Automatic chemical vapor deposition device and application thereof

Abstract

The invention discloses an automatic chemical vapor deposition device and application thereof. The automatic chemical vapor deposition device comprises a furnace body, a sample tube, a sample rod, a sealing piece and a displacement platform, the furnace body is provided with a cavity for accommodating a sample tube; the sealing element is used for sealing the furnace body and the sample tube and is provided with an opening, so that the sample rod can conveniently penetrate through and extend into the sample tube; the sample rod is detachably mounted on the displacement platform, one end of the sample rod is provided with a sample table, and the other end of the sample rod is provided with a limiting structure; the displacement platform comprises a linear module and is used for driving the sample rod to do linear motion so as to complete automatic sample feeding and discharging. The linear module is adopted for automatic sample feeding and discharging, the automatic sample feeding and discharging process can be rapidly and stably completed, by designing the multiple sample rods, the multi-round rapid experiment process can be fully automatically executed, the inter-group operation time is shortened, and the automatic sample feeding and discharging device is suitable for chemical vapor deposition reaction and scientific research under various chemical systems and has very high practicability.

Description

Technical Field

[0001] This application relates to the technical field of chemical vapor deposition, and particularly relates to an automatic chemical vapor deposition device and its application. Background Art

[0002] Chemical Vapor Deposition (CVD for short) is a key technology that enables gaseous or vaporous substances to react at high temperatures on the gas phase or gas-solid interface to obtain solid materials. It plays a crucial role in fields such as the research and development of new crystals, the deposition of thin film materials, and the manufacturing of semiconductor devices.

[0003] The entire process in CVD experiments is like a black box, and the experimental results can only be obtained by conducting the next experiment after adjusting all macroscopic parameters in the experiment. Therefore, the design of experimental parameters is a key challenge. For the chemical vapor deposition process, the key macroscopic parameters that can be controlled include, but are not limited to: the temperature of the reaction chamber, the system pressure, the type and flow rate of the gas fluid used to carry the gaseous reactants for migration, the type of the substrate holder, and the type of reactants. In a set of CVD experiments, for each additional experimental parameter explored, the number of experiments required will increase exponentially, causing the curse of dimensionality, which hinders the in-depth exploration of scientific principles.

[0004] The basic experimental process of CVD includes, but is not limited to: pushing the experimental materials into the CVD furnace body, installing sealing components such as flanges to seal the CVD furnace body, connecting the gas path to the furnace body and then heating the furnace body to make it react. After the experiment ends, wait for the temperature to drop, disassemble the sealing device, and take out the experimental samples, thus completing the preparation of specific materials. During the CVD process, the original experimental method has certain limitations: manually placing experimental samples has certain requirements for the operation of technicians. If there is an operation error during the process of putting them into the furnace body, the samples are likely to spill out; moreover, the installation of sealing components will also increase the operation burden on experimental personnel. Especially for the implementation of multiple groups of experiments, it is necessary to repeatedly install and disassemble the sealing device, spending extra time.

[0005] At the same time, due to the many influencing factors of CVD, the quantitative control scheme in the manual experimental plan has limitations, resulting in poor repeatability of the CVD experiment reaction, which hinders the further acquisition of high-quality experimental data and the quantitative analysis of experimental parameters in CVD experiments.

[0006] Therefore, how to achieve fast and stable CVD experiments, improve experimental efficiency, and at the same time provide more exploitable parameters for exploring the growth conditions of new materials remains the research focus and difficulty in the field of chemical vapor deposition technology. Summary of the Invention

[0007] The purpose of this application is to provide an improved automatic chemical vapor deposition device and its application.

[0008] To achieve the above object, the present application adopts the following technical solutions:

[0009] On the one hand, the present application discloses an automatic chemical vapor deposition device, including a furnace body, a sample tube, a sample rod, a seal, and a displacement platform; the furnace body has a cavity for accommodating the sample tube and is used for heating; the sample tube is placed in the cavity of the furnace body for placing the sample rod and performing chemical vapor deposition therein; the seal is used to seal the furnace body and the sample tube, and the seal has an opening to facilitate the sample rod to pass through and extend into the interior of the furnace body and the sample tube; the sample rod is detachably installed on the displacement platform, and one end of the sample rod has a sample stage and the other end has a limiting structure. After the sample rod is inserted into the opening of the seal, the two are in a sealed fit; the displacement platform includes a linear module, and the linear module controls the linear movement of the displacement platform to drive the sample rod to perform linear movement to complete the automatic sample loading and unloading operation; alternatively, the sample rod is detachably installed on the linear module, and the linear module directly drives the sample rod to perform the sample loading and unloading operation.

[0010] It should be noted that the present application uses a linear module to drive the displacement platform or the sample rod to perform the automatic sample loading and unloading operation to realize the automatic control of the chemical vapor deposition device, which is not only simpler and more convenient to use, but also improves the stability of the sample loading and unloading process; for multiple groups of experiments, only multiple groups of sample rods need to be prepared. After the previous group of sample rods is taken out, the next group of sample rods can be replaced to start the next group of experiments, shortening the operation time between groups. In short, the present application can load and unload samples with high stability and high efficiency, shorten the operation time between groups, and is applicable to chemical vapor deposition reactions and scientific research under various chemical systems; using the automatic chemical vapor deposition device of the present application for CVD experiments can improve the stability of experimental results while improving experimental efficiency, and has strong practicability.

[0011] In one implementation manner of the present application, the displacement platform includes a plurality of sample rods, and different sample rods are switched in the following ways:

[0012] a) Use a robotic arm to replace the sample rod to achieve the switching of different sample rods;

[0013] b) The displacement platform further includes a translation module for controlling the parallel movement of the displacement platform relative to the furnace body to achieve the switching of different sample rods.

[0014] In one implementation manner of the present application, the furnace body is a micro hot stage with rapid heating.

[0015] In one implementation manner of the present application, the rapid heating can reach a heating rate of 100 °C / min.

[0016] In one implementation manner of the present application, the furnace body further includes a cooling system for cooling the furnace body.

[0017] In one implementation of the present application, the cooling system is a water cooling system.

[0018] In one implementation of the present application, the automated chemical vapor deposition apparatus of the present application further includes an in-situ optical microscope system; an observation window is opened in the furnace body and sealed with a transparent material, the sample tube is made of a transparent material, and the objective lens of the optical microscope system faces the observation window for in-situ observation of the experimental sample.

[0019] In one implementation of the present application, the in-situ optical microscope system includes at least one of a charge-coupled device and a Raman spectrometer.

[0020] In one implementation of the present application, the observation window uses a plano-convex lens, and the corresponding sample tube is square or the tube wall at the corresponding position of the sample tube is parallel to the plano-convex lens.

[0021] In one implementation of the present application, the sealing method between the sample rod and the seal is at least one of the following methods:

[0022] a) A gasket is provided between the limiting structure and the seal to form an end-to-end seal;

[0023] b) The outer side surface of the sample rod and the inner side surface of the seal are used to form a side seal, so that the sample rod can be sealed everywhere during its movement.

[0024] In one implementation of the present application, the middle part of the sample rod and the opening of the seal are in a sliding and tight fit.

[0025] In one implementation of the present application, the sample stage includes a groove and / or a connection port; the groove is used to place the sample, and the connection port is used to place the sample boat.

[0026] In one implementation of the present application, the seal is fixedly connected to the furnace body, and both use end face sealing or side sealing.

[0027] In one implementation of the present application, the fixed connection includes at least one of bolt connection and welding.

[0028] In one implementation of the present application, any position of the furnace body, the sample rod, and the seal has an external gas path connection port for connecting to a gas source.

[0029] In one implementation of the present application, the external gas path uses a digital mass flow meter to control the gas flow rate and flow.

[0030] In one implementation of the present application, the automated chemical vapor deposition apparatus further includes a sample boat, and the sample boat is connected to the sample stage of the sample rod; the sample boat includes at least one crucible profiling positioning groove and several substrate profiling positioning grooves; the crucible profiling positioning groove is used to place the crucible, and the substrate profiling positioning groove is used to place the substrate.

[0031] In one implementation of the present application, the crucible profiling positioning groove is arranged upstream of the substrate profiling positioning groove; when in use, the direction in which the gas flow passes from upstream to downstream is the positive direction.

[0032] In one implementation of the present application, the automated chemical vapor deposition apparatus further includes a crucible that is compatible with the sample boat and is used to place samples.

[0033] In one implementation of the present application, the automated chemical vapor deposition apparatus further includes a substrate that is compatible with the sample boat.

[0034] In one implementation of the present application, the substrate includes at least one of a silicon wafer, sapphire, and magnesia.

[0035] In one implementation of the present application, the sample positioning boat is an integrally formed structure.

[0036] In one implementation of the present application, the sample positioning boat is prepared from an inert high-temperature resistant solid material.

[0037] In one implementation of the present application, the sample positioning boat is prepared from quartz glass, corundum, or silicon carbide.

[0038] In one implementation of the present application, the automated chemical vapor deposition apparatus of the present application further includes an electrical control system; the electrical control system includes completing various process controls of the automated chemical vapor deposition apparatus through a PLC control system, including at least one of temperature control, mechanical movement action control, gas flow control, in-situ characterization optical microscope control, time control, and alarm control.

[0039] Another aspect of the present application discloses the application of the automated chemical vapor deposition apparatus of the present application in crystal research and development, thin film material deposition, or semiconductor device fabrication.

[0040] It should be noted that for the automated chemical vapor deposition apparatus of the present application, the specific fields to which it can be applied can refer to existing chemical vapor deposition, including but not limited to crystal research and development, thin film material deposition, and semiconductor device fabrication.

[0041] Due to the above technical solutions, the beneficial effects of the present application are as follows:

[0042] The automated chemical vapor deposition apparatus of the present application uses a linear module for automatic sample loading and unloading, and can quickly and stably complete the automated process of loading and unloading samples. In a further improved solution, by designing a number of sample rods, it can fully automatically execute multiple rounds of rapid experimental processes, shortening the operation time between groups, and is applicable to chemical vapor deposition reactions and scientific research under various chemical systems; using the automated chemical vapor deposition apparatus of the present application for experiments can improve the stability of experimental results while enhancing experimental efficiency, and has strong practicality. Brief Description of the Drawings

[0043] Figure 1 It is a schematic structural diagram of an automatic chemical vapor deposition device in an embodiment of the present application;

[0044] Figure 2 It is a schematic diagram of the furnace body and the quartz tube of the automatic chemical vapor deposition device in an embodiment of the present application;

[0045] Figure 3 It is a schematic structural diagram of the sample inlet / outlet device of the automatic chemical vapor deposition device in an embodiment of the present application;

[0046] Figure 4 It is a schematic structural diagram of the seal of the automatic chemical vapor deposition device in an embodiment of the present application;

[0047] Figure 5 It is a schematic structural diagram of the displacement platform of the automatic chemical vapor deposition device in an embodiment of the present application;

[0048] Figure 6 It is a schematic diagram of the gas inlet / outlet system of the automatic chemical vapor deposition device in an embodiment of the present application;

[0049] Figure 7 It is a schematic structural diagram of the sample boat of the automatic chemical vapor deposition device in an embodiment of the present application;

[0050] Figure 8 It is a schematic diagram of the electrical control system of the automatic chemical vapor deposition device in an embodiment of the present application. Detailed Embodiments

[0051] To overcome the deficiencies of the prior art, achieve fast, stable, and high-throughput CVD experiments, improve experimental efficiency, and at the same time provide more exploitable parameters for exploring the growth conditions of new materials. The present application has developed an improved automatic chemical vapor deposition device, including a furnace body, a sample tube, a sample rod, a seal, and a displacement platform; the furnace body has a cavity for accommodating the sample tube and is used for heating; the sample tube is placed in the cavity of the furnace body for placing the sample rod and performing chemical vapor deposition therein; the seal is used to seal the furnace body and the sample tube, and the seal has an opening to facilitate the sample rod to pass through and extend into the interior of the furnace body and the sample tube; the sample rod is detachably installed on the displacement platform, and one end of the sample rod has a sample stage and the other end has a limiting structure. After the sample rod is inserted into the opening of the seal, the two are in a sealed fit; the displacement platform includes a linear module, and the linear module controls the linear movement of the displacement platform to drive the sample rod to perform linear movement to complete the automatic sample inlet / outlet operation; alternatively, the sample rod is detachably installed on the linear module, and the linear module directly drives the sample rod to perform the sample inlet / outlet operation.

[0052] The fast and stable performance of this application means that a new sample injection method is adopted, which, in combination with a linear module, can quickly and stably complete the automated process of loading and unloading samples. In a further improvement scheme, high throughput means that by placing multiple sample rods and coordinating the parallel movement of a robotic arm or a displacement platform, multiple groups of experiments can be fully automated.

[0053] In a further improvement scheme, an in-situ optical microscope system is installed, which can simultaneously obtain the synthesis of the sample itself and the optical information during the sample synthesis process in a single group of experiments, expanding the richness of data in a single group of experiments. Further, the multi-functionality of this application means that a generalized sample rod is adopted, and various forms of sample boats with specific shapes can be connected to the end of the sample rod. The sample boats are compatible with various placement combinations of solid raw materials, liquid raw materials, and substrates, with a large parameter space, and can be applied to various CVD chemical systems, meeting the quantitative exploration of CVD experiments in a large parameter space. The automatic chemical vapor deposition device of this application is suitable for scientific research on the chemical vapor deposition process under various systems, can meet the growth conditions of various material systems; has a large parameter space and can be used to explore the growth process of new materials; can realize a fast, stable, and high-throughput experimental process, which is of great significance for rapid experiments and in-depth exploration of scientific principles.

[0054] The automatic chemical vapor deposition device of this application mainly includes a CVD furnace body, an automated sample loading and unloading system, a high-throughput cooperation system, an in-situ optical microscope system, an air inlet and outlet system, and an electrical control system according to its functions.

[0055] Among them, the core component for chemical reactions is the CVD furnace body, including but not limited to equipment reaction chambers (quartz reaction tubes, i.e., sample tubes) with a diameter of 1 inch or larger or a micro CVD furnace body (with a diameter of 10 mm). The furnace body is equipped with a heating system to create a high-temperature environment inside the furnace body. Parameters such as the heating rate and holding time are controlled through a temperature control program. The time for a single experiment is controlled by the heating and cooling rates of the furnace body. This application uses a micro hot stage with a fast heating and cooling function. Due to the small size of the hot stage, a heating rate of up to 100 °C / min can be achieved, and a water cooling system is equipped on the hot stage to achieve a rapid cooling process. The fast heating and cooling process significantly improves the experimental efficiency compared to traditional CVD tube furnaces.

[0056] Furthermore, in order to achieve the function of in-situ observation, the reaction chamber of the equipment is made of high-quality quartz tubing, which is square in the middle of the quartz tube. Compared with a circular quartz tube, the square quartz tube will not affect the light path, so in-situ optical observation can be realized.

[0057] Furthermore, an in-situ observation window is opened above the furnace body, which allows the optical path to pass through the in-situ observation window and the quartz tube, focusing the optical path on the experimental sample to achieve in-situ observation. The experimental optical path can be connected to a variety of characterization instruments: if the optical path is connected to a CCD, in-situ electronic collection of optical image information can be achieved; if the optical path is connected to a Raman spectrometer, in-situ Raman spectroscopy characterization can be achieved, etc.

[0058] The furnace body needs to be sealed to prevent the gas atmosphere inside the quartz tube from being disturbed by air. In traditional CVD tube furnaces, the gas path is connected to the quartz tube through a flange device, and the sample also needs to be manually placed in the center of the quartz tube. The installation, disassembly, and sample injection method of the flange device are not suitable for automated experimental devices; therefore, this application designs a new type of sample loading and unloading device. By setting a seal, the quartz tube and the seal are permanently sealed. At the same time, a sample rod is designed. Pushing the sample rod into the furnace body can complete the sample placement in the furnace, and the sample rod and the seal can achieve sealing, ensuring that when the sample rod is pushed into the furnace body and placed, the sealing state between the sample rod and the seal can be maintained.

[0059] Based on this sample injection method, this application is equipped with a linear module. By electrically controlling the displacement platform, the sample rod placed on the displacement platform can perform precise linear motion. At the same time, a pressing cylinder is installed on the displacement platform to ensure a rigid connection between the sample rod and the displacement platform, ensuring that the sample rod does not slide or shift during the movement, and ensuring a stable automated sample loading and unloading process.

[0060] For multiple experiments, this application is equipped with multiple identical sample rods, designs a jaw with a specific shape, and at the same time, a profiling groove adapted to the jaw is opened on the sample rod. Connecting the jaw to the robotic arm, through robotic arm programming, automated clamping and placement of the sample rod can be achieved. This application sets multiple groups of sample rod profiling grooves on the displacement platform, which can stably place multiple groups of sample rods. During the interval between each group of experiments, the robotic arm automatically clamps the sample rod completed in the previous group of experiments and exchanges positions with the next group of experimental groups to be reacted on the displacement platform, thus realizing a fully automated process for multiple groups of experiments.

[0061] Furthermore, the gas path system of the equipment can select a corresponding digital mass flowmeter according to the CVD material system. In this application, the connection of the gas path to the gas path of the furnace body is set on the seal. The gas path connector can use a ferrule or a VCR connection, preferably a VCR connection. The gas path valve uses a gas path valve with a VCR joint to ensure high cleanliness, high sealing performance, and high safety of the gas path.

[0062] Furthermore, for the electrical control system, the operator can program the process according to the process requirements, and complete the process control through the PLC control system. The main contents include: temperature control, gas flow control, linear module motor movement control, pressing cylinder movement control, robotic arm movement control, in-situ observation and characterization control, and other necessary control modules, as well as an alarm system; the industrial computer can execute automatically according to the process program to control the entire process.

[0063] The present invention will be further described in detail below in conjunction with the accompanying drawings through specific embodiments. The following embodiments are only for further illustration of the present application and should not be construed as a limitation of the present application.

[0064] Embodiment

[0065] The automatic chemical vapor deposition device in this example, as Figures 1 to 3 shown, includes a furnace body 1, a sample tube 2, a sample rod 3, a seal 4, and a displacement platform 5; the furnace body 1 has a cavity for accommodating the sample tube 2 and is used for heating; the sample tube 2 is placed in the cavity of the furnace body 1, used for placing the sample rod 3, and chemical vapor deposition is carried out therein; the seal 4 is used to seal the furnace body 1 and the sample tube 2. As Figure 3 shown, the seal 4 has an opening 41 to facilitate the sample rod 3 to pass through and extend into the furnace body 1 and the sample tube 2; the sample rod 3 is detachably installed on the displacement platform 5, and one end of the sample rod 3 has a sample stage, and the other end has a limiting structure 31. After the sample rod 3 is inserted into the opening 41 of the seal 4, the two are in a sealed fit; the displacement platform 5 includes a linear module 51, and the linear module 51 controls the linear movement of the displacement platform 5 to drive the sample rod 3 to perform linear movement to complete the automatic sample loading and unloading operation. It can be understood that the sample rod 3 can also be detachably installed on the linear module 51, and the linear module 51 directly drives the sample rod 3 to perform the sample loading and unloading operation, and the displacement platform 5 remains stationary during the sample loading and unloading process. The sample tube in this example is a quartz tube made of quartzite.

[0066] As Figure 1 and Figure 5 shown, the displacement platform 5 in this example includes a plurality of sample rods 3, and a robotic arm 8 is used to replace the sample rods 3 to realize the switching of different sample rods. It can be understood that in addition to using a robotic arm to switch the sample rods, a translation module can also be designed on the displacement platform 5 to control the relative parallel movement of the displacement platform 5 with respect to the furnace body 1, so as to realize the switching of different sample rods 3.

[0067] The furnace body 1 in this example is a micro hot stage with rapid heating, and the heating rate can reach 100 °C / min; moreover, a cooling system is provided on the furnace body 1 to cool the furnace body 1. In this example, a water cooling system is specifically used.

[0068] For the convenience of observation, in the improved solution of this example, an in-situ optical microscope system 6 is also added; an observation window 11 is opened at the top of the furnace body 1 and sealed with a transparent material. The sample tube 2 is made of a transparent material. The objective lens of the in-situ optical microscope system 6 faces the observation window 11 and is used for in-situ observation of the experimental sample. According to requirements, the in-situ optical microscope system 6 can adopt a charge-coupled device (CCD) or a Raman spectrometer. If the optical path is connected to the CCD, the in-situ electronic collection of optical image information can be achieved; if the optical path is connected to the Raman spectrometer, the in-situ Raman spectrum characterization can be realized, etc. Further, for better observation, the middle part of the sample tube is square, as Figure 2 shown. Compared with the circular quartz tube, the square quartz tube will not affect the optical path, so in-situ optical observation can be realized. Of course, the observation window is also sealed with a plano-convex lens, that is, the influence on the optical path is avoided as much as possible.

[0069] As Figure 3 shown, in this example, the sample rod 3 and the seal 4 can adopt a variety of sealing methods. For example, a) a gasket is arranged between the limit structure 31 and the seal 4 to form end-to-end sealing; b) the outer side surface of the sample rod 3 and the inner side surface of the seal 4 are used to form side sealing, so that the sample rod 3 can be sealed everywhere during the movement position. In this example, the two methods are combined to improve the sealing effect. Further, the middle part of the sample rod 3 and the opening 41 of the seal 4 are in a sliding and tight fit. The seal 4 of this example is as Figure 4 shown.

[0070] In this example, the seal 4 and the furnace body 1 are fixedly connected, and end face sealing or side sealing is adopted between the two; the fixed connection includes at least one of bolt connection and welding.

[0071] As Figure 6 shown, the gas path system of this example can select a corresponding digital mass flowmeter according to the CVD material system. In order to make the flow control be called informatization, this example adopts an informatization digital flowmeter. In this example, the connection of the gas path and the gas path of the furnace body is arranged on one of the sample rod, the seal, and the furnace body. In this example, it is arranged on the seal, and a threaded joint is used to connect with the gas path. The gas path joint can adopt a ferrule or a VCR connection. The VCR connection is preferred. The gas path valve adopts a gas path valve with a VCR joint to ensure high cleanliness, high tightness, and high safety of the gas path.

[0072] In this example, the sample stage includes a groove and / or a connection port; the groove is used to place the sample, and the connection port is used to place the sample boat. It can be understood that the chemical vapor deposition device of this example is equipped with multiple sample rods for placing different samples. For example, some sample rods have grooves, and some sample rods have connection ports for placing sample boats.

[0073] In the improvement scheme of this example, the automatic chemical vapor deposition device further includes a sample boat 7, as Figure 7 shown, the sample boat 7 is connected to the sample stage of the sample rod 3; the sample boat 7 includes at least one crucible profiling positioning groove 71 and a plurality of substrate profiling positioning grooves 72; the crucible profiling positioning groove 71 is used to place the crucible, and the substrate profiling positioning groove 72 is used to place the substrate.

[0074] In this example, the crucible profiling positioning groove 71 is arranged upstream of the substrate profiling positioning groove 72. In this example, the direction in which the gas flow flows from upstream to downstream is defined as the positive direction. After placing the crucible 711 on the positioning boat, there are a plurality of substrate profiling positioning grooves 72 downstream of the crucible 711, and the substrates 721 can be placed at different positions according to the experimental requirements.

[0075] For convenience of use, a crucible 711 is provided in this example. The outer shape and size of the crucible 711 match those of the crucible profiling positioning groove 71 and can be accurately placed therein. Further, a substrate 721 is provided. For all the substrate profiling positioning grooves 72, substrates that match their shapes and sizes can be placed. The type of the substrate is determined by the substrate itself selected to be placed. Specific types of substrates include, but are not limited to, silicon wafers, sapphires, and magnesia. The number of substrates placed in the substrate profiling positioning grooves downstream of the crucible can be several, that is, in a plurality of substrate profiling positioning grooves, a plurality of substrates can be placed.

[0076] The sample positioning boat in this example is of an integrally formed structure. To meet the usage requirements of chemical vapor deposition reactions, the sample positioning boat is made of an inert high-temperature resistant solid material, including but not limited to quartz glass, corundum, or silicon carbide.

[0077] The multi-compatible space positioning boat adopted in this example can meet the quantitative exploration of CVD experiments in a large parameter space. This chemical vapor deposition device is suitable for scientific research on the chemical vapor deposition process under various systems, can meet the growth conditions of various material systems; has a large parameter space and can be used to explore the growth process of new materials.

[0078] In the improvement scheme of this example, the automatic chemical vapor deposition device further includes an electrical control system, as Figure 8As shown, the process program can be compiled according to the needs of the process, and the process control is completed through the PLC control system. The main contents include: temperature control, gas flow control, linear module motor movement control, pressing cylinder movement control, robotic arm movement control, in-situ observation and characterization control, and other necessary control modules, as well as an alarm system. For the step control of the movement module, it is solved by setting the host computer. After calibrating the movement instructions of the linear module, the clamping and placing instructions of the robotic arm, etc. in space, the execution actions are packaged into action functions, and an interface is provided for the host computer to call. Modules such as the real-time call of the in-situ characterization optical microscope are also packaged into callable functions based on the same principle. By setting the execution order of each step through the host computer, the entire process can be controlled in any combination of actions.

[0079] In this example, a fast, stable, and high-throughput automated chemical vapor deposition equipment was developed. Among them, fast and stable means that a new sample injection method is adopted, combined with a linear module, which can quickly and stably complete the automated sample loading and unloading process; high-throughput means that multiple sets of experiments can be fully automated by placing multiple sample rods and combining the feeding and discharging functions of the robotic arm. On the other hand, it also means that an in-situ optical microscope system is installed, and in one set of experiments, the synthesis of the sample itself and the optical information during the sample synthesis process can be obtained simultaneously, expanding the richness of data in one set of experiments; multi-functional means that a general-purpose sample rod is adopted, and the end of the sample rod can be connected to various forms of inert high-temperature-resistant structural parts with specific shapes for holding raw materials, which can be applicable to multiple CVD chemical systems. Specifically, the multi-compatible space positioning boat adopted in this example can meet the quantitative exploration of CVD experiments in a large parameter space. The chemical vapor deposition equipment in this example is suitable for scientific research on the chemical vapor deposition process under various systems, can meet the growth conditions of multiple material systems; has a large parameter space and can be used to explore the growth process of new materials; can experiment with a fast, stable, and high-throughput experimental process, which is of great significance for rapid experiments and in-depth exploration of scientific principles.

[0080] The above content is a further detailed description of the present application in combination with specific implementation manners, and it cannot be determined that the specific implementation of the present application is only limited to these descriptions. For those of ordinary skill in the technical field to which the present invention belongs, without departing from the concept of the present invention, several simple deductions or substitutions can still be made.

Claims

1. An automatic chemical vapor deposition device, characterized in that: It comprises a furnace body (1), a sample tube (2), a sample rod (3), a sealing member (4) and a displacement platform (5); The furnace body (1) has a cavity for accommodating a sample tube (2) and is used for heating; The sample tube (2) is placed in the cavity of the furnace body (1) and is used to place the sample rod (3) and perform chemical vapor deposition therein; The sealing member (4) is used to seal the furnace body (1) and the sample tube (2), and the sealing member (4) has an opening (41) to facilitate the sample rod (2) to pass through and extend into the furnace body (1) and the sample tube (2); The sample rod (3) is detachably mounted on the displacement platform (5), and one end of the sample rod (3) is provided with a sample stage, and the other end is provided with a limiting structure (31). After the sample rod (3) is inserted into the opening (41) of the sealing member (4), the two are in sealing cooperation; The displacement platform (5) comprises a linear module (51), which controls the displacement platform (5) to move linearly, thereby driving the sample rod (3) to move linearly, thereby completing the automatic sample in and out operation; or, the sample rod (3) is detachably mounted on the linear module (51), and the linear module (51) directly drives the sample rod (3) to perform the sample in and out operation.

2. The automatic chemical vapor deposition device according to claim 1, characterized in that: The displacement platform (5) comprises a plurality of sample rods (3), and the switching of different sample rods (3) is performed in the following manner; a) using a mechanical arm (8) to replace the sample rod (3) to achieve switching between different sample rods; b) The displacement platform (5) further comprises a translation module, which is used to control the displacement platform (5) to move parallel to the furnace body (1), thereby realizing the switching of different sample rods (3).

3. The automatic chemical vapor deposition device according to claim 1, characterized in that: The furnace body (1) is a micro hot plate that heats up rapidly; Preferably, the rapid heating can reach a heating rate of 100°C / min; Preferably, the furnace body (1) further comprises a cooling system for cooling the furnace body (1); Preferably, the cooling system is a water cooling system.

4. The automatic chemical vapor deposition device according to claim 1, characterized in that: It also includes an in-situ optical microscope system (6); the furnace body (1) is provided with an observation window (11) and is sealed with a transparent material; the sample tube (2) is made of a transparent material; the objective lens of the in-situ optical microscope system (6) faces the observation window (11) and is used for in-situ observation of the experimental sample; Preferably, the in-situ optical microscope system (6) comprises at least one of a charge coupled device and a Raman spectrometer.

5. The automatic chemical vapor deposition device according to claim 4, characterized in that: The observation window (11) adopts a plane lens, and the corresponding sample tube (2) is square or the tube wall at the corresponding position of the sample tube (2) is parallel to the plane lens.

6. The automatic chemical vapor deposition device according to claim 1, characterized in that: The sealing method between the sample rod (3) and the sealing member (4) is at least one of the following methods; a) a gasket is provided between the limiting structure (31) and the sealing member (4) to form an end-to-end seal; b) The outer side surface of the sample rod (3) and the inner side surface of the sealing member (4) are used to form a side seal, so that the sample rod (3) can be sealed at any position in the movement.

7. The automatic chemical vapor deposition device according to claim 1, characterized in that: The middle portion of the sample rod (3) is tightly fitted with the opening (41) of the sealing member (4) in a sliding manner; Preferably, the sample stage comprises a groove and / or a connection port; the groove is used to place the sample, and the connection port is used to place the sample boat; Preferably, the sealing member (4) and the furnace body (1) are connected in a fixed manner, and both are sealed at the end face or at the side face; Preferably, the fastening connection includes at least one of bolt connection and welding; Preferably, any position of the furnace body (1), the sample rod (3) and the sealing member (4) has an external gas connection port for connecting to a gas source; Preferably, the external gas circuit uses a digital mass flow meter to control the gas flow velocity and flow rate.

8. The automatic chemical vapor deposition device according to claim 1, characterized in that: It also includes a sample boat (7), which is connected to the sample stage of the sample rod (3); The sample boat (7) comprises at least one crucible profiling positioning groove (71) and a plurality of substrate profiling positioning grooves (72); the crucible profiling positioning groove (71) is used to place the crucible, and the substrate profiling positioning groove (72) is used to place the substrate; Preferably, the crucible profiling positioning groove (71) is arranged upstream of the substrate profiling positioning groove (72); when in use, the direction of the airflow flowing from the upstream to the downstream is the positive direction; Preferably, the automatic chemical vapor deposition device further comprises a crucible (711) matched with the sample boat (7) for placing the sample; Preferably, the automatic chemical vapor deposition device further comprises a substrate matched with the sample boat (7); Preferably, the substrate comprises at least one of silicon wafer, sapphire and magnesium oxide; Preferably, the sample positioning boat (7) is an integrally formed structure; Preferably, the sample positioning boat (7) is made of an inert high temperature resistant solid material; Preferably, the sample positioning boat (7) is made of quartz glass, corundum or silicon carbide.

9. The automatic chemical vapor deposition device according to any one of claims 1 to 8, characterized in that: It also includes an electrical control system; The electrical control system includes completing various process controls of the automatic chemical vapor deposition device through a PLC control system, including at least one of temperature control, mechanical motion control, gas flow control, in-situ characterization optical microscope control, time control and alarm control.

10. Use of the automatic chemical vapor deposition device according to any one of claims 1 to 9 in crystal development, thin film material deposition or semiconductor device preparation.

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