understood as indicating or implying their relative importance or implicitly indicating the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one of such features. In the description of the present invention, "a plurality" means at least two, for example, two, three, etc., unless otherwise specifically defined.

[0055] In the present invention, unless otherwise clearly specified and defined, terms such as "fixing" and "connecting" shall be understood in a broad sense. For example, "fixing" can be a fixed connection, a detachable connection, or integrated; "connecting" can be a mechanical connection, an electrical connection, a physical connection, or a wireless communication connection; it can be directly connected or indirectly connected through an intermediate medium, and can be the communication inside two components or the interaction relationship between two components, unless otherwise clearly defined. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0056] In addition, the technical solutions between various embodiments of the present invention can be combined with each other, but it must be based on the ability of those of ordinary skill in the art to implement. When the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such a combination of technical solutions does not exist and is not within the protection scope required by the present invention.

[0057] As shown in the Figure 1 - attached Figure 11 accompanying drawings, the present invention provides a method for continuously preparing two-dimensional materials using an automated CVD device. The automated CVD device includes a reaction furnace 1, a boat assembly 2, a linear movement mechanism 3, a material storage device 4, and a loading and unloading mechanism 5. Preferably, the automated CVD device further includes a workbench 6, and the reaction furnace 1, the boat assembly 2, the linear movement mechanism 3, the material storage device 4, and the loading and unloading mechanism 5 are all arranged on the workbench 6 to improve the integrity of the device;

[0058] The reaction furnace 1 includes a furnace body 11 for chemical vapor deposition, where the furnace body 11 is used to provide the required temperature, atmosphere, and other environmental requirements for the substrate and the precursor. A material inlet and outlet 133 is arranged on one side of the furnace body 11, and the material inlet and outlet 133 is used for the boat assembly 2 loaded with the substrate and the precursor to enter and exit the furnace body 11;

[0059] The boat assembly 2 includes a boat 21 and a boat rod 22 arranged in sequence. The boat rod 22 is arranged at the output end of the linear movement mechanism 3, used to drive the boat 21 to move and achieve the airtightness requirement between the boat assembly 2 and the furnace body 11. The boat 21 is used to carry the substrate and the crucible. The linear movement mechanism 3 is used to drive the boat assembly 2 to enter the furnace body 11 through the material inlet and outlet 133; when the boat assembly 2 enters the furnace body 11, the boat rod 22 and the material inlet and outlet 133 are sealed through the sealing ring 221 on the boat rod 22, that is, the boat rod 22 seals the material inlet and outlet 133, realizing the operation of sealing during sample introduction, greatly improving the efficiency of loading and unloading, and thus improving the overall working efficiency;

[0060] The material storage device 4 is used to store the substrates and crucibles to be subjected to chemical vapor deposition, wherein the crucibles are used to hold the precursors;

[0061] The loading and unloading mechanism 5 is used to transfer the substrates and crucibles on the material storage device 4 to the ceramic boat 21 for chemical vapor deposition, and is also used to transfer the substrates and crucibles that have completed vapor deposition on the ceramic boat 21 to the next station, where the next station can be the material storage device 4 or another storage device for storing the prepared two-dimensional materials;

[0062] The loading and unloading mechanism 5 is used to transfer the substrates and crucibles to realize the automatic operation of the system, and thus can realize continuous operation for 24 hours and ensure the working quality.

[0063] The method for continuously preparing two-dimensional materials by the automatic CVD device is to use the automatic CVD device to conduct continuous automatic experiments.

[0064] The method for continuously preparing two-dimensional materials by the automatic CVD device provided by the present invention completely abandons the cumbersome processes of traditional manual double-sided sample loading and bolt fixation, innovatively adopts single-sided automatic sample injection, and through the coordinated cooperation of designing a variety of parts, successfully realizes the effect of immediately sealing after the ceramic boat assembly 2 is sampled, simplifies the process and greatly improves the working efficiency. In addition, by designing the loading and unloading mechanism 5, the problem of sample loading failure caused by the uneven surface of the loading tray is effectively overcome, the loading and unloading self-adaptive deviation correction is realized, and then the automatic operation of the entire preparation process is realized, and finally the continuous automatic experiment for 24 hours is realized.

[0065] In one embodiment, the reaction furnace 1 includes a furnace body 11 and a furnace tube 12 placed in the furnace body 11. The furnace body 11 is hollow inside and provided with a furnace cavity, and the furnace tube 12 is arranged in the furnace cavity;

[0066] A connecting flange 13 is provided at one end of the furnace body 11. The connecting flange 13 can be detachably arranged on the side wall of the furnace body 11, or can be integrally arranged on the side wall of the furnace body 11. An inlet / outlet air cavity 131 is provided on the connecting flange 13. An inlet / outlet air hole I 132 communicating with the furnace body 11 is provided at one end of the inlet / outlet air cavity 131, and a material inlet / outlet 133 is provided at the other end. An inlet / outlet air hole II 134 communicating with the outside of the furnace body 11 is also provided on the inlet / outlet air cavity 131. When the inlet / outlet air cavity 131 is used to inlet air into the furnace tube 12, the inlet / outlet air hole II 134 is used to transport gas to the inlet / outlet air cavity 131. The gas passes through the inlet / outlet air cavity 131 and then rectifies and exits. The air inlet / outlet hole Ⅰ132 enters the furnace tube 12, which can ensure the flow field stabilization effect of the air flow; when the air inlet / outlet cavity 131 is used to receive and discharge the gas in the furnace tube 12, the gas in the furnace tube 12 enters the air inlet / outlet cavity 131 from the air inlet / outlet hole Ⅰ132, and then is discharged from the air inlet / outlet hole Ⅱ134, wherein the air inlet / outlet hole Ⅰ132 and the material inlet / outlet 133 are arranged relatively, and the porcelain boat assembly 2 can enter the furnace tube 12 in the furnace cavity by passing through the material inlet / outlet 133, the air inlet / outlet cavity 131 and the air inlet / outlet hole Ⅰ132 in sequence, so that the connecting flange 13 is used for both the air inlet / outlet of the furnace tube 12 and the porcelain boat assembly 2 can enter and exit the furnace tube 12;

[0067] The furnace tube 12 is hollow inside and has two openings at both ends, one of which is open to the outside of the furnace body 11 for air inlet / outlet, and the end of the furnace tube 12 and the side of the connecting flange 13 form a gas flow channel in the furnace tube 12, and the gas can flow from the end to the connecting flange 13, during which the atmosphere requirements in the furnace tube 12 are ensured, or flow from one end of the connecting flange 13 to the end, during which the atmosphere requirements in the furnace tube 12 are ensured, and the other end of the furnace tube 12 is open against the end of the inlet / outlet hole I 132 away from the inlet / outlet cavity 131, thereby achieving direct communication between the furnace tube 12 and the inlet / outlet cavity 131;

[0068] One end of the porcelain boat assembly 2 can extend into the furnace tube 12 through the material inlet and outlet 133, the inlet / outlet air cavity 131 and the inlet / outlet hole I132 in sequence. An inlet / outlet air gap 135 is provided between the outer wall of the porcelain boat rod 22 and the inlet / outlet air hole I132. The inlet / outlet air gap 135 is used to realize gas circulation between the inlet / outlet air cavity 131 and the furnace tube 12. The outer wall of the porcelain boat rod 22 and the material inlet and outlet 133 are sealed and matched through the sealing ring 221 on the porcelain boat rod 22. Therefore, when the porcelain boat assembly 2 enters the furnace tube 12, the material inlet and outlet 133 can be blocked to prevent air leakage from the material inlet and outlet 133.

[0069] In this embodiment, the loading and unloading of the substrate and the precursor can be achieved through one side of the reaction furnace 1. Compared with the two-way feeding and discharging in the prior art (CN215887222U - an apparatus for gas-phase preparation of two-dimensional materials), the loading and unloading efficiency can be greatly improved, and only the movable sealing cooperation between the outer wall of the boat rod 22 and the material inlet and outlet 133 is required, which can reduce the overall sealing difficulty. The structural design of the connecting flange 13 and the furnace tube 12 not only facilitates meeting the atmosphere requirements inside the furnace tube 12 but also facilitates the feeding and discharging of the boat assembly 2.

[0070] In one embodiment, the inlet / outlet gas chamber 131 includes a side enclosure I 1311, a fixed side wall I 1312 provided at one end of the side enclosure I 1311, and a sliding side wall I 1313 slidably disposed within the side enclosure I 1311. Preferably, the side enclosure I 1311 is of a cylindrical structure, and both the fixed side wall I 1312 and the sliding side wall I 1313 are of circular plate structures, so that the inlet / outlet gas chamber 131 is a cylindrical cavity. Preferably, the sliding side wall I 1313 is made of high-temperature resistant fluororubber, which can not only ensure the sealing effect but also ensure the service life.

[0071] The inlet / outlet gas hole I 132 is provided on the sliding side wall I 1313.

[0072] The material inlet and outlet 133 is provided on the fixed side wall I 1312.

[0073] The inlet / outlet gas hole II 134 is provided on the side enclosure I 1311 or the fixed side wall I 1312. Preferably, the inlet / outlet gas hole II 134 is provided on the side enclosure I 1311.

[0074] A spring I 1314 is further provided between the sliding side wall I 1313 and the fixed side wall I 1312, and the spring I 1314 pushes the sliding side wall I 1313 to abut against the opening of the furnace tube 12. In this embodiment, by providing the spring I 1314 and the sliding side wall I 1313, the sliding side wall I 1313 is a movable structure, so that the sliding side wall I 1313 can be closely attached to the opening of the furnace tube 12, ensuring the seal between the opening of the furnace tube 12 and the sliding side wall I 1313 and preventing gas from flowing into the furnace cavity. In this embodiment, the sliding side wall I 1313 can serve as a fixing structure for fixing this end of the furnace tube 12, thus facilitating the fixed installation of this end of the furnace tube 12.

[0075] The design of the connecting flange 13 in this embodiment, together with the internal spring I 1314 and the sliding side wall I 1313 (the spring I 1314 and the sliding side wall I 1313 not only play a sealing role but also buffer the furnace tube 12 so as not to damage the furnace tube 12), the cooperation between the sliding side wall I 1313 and the furnace tube 12, and the interlocking cooperation between the boat rod 22 and the connecting flange 13 form an airtight system, realizing the operation of good sealing upon sample injection.

[0076] In one embodiment, a sealing cylinder 136 is provided extending towards one side of the sliding side wall I 1313 at the material inlet and outlet 133.

[0077] At least one sealing ring 221 is provided on the outer wall of the boat rod 22. When the boat rod 22 cooperates with the reaction furnace 1, the sealing ring 221 is in sealing cooperation with the inner wall of the sealing cylinder 136. Preferably, a plurality of sealing rings 221 are provided on the outer wall of the boat rod 22 to improve the sealing effect. In this embodiment, the outer wall of the sealing cylinder 136 can also be used as the guiding column of the spring I 1314. Preferably, the sealing ring 221 is made of high-temperature resistant fluororubber.

[0078] In one embodiment, an air inlet / outlet flange 14 is provided at the other end of the furnace body 11.

[0079] The air inlet / outlet flange 14 includes a side enclosure II 141, a fixed side wall II 142 provided at one end of the side enclosure II 141, and a sliding side wall II 143 slidably disposed within the side enclosure II 141. Preferably, the side enclosure II 141 is of a cylindrical structure, and both the fixed side wall II 142 and the sliding side wall II 143 are of a circular plate structure. Preferably, the sliding side wall II 143 is made of high-temperature resistant fluororubber, which can not only ensure the sealing effect but also ensure the service life.

[0080] An air inlet / outlet port I 144 connecting to the outside of the furnace body 11 is provided on the side enclosure II 141 or the fixed side wall II 142. Preferably, the air inlet / outlet port I 144 is provided at the end face of the fixed side wall II 142.

[0081] An air inlet / outlet port II 145 communicating with the inside of the furnace body 11 is provided on the sliding side wall II 143.

[0082] A spring II 146 is further provided between the sliding side wall II 143 and the fixed side wall II 142. The spring II 146 pushes the sliding side wall II 143 to abut against the opening of the furnace tube 12, and the opening of the furnace tube 12 is in communication with the air inlet / outlet port II 145, wherein the diameter of the air inlet / outlet port II 145 is smaller than the opening of the furnace tube 12. In this embodiment, by providing the spring II 146 and the sliding side wall II 143, the sliding side wall II 143 is a movable structure, and thus the sliding side wall II 143 can be closely attached to the opening on this side of the furnace tube 12 to ensure the sealing between the opening on this side of the furnace tube 12 and the sliding side wall II 143, preventing gas from flowing into the furnace cavity. In this embodiment, the sliding side wall I 1313 can be used as the fixing structure for fixing this end of the furnace tube 12, thus facilitating the fixed installation of this end of the furnace tube 12.

[0083] In one embodiment, the furnace tube 12 is a rectangular quartz glass tube. By using a rectangular quartz glass tube, compared with the furnace tube in the prior art (CN221141863U - A furnace tube suitable for visual CVD and with strong airtight performance) which has a rectangular structure in the middle and cylindrical structures at both ends, it is possible to avoid the turbulence of the gas generated when the area inside the tube changes, which affects the experimental results. At the same time, it is also convenient for the processing of the furnace tube 12.

[0084] In one embodiment, a rectangular groove 211 with an upward opening is provided on the boat 21. This rectangular groove 211 is used to accommodate the substrate and the crucible containing the precursor. The side walls of the rectangular groove 211 can prevent the lateral displacement of the substrate and avoid the tipping of the crucible. At the same time, the boat 21 can also keep the substrate and the crucible on it always horizontal. Two limiting grooves 212 are provided on the bottom wall of the rectangular groove 211. One of the limiting grooves 212 is used to place the substrate, and the other limiting groove 212 is used to place the crucible; the limiting grooves 212 can be used to accommodate the crucible or the substrate, thereby preventing the crucible or the substrate from displacing along the length direction of the rectangular groove 211, and further ensuring the relative distance between the two.

[0085] The material storage device 4 includes a substrate storage tray 41 for storing a plurality of substrates and a crucible storage tray 42 for storing a plurality of crucibles. The number of substrates and crucibles arranged on the substrate storage tray 41 and the crucible storage tray 42 is the same and they are grouped correspondingly. The spacing between each group of substrates and crucibles is the same.

[0086] The loading and unloading mechanism 5 includes two clamping heads. One of the clamping heads is used to clamp the substrate, and the other clamping head is used to clamp the crucible.

[0087] The spacing between the two limiting grooves 212, the spacing between each group of substrates and crucibles, and the spacing between the two clamping heads are all the same; at this time, when the loading and unloading mechanism 5 drives the two clamping heads to move, the crucible and the substrate on the material storage device 4 can be clamped at the same time, and the crucible and the substrate can be placed in the limiting grooves 212 at the same time, which can greatly improve the extraction efficiency of the crucible and the substrate and realize one-step sample loading, with simple and fast operation.

[0088] In one embodiment, the gripper for gripping the substrate is a suction cup 52; the gripper for gripping the crucible is a jaw 53. The loading and unloading mechanism 5 further includes a robot 51, and the gripper is disposed at the output end of the robot 51. In this embodiment, the output end of the robot 51 is provided with a suction cup 52 for sucking the substrate and a jaw 53 for gripping the crucible containing the precursor. The robot 51 grabs the substrate and the crucible from the material storage device 4 and places them on the ceramic boat 21. After the two-dimensional material is prepared, the substrate and the crucible are taken out from the ceramic boat 21 and placed on the material storage device 4, and then new substrate and crucible are taken from the material storage device 4, and so on in a cycle to realize the continuous preparation of the two-dimensional material by automated chemical vapor deposition.

[0089] Specifically, the loading and unloading mechanism 5 controls the movement of the robot 51 through the feedback of the suction cup 52 to ensure that the suction cup 52 stably sucks the substrate. The logic is as follows: if the signal given during the process of the suction cup 52 gripping the substrate is positive, the robot 51 rises a certain distance, which is process one; the signal of the suction cup 52 is read again, which is process two; Case one: if the signal of process one is positive and the signal of process two is also positive, the robot 51 transfers the substrate and the crucible to the ceramic boat 21; Case two: if the signal of process one is positive and the signal of process two is negative, the robot 51 descends and repeats the gripping operation of the suction cup 52, and the horizontal height of the suction cup 52 during gripping rises by 0.1 mm relative to the previous time, and the cycle is executed until case one is met; Case three: if the signal of process one is negative and the signal of process two is negative, the robot 51 descends and repeats the gripping operation of the suction cup 52, and the horizontal height of the suction cup 52 during gripping drops by 0.1 mm relative to the previous time, and the continuous adjustment is made until case one is met. This logic can solve the problem of gripping failure caused by the slight unevenness on the surface of the material storage device 4 through the dual detection mechanism (process one + process two) combined with dynamic displacement compensation.

[0090] In one embodiment, the linear movement mechanism 3 is a linear drive mechanism, which has the characteristics of precise control and long moving stroke, and can ensure that the ceramic boat assembly 2 accurately enters the reaction furnace 1.

[0091] The above is only this embodiment and does not impose any limitation on the present invention. Any person skilled in the art can make many possible changes, modifications or equivalents to the technical solution of the present invention by using the technical content disclosed above without departing from the scope of the technical solution of the present invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention shall fall within the scope of protection of the technical solution of the present invention.

Claims

1. A method for continuously preparing two-dimensional materials using an automated CVD device, characterized in that: Continuously preparing two-dimensional materials using an automated CVD device, the automated CVD device comprising a reaction furnace (1), a porcelain boat assembly (2), a linear motion mechanism (3), a material storage device (4), and a loading and unloading mechanism (5); The reaction furnace (1) comprises a furnace body (11) for performing vapor deposition, and a material inlet and outlet (133) is provided on one side of the furnace body (11); The porcelain boat assembly (2) comprises a porcelain boat (21) and a porcelain boat rod (22) which are arranged in sequence, the porcelain boat rod (22) being arranged at the output end of the linear motion mechanism (3), and the linear motion mechanism (3) being used to drive the porcelain boat assembly (2) to enter the furnace body (11) through the material inlet and outlet (133); when the porcelain boat assembly (2) enters the furnace body (11), the porcelain boat rod (22) cooperates with the material inlet and outlet (133) to complete sealing through the sealing ring (221) on the porcelain boat rod (22); The material storage device (4) stores substrates for vapor deposition and crucibles for storing precursors; The loading and unloading mechanism (5) is used to transfer the substrate and the crucible on the material storage device (4) to the porcelain boat (21) for vapor deposition, and the loading and unloading mechanism (5) is also used to transfer the substrate and the crucible on which the vapor deposition has been completed on the porcelain boat (21) to the next workstation; The method for continuously preparing two-dimensional materials by the automated CVD device is to use the automated CVD device to perform continuous automated experiments; The reaction furnace (1) comprises a furnace body (11) and a furnace tube (12) placed in the furnace body (11); A connecting flange (13) is provided at one end of the furnace body (11), an air inlet / outlet cavity (131) is provided on the connecting flange (13), an air inlet / outlet hole I (132) communicating with the furnace body (11) is provided at one end of the air inlet / outlet cavity (131), a material inlet / outlet hole (133) is provided at the other end, and an air inlet / outlet hole II (134) communicating with the outside of the furnace body (11) is also provided on the air inlet / outlet cavity (131); The furnace tube (12) is hollow inside and has two openings at both ends, one of which is connected to the outside of the furnace body (11) for air inlet / outlet, and the other is abutted against an end of the air inlet / outlet hole I (132) away from the air inlet / outlet cavity (131); One end of the porcelain boat assembly (2) can extend into the furnace tube (12) through the material inlet and outlet (133) and the air inlet / outlet hole I (132) in sequence, and an air inlet / outlet gap (135) is provided between the outer wall of the porcelain boat rod (22) and the air inlet / outlet hole I (132), and the porcelain boat rod (22) and the material inlet and outlet (133) are sealed by cooperation through a sealing ring (221) on the porcelain boat rod (22); The air inlet / outlet cavity (131) comprises a side enclosure I (1311), a fixed side wall I (1312) arranged at one end of the side enclosure I (1311), and a sliding side wall I (1313) slidably arranged in the side enclosure I (1311); The air inlet / outlet hole I (132) is arranged on the sliding side wall I (1313); The material inlet and outlet (133) is arranged on the fixed side wall I (1312); The air inlet / outlet hole II (134) is arranged on the side wall I (1311) or the fixed side wall I (1312); A spring I (1314) is also provided between the sliding side wall I (1313) and the fixed side wall I (1312), and the spring I (1314) pushes the sliding side wall I (1313) to abut against the opening of the furnace tube (12).

2. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 1, characterized in that: A sealing cylinder (136) is provided on one side of the material inlet and outlet (133) extending toward the sliding side wall I (1313); At least one sealing ring (221) is provided on the outer wall of the porcelain boat rod (22); when the porcelain boat rod (22) is matched with the reaction furnace (1), the sealing ring (221) is sealed and matched with the inner wall of the sealing cylinder (136).

3. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 1, characterized in that: The other end of the furnace body (11) is provided with an air outlet / inlet flange (14); The air outlet / inlet flange (14) comprises a side enclosure II (141), a fixed side wall II (142) arranged at one end of the side enclosure II (141), and a sliding side wall II (143) slidably arranged in the side enclosure II (141); The side enclosure II (141) or the fixed side wall II (142) is provided with an air inlet / outlet I (144) connected to the outside of the furnace body (11); The sliding side wall II (143) is provided with an air inlet / outlet II (145) communicating with the furnace body (11); A spring II (146) is also provided between the sliding side wall II (143) and the fixed side wall II (142), and the spring II (146) pushes the sliding side wall II (143) to abut against the opening of the furnace tube (12).

4. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 2, characterized in that: The furnace tube (12) is a rectangular quartz glass tube.

5. The method for continuously preparing two-dimensional materials using an automated CVD device according to any one of claims 1 to 4, characterized in that: The porcelain boat (21) is provided with an upwardly open rectangular groove (211), and the bottom wall of the rectangular groove (211) is provided with two limiting grooves (212), wherein one of the limiting grooves (212) is used to place a substrate, and the other limiting groove (212) is used to place a crucible; The distance between the two limiting grooves (212), the distance between each group of substrates and the crucible, and the distance between the two clamping heads are all kept consistent; The material storage device (4) comprises a substrate storage tray (41) for storing a plurality of substrates and a crucible storage tray (42) for storing a plurality of crucibles, the number of substrates and crucibles arranged on the substrate storage tray (41) and the crucible storage tray (42) being the same and being arranged in corresponding groups, and the spacing between the substrates and crucibles in each group being the same; The loading and unloading mechanism (5) comprises two clamping heads, one of which is used to clamp the substrate, and the other of which is used to clamp the crucible.

6. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 5, characterized in that: The clamping head for clamping the substrate is a suction cup (52); The clamping head for clamping the crucible is a clamping claw (53).

7. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 6, characterized in that: The loading and unloading mechanism (5) further comprises a robot (51), and the clamping head is arranged at the output end of the robot (51).

8. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 7, characterized in that: The suction cup (52) sucks the substrate, comprising the following steps: If the signal given by the suction cup (52) during the process of grabbing the substrate is positive, the robot arm (51) is raised for a certain distance, which is process one; the signal of the suction cup (52) is read again, which is process two; Case 1: If the signal of process 1 is positive and the signal of process 2 is also positive, the robot (51) transfers the substrate and the crucible to the porcelain boat (21); Case 2: If the signal of process 1 is positive and the signal of process 2 is negative, the manipulator (51) descends and repeats the gripping operation of the suction cup (52). During the gripping operation, the horizontal height of the suction cup (52) rises by 0.1 mm relative to the last time. The cycle is executed until case 1 is met; Case 3: If the signal of process one is negative and the signal of process two is negative, the robot arm (51) descends and repeats the gripping operation of the suction cup (52). During the gripping, the horizontal height of the suction cup (52) decreases by 0.1 mm relative to the last time, and the adjustment is continued until it meets case one.

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