Method for continuously preparing two-dimensional material by automatic CVD (Chemical Vapor Deposition) device

Abstract

The invention belongs to the field of two-dimensional material preparation, and particularly relates to a method for continuously preparing a two-dimensional material through an automatic CVD device, and the device for continuously preparing the two-dimensional material through the automatic CVD device comprises a reaction furnace, a porcelain boat assembly, a linear moving mechanism, a material storage device and a feeding and discharging mechanism; according to the method for continuously preparing the two-dimensional material through the automatic CVD device, the tedious processes of traditional manual double-side sample loading and bolt fixing are thoroughly abandoned, single-side automatic sample injection is innovatively adopted, and the effect of immediate sealing after sample injection of the porcelain boat assembly is successfully achieved through cooperation of various parts; the process is simplified; and the working efficiency is greatly improved. In addition, by designing the feeding and discharging mechanism, the problem of sample feeding failure caused by the factor that the surface of a feeding disc is uneven is effectively solved, feeding and discharging self-adaptive deviation correction is achieved, the whole preparation process is automatically carried out, and finally 24-hour continuous automatic experiments are achieved.

Description

Technical Field

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

[0002] In the field of two-dimensional material preparation, chemical vapor deposition (CVD) is currently one of the most commonly used methods for growing high-quality two-dimensional materials. Commercial miniaturized CVD equipment can quickly and flexibly prepare small batches in a laboratory environment, accurately control process parameters, and help researchers gain a deep understanding of the material growth mechanism. At present, 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 performed on both sides of the reaction furnace body, and the loading operation is to fix the sample rod on the corresponding flange with three bolts. However, the above process steps are cumbersome to operate, and the manual operation of fixing with bolts greatly increases the time cost. Secondly, the existing sample rod is difficult to level when placing the substrate, which directly leads to poor parallelism of the experiment. In addition, there are many process parameters that affect material growth, including temperature, gas flow rate, precursor quality, etc. Manual sample delivery will cause deviations in the placement positions of the substrate and the precursor in the furnace, the repeatability of manual experiments is poor, and the low efficiency of manual experiments cannot achieve high-throughput experiments. 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 using an automated CVD device, which can perform single-sided automatic sampling while maintaining the air tightness of the furnace and the horizontality of the sample, thereby shortening the time cost. At the same time, automated and continuous operations can reduce manual experimental errors, improve the accuracy and parallelism of the experiment, and realize 24-hour high-throughput experiments.

[0004] The present invention provides a method for continuously preparing two-dimensional materials using an automated CVD device, wherein the automated CVD device includes a reaction furnace, a porcelain boat assembly, a linear motion mechanism, a material storage device, and a loading and unloading mechanism; The reaction furnace comprises a furnace body for performing vapor deposition, and a material inlet and outlet are arranged on one side of the furnace body; The porcelain boat assembly comprises a porcelain boat and a porcelain boat rod which are arranged in sequence, wherein the porcelain boat rod is arranged at the output end of the linear motion mechanism, and the linear motion mechanism is used to drive the porcelain boat assembly to enter the furnace body through the material inlet and outlet; when the porcelain boat assembly enters the furnace body, the porcelain boat rod cooperates with the material inlet and outlet through the sealing ring on the porcelain boat rod to complete the sealing; The material storage device stores substrates for vapor deposition and crucibles for storing precursors; 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; The method for continuously preparing two-dimensional materials using the automated CVD device is to perform continuous automated experiments using the automated CVD device.

[0005] Furthermore, the reaction furnace comprises a furnace body and a furnace tube placed in the furnace body; 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; 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; 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.

[0006] 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; The inlet / outlet hole I is arranged on the sliding side wall I; The material inlet and outlet are arranged on the fixed side wall I; The air inlet / outlet II is arranged on the side wall I or the fixed side wall I; 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.

[0007] Furthermore, a sealing cylinder is provided on one side of the material inlet and outlet extending toward the sliding side wall I; 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.

[0008] Furthermore, an air outlet / inlet flange is provided at the other end of the furnace body; The outlet / inlet flange includes a side enclosure II, a fixed side wall II arranged at one end of the side enclosure II, and a sliding side wall II slidably arranged in the side enclosure II; The side enclosure II or the fixed side wall II is provided with an air inlet / outlet I connected to the outside of the furnace body; The sliding side wall II is provided with an air inlet / outlet II communicating with the furnace body; A spring II is also 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 furnace tube opening.

[0009] Furthermore, the furnace tube is a rectangular quartz glass tube.

[0010] Furthermore, the porcelain boat is provided with an upwardly open rectangular groove, and the bottom wall of the rectangular groove is provided with two limiting grooves, one of which is used to place the substrate, and the other is used to place the crucible; The material storage device comprises 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 are the same and they are grouped correspondingly, and the spacing between the substrates and crucibles in each group is the same; The loading and unloading mechanism comprises two clamping heads, one of which is used to clamp the substrate, and the other is used to clamp the crucible; The distance between the two limiting grooves, the distance between each group of substrates and the crucible, and the distance between the two clamping heads are all kept consistent.

[0011] Furthermore, the clamping head for clamping the substrate is a suction cup; The clamping head for clamping the crucible is a clamping claw.

[0012] Furthermore, the loading and unloading mechanism also includes a robot, and the clamping head is arranged at the output end of the robot.

[0013] Furthermore, the suction cup sucking the substrate comprises the following steps: If the signal given during the process of the suction cup grabbing the substrate is positive, the robot arm will rise a certain distance, which is process one; the signal of the suction cup will be 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 transfers the substrate and the crucible to the porcelain boat; Case 2: If the signal of process 1 is positive and the signal of process 2 is negative, the robot arm descends and repeats the suction cup grabbing operation. The horizontal height of the suction cup during grabbing rises by 0.1 mm relative to the last time, and the cycle is executed until the 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 descends and repeats the suction cup grabbing operation. The horizontal height of the suction cup during grabbing is 0.1 mm lower than the last time, and the robot arm continues to adjust until it meets case one.

[0014] The beneficial effect of the present invention is that the method for continuously preparing two-dimensional materials by an automated CVD device provided by the present invention completely abandons the cumbersome process of traditional manual bilateral loading and bolt fixing, and innovatively adopts unilateral automated loading. By designing the coordinated cooperation of multiple parts, the ceramic boat assembly is successfully sealed immediately after loading, simplifying the process and greatly improving work efficiency. In addition, by designing the loading and unloading mechanism, the problem of loading failure caused by the uneven surface of the loading plate is effectively overcome, and adaptive deviation correction of loading and unloading is realized, thereby realizing the automation of the entire preparation process, and finally realizing 24 hours of continuous automated experiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Attached Figure 1 It is a schematic diagram of the structure from a first angle of the present invention; Attached Figure 2 It is a schematic diagram of the structure from a second angle of the present invention; Attached Figure 3 The present invention is attached Figure 2 A partial enlarged view of the middle A; Attached Figure 4 This is a schematic diagram of the structure of the porcelain boat assembly of the present invention located outside the reaction furnace; Attached Figure 5 It is a front cross-sectional view of the reaction furnace in the present invention; Attached Figure 6 It is a structural schematic diagram of the porcelain boat assembly in the present invention; Attached Figure 7 This is a schematic diagram of the structure of the porcelain boat assembly of the present invention located in a reaction furnace; Attached Figure 8 It is a front cross-sectional view of the porcelain boat assembly of the present invention located in a reaction furnace; Attached Fig. 9 For attachment Figure 8 A partial enlarged view of point B in the middle; Attached Fig.10 For attachment Figure 8 A partial enlarged view of point C in the middle; Attached Fig.11 For attachment Figure 8 A partial enlarged view of point D in the middle.

[0016] In the figure, 1-reaction furnace; 11-furnace body; 12-furnace tube; 13-connecting flange; 131-inlet / outlet gas 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 and outlet; 134-inlet / outlet hole Ⅱ; 135-inlet / outlet interval; 136-sealing cylinder; 14-inlet / outlet flange; 141-side enclosure Ⅱ; 142-fixed side wall Ⅱ; 143-sliding side wall Ⅱ; 144-inlet / outlet port Ⅰ; 145-inlet / outlet port Ⅱ; 146-spring Ⅱ; 2-porcelain boat assembly; 21-porcelain boat; 211-rectangular groove; 212-limiting groove; 22-porcelain boat rod; 221-sealing ring; 3-linear moving mechanism; 4-material storage device; 41-substrate storage tray; 42-crucible storage tray; 5-loading and unloading mechanism; 51-manipulator; 52-suction cup; 53-gripper; 6-workbench. DETAILED DESCRIPTION

[0017] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0018] It should be noted that all directional indications (such as up, down, left, right, front, back, etc.) in the embodiments of the present invention 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 indication will also change accordingly.

[0019] In addition, in the present invention, descriptions such as "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 the indicated technical features. Therefore, the features defined as "first" or "second" may explicitly or implicitly include at least one of the features. In the description of the present invention, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0020] In the present invention, unless otherwise clearly specified and limited, the terms "fixed", "connected", etc. should be understood in a broad sense. For example, "fixed" can be a fixed connection, a detachable connection, or an integral connection; "connected" can be a mechanical connection, an electrical connection, a physical connection, or a wireless communication connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0021] In addition, the technical solutions between the various embodiments of the present invention can be combined with each other, but it must be based on the fact that ordinary technicians in the field can implement it. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0022] As attached Figure 1 -Attached Fig.11 As shown, the present invention provides a method for continuously preparing two-dimensional materials using an automated CVD device, 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. Preferably, the automated CVD device further comprises a workbench 6, and the reaction furnace 1, the porcelain boat assembly 2, the linear motion 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; The reaction furnace 1 includes a furnace body 11 for performing vapor deposition, wherein the furnace body 11 is used to provide the substrate and the precursor with the required temperature and atmosphere and other environmental requirements, and a material inlet and outlet 133 is provided on one side of the furnace body 11, and the material inlet and outlet 133 is used to allow the porcelain boat assembly 2 containing the substrate and the precursor to enter and exit the furnace body 11; The porcelain boat assembly 2 includes a porcelain boat 21 and a porcelain boat rod 22 which are arranged in sequence. The porcelain boat rod 22 is arranged at the output end of the linear motion mechanism 3, and is used to drive the porcelain boat 21 to move and achieve the airtightness requirements of the porcelain boat assembly 2 and the furnace body 11. The porcelain boat 21 is used to carry a substrate and a crucible. The linear motion mechanism 3 is 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 and the material inlet and outlet 133 cooperate to complete the sealing through the sealing ring 221 on the porcelain boat rod 22, that is, the porcelain boat rod 22 seals the material inlet and outlet 133, realizing the operation of injection and sealing, which greatly improves the efficiency of loading and unloading, and thus improves the overall work efficiency; The material storage device 4 is used to store the substrate to be subjected to chemical vapor deposition and the crucible, wherein the crucible is used to hold the precursor; 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 chemical vapor deposition, and is also used to transfer the substrate and the crucible on the porcelain boat 21 that have completed the vapor deposition to the next station, wherein the next station can be the material storage device 4 or another storage device for storing the prepared two-dimensional material; The loading and unloading mechanism 5 is used to transfer the substrate and the crucible to realize the automation of the system, thereby achieving 24-hour continuous operation and ensuring the work quality.

[0023] The method for continuously preparing two-dimensional materials using the automated CVD device is to perform continuous automated experiments using the automated CVD device.

[0024] The method for continuously preparing two-dimensional materials by an automated CVD device provided by the present invention completely abandons the cumbersome process of traditional manual bilateral loading and bolt fixing, and innovatively adopts unilateral automated loading. By designing the coordinated cooperation of various parts, the ceramic boat assembly 2 is successfully sealed immediately after loading, which simplifies the process and greatly improves work efficiency. In addition, by designing the loading and unloading mechanism 5, the problem of loading failure caused by the uneven surface of the loading plate is effectively overcome, and adaptive deviation correction of loading and unloading is realized, thereby realizing the automation of the entire preparation process, and finally realizing 24 hours of continuous automated experiments.

[0025] 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 has a furnace cavity, and the furnace tube 12 is arranged in the furnace cavity. 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; 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; 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.

[0026] In this embodiment, the substrate and precursor can be loaded and unloaded through one side of the reaction furnace 1. Compared with the two-way loading and unloading in the prior art (CN215887222U-a device for gas phase preparation of two-dimensional materials), the efficiency of loading and unloading can be greatly improved, and only the movable sealing cooperation between the outer wall of the porcelain 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 is convenient for meeting the atmosphere requirements in the furnace tube 12 and for loading and unloading the porcelain boat assembly 2.

[0027] In one embodiment, the inlet / outlet air cavity 131 includes a side enclosure Ⅰ1311, a fixed side wall Ⅰ1312 arranged at one end of the side enclosure Ⅰ1311, and a sliding side wall Ⅰ1313 slidably arranged in the side enclosure Ⅰ1311. Preferably, the side enclosure Ⅰ1311 is a cylindrical structure, and the fixed side wall Ⅰ1312 and the sliding side wall Ⅰ1313 are both circular plate structures, so that the inlet / outlet air cavity 131 is a cylindrical cavity. Preferably, the sliding side wall Ⅰ1313 is made of high temperature resistant fluororubber, which can ensure both the sealing effect and the service life. The inlet / outlet hole Ⅰ132 is arranged on the sliding side wall Ⅰ1313; 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 enclosure I 1311 or the fixed side wall I 1312. Preferably, the air inlet / outlet hole II 134 is arranged on the side enclosure I 1311. A spring Ⅰ1314 is also provided between the sliding side wall Ⅰ1313 and the fixed side wall Ⅰ1312, and the spring Ⅰ1314 pushes the sliding side wall Ⅰ1313 to abut against the opening of the furnace tube 12. In this embodiment, by providing the spring Ⅰ1314 and the sliding side wall Ⅰ1313, the sliding side wall Ⅰ1313 is a movable structure, so that the sliding side wall Ⅰ1313 can be close to the opening of the furnace tube 12, ensuring the sealing between the opening of the furnace tube 12 and the sliding side wall Ⅰ1313, and preventing gas from flowing into the furnace chamber. In this embodiment, the sliding side wall Ⅰ1313 can be used as a fixed structure for fixing the end of the furnace tube 12, thereby facilitating the fixed installation of the end of the furnace tube 12.

[0028] The design of the connecting flange 13 of this embodiment, together with the internal spring Ⅰ1314 and the sliding side wall Ⅰ1313 (the spring Ⅰ1314 and the sliding side wall Ⅰ1313 not only seal but also buffer the furnace tube 12 to prevent the furnace tube 12 from being damaged), the sliding side wall Ⅰ1313 and the furnace tube 12, and the porcelain boat rod 22 and the connecting flange 13 form an airtight system that is interlocked with each other, thereby realizing the operation of good sealing during sample injection.

[0029] In one embodiment, the material inlet and outlet 133 is provided with a sealing cylinder 136 extending toward one side of 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 with the inner wall of the sealing cylinder 136. Preferably, a plurality of sealing rings 221 are provided on the outer wall of the porcelain boat rod 22 to improve the sealing effect. In this embodiment, the outer wall of the sealing cylinder 136 can also be used as a guide column for the spring I 1314. Preferably, the sealing ring 221 is made of high temperature resistant fluororubber.

[0030] In one embodiment, the other end of the furnace body 11 is provided with an air outlet / inlet flange 14; The outlet / inlet flange 14 includes 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. Preferably, the side enclosure II 141 is a cylindrical structure, and the fixed side wall II 142 and the sliding side wall II 143 are both circular plate structures. Preferably, the sliding side wall II 143 is made of high temperature resistant fluororubber, which can ensure both the sealing effect and the service life. 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. Preferably, the air inlet / outlet I 144 is provided on the end surface of the fixed side wall II 142. The sliding side wall II 143 is provided with an air inlet / outlet II 145 communicating with the furnace body 11; A spring II146 is also provided between the sliding side wall II143 and the fixed side wall II142, and the spring II146 pushes the sliding side wall II143 to abut against the opening of the furnace tube 12, and the opening of the furnace tube 12 is connected to the air outlet / inlet II145, wherein the diameter of the air outlet / inlet II145 is smaller than the opening of the furnace tube 12. In this embodiment, by providing the spring II146 and the sliding side wall II143, the sliding side wall II143 is a movable structure, so that the sliding side wall II143 can be closely attached to the opening of the furnace tube 12, ensuring the sealing of the opening of the furnace tube 12 and the sliding side wall II143, and preventing gas from flowing into the furnace chamber. In this embodiment, the sliding side wall I1313 can be used as a fixed structure for fixing the end of the furnace tube 12, so as to facilitate the fixed installation of the end of the furnace tube 12.

[0031] In one of the embodiments, the furnace tube 12 is a rectangular quartz glass tube. Compared with the furnace tube in the prior art (CN221141863U-a furnace tube suitable for visualized CVD with strong airtightness) with a rectangular structure in the middle and cylindrical structures at both ends, the turbulence of the gas generated when the area inside the tube changes can be avoided, which affects the experimental results, and the processing of the furnace tube 12 is also convenient.

[0032] In one embodiment, the porcelain boat 21 is provided with an upwardly open rectangular groove 211, which is used to accommodate a substrate and a crucible containing a precursor. The side wall of the rectangular groove 211 can prevent the substrate from being displaced laterally and the crucible from tipping over. At the same time, the porcelain boat 21 can also keep the substrate and the crucible thereon level at all times. The bottom wall of the rectangular groove 211 is provided with two limiting grooves 212, one of which is used to place a substrate, and the other is used to place a crucible. The limiting groove 212 can be used to accommodate a crucible or a substrate, thereby preventing the crucible or the substrate from being displaced along the length direction of the rectangular groove 211, thereby ensuring the relative distance between the two. 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 is the same and they are grouped correspondingly, and the spacing between the substrates and crucibles in each group is the same; The loading and unloading mechanism 5 includes two clamping heads, one of which is used to clamp the substrate, and the other is used to clamp the crucible; 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 kept consistent; 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 groove 212 at the same time, which can greatly improve the extraction efficiency of the crucible and the substrate, realize one-step loading, and the operation is simple and fast.

[0033] In one embodiment, the clamping head for clamping the substrate is a suction cup 52; the clamping head for clamping the crucible is a clamping claw 53. The loading and unloading mechanism 5 also includes a manipulator 51, and the clamping head is arranged at the output end of the manipulator 51. In this embodiment, the output end of the manipulator 51 is provided with a suction cup 52 for sucking the substrate and a clamping claw 53 for clamping the crucible containing the precursor. The manipulator 51 grabs the substrate and the crucible from the material storage device 4 and places them on the porcelain boat 21. After the preparation of the two-dimensional material is completed, the substrate and the crucible are taken out from the porcelain boat 21 and placed on the material storage device 4, and then a new substrate and crucible are taken from the material storage device 4. This reciprocating cycle is carried out to realize the continuous preparation of two-dimensional materials by automated chemical vapor deposition.

[0034] Specifically, the loading and unloading mechanism 5 controls the movement of the manipulator 51 through the feedback of the suction cup 52, so as to ensure that the suction cup 52 stably absorbs the substrate. The logic is: if the signal given during the process of the suction cup 52 grabbing the substrate is positive, the manipulator 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 manipulator 51 transfers the substrate and the crucible to the porcelain boat 21; case two: if the signal of process one is positive and the signal of process two is negative, the manipulator 51 descends and repeats the grabbing operation of the suction cup 52. When grabbing, the horizontal height of the suction cup 52 increases by 0.1 mm relative to the last 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 manipulator 51 descends and repeats the grabbing operation of the suction cup 52. When grabbing, the horizontal height of the suction cup 52 decreases by 0.1 mm relative to the last 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 manipulator 51 descends and repeats the grabbing operation of the suction cup 52. When grabbing, the horizontal height of the suction cup 52 decreases by 0.1 mm relative to the last time, and the cycle is executed until case one is met. This logic can solve the problem of clamping failure caused by tiny unevenness on the surface of the material storage device 4 through a double detection mechanism (process one + process two) combined with dynamic displacement compensation.

[0035] In one embodiment, the linear moving mechanism 3 is a linear driving mechanism, which has the characteristics of precise control and long moving stroke, and can ensure that the porcelain boat assembly 2 accurately enters the reaction furnace 1.

[0036] The above is only an embodiment and does not limit the present invention in any way. Any person skilled in the art can use the above disclosed technical contents to make many possible changes, modifications or modifications to the technical solutions of the present invention into equivalent embodiments of equivalent changes without departing from the scope of the technical solutions of the present invention. Therefore, any simple modification, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solutions of the present invention shall fall within the scope of protection of the technical solutions 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 using the automated CVD device is to perform continuous automated experiments using the automated CVD device.

2. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 1, characterized in that: 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. 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). The porcelain boat rod (22) and the material inlet and outlet (133) are sealed by means of a sealing ring (221) on the porcelain boat rod (22).

3. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 2, characterized in that: 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).

4. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 3, 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).

5. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 2, 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).

6. 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.

7. The method for continuously preparing two-dimensional materials using an automated CVD device according to any one of claims 1 to 6, 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.

8. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 7, 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).

9. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 8, 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).

10. The method for continuously preparing two-dimensional materials using an automated CVD device as claimed in claim 9, 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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