Drum type multi-temperature-zone vapor deposition growth and in-situ characterization cavity device

Abstract

The invention provides a drum type multi-temperature-zone vapor deposition growth and in-situ characterization cavity device. Comprising a drum-shaped cavity shell mounted on an X-ray experiment detection device, a plurality of air inlet pipelines inserted into the drum-shaped cavity shell, a platform-type central heating module arranged in the drum-shaped cavity shell, heating sleeve-type two-side heating modules and an experiment sample table arranged below the drum-shaped cavity shell, a sample growth substrate can be arranged on the central heating module, each gas inlet pipeline is connected with the corresponding heating modules on the two sides, and different gas inlet pipelines are used for introducing different precursors and transporting gas. According to the drum-type multi-temperature-zone vapor deposition growth and in-situ characterization cavity device disclosed by the invention, through unique drum-type cavity design and independent and accurate control of multiple heating modules, the growth quality of a two-dimensional semiconductor film is improved, and in-situ observation requirements of a film growth structure and mechanism in different working condition environments are met.

Description

Technical Field

[0001] The invention relates to a vapor deposition growth and in-situ characterization device, in particular to a drum-type vapor deposition growth chamber device with multiple heating modules independently controlled and suitable for in-situ scientific research. Background Art

[0002] In recent years, the application research of two-dimensional semiconductor films in new high-performance devices has become increasingly extensive due to their unique physical and chemical properties, and has shown great potential in the fields of field effect transistors, photodetectors, gas sensors, etc. In these applications, two-dimensional semiconductors not only improve the performance of the devices, but also significantly reduce energy consumption, becoming an indispensable core material for the new generation of electronic and optoelectronic devices. Therefore, researching and developing efficient and controllable two-dimensional semiconductor film preparation technology has become an important task in the current scientific and technological field.

[0003] Vapor deposition (including CVD, CVT, PVD, PVT, etc.) technology has developed rapidly due to its significant advantages in the growth of large-area, high-quality two-dimensional semiconductor thin films. In this technology, the source material (precursor component) is transported to the surface of the sample growth substrate in gaseous form, forming the desired substance on the heated substrate surface, while the residual components are desorbed from the surface and discharged from the reaction device. However, vapor deposition involves complex growth control conditions, and in-depth insight into its deposition reaction mechanism is required to achieve high-quality preparation. Advanced in situ growth characterization technology can directly detect the growth process and mechanism of two-dimensional semiconductors, and then achieve on-demand dynamic regulation. This is the only way for large-scale preparation and industrial development of two-dimensional semiconductors.

[0004] In terms of growth devices, most traditional vapor deposition equipment is based on large sealed structures (large size, heavy weight, and difficult to visualize). The design cannot meet the needs of conducting in-situ research on the thin film growth mechanism and it is difficult to provide effective guidance for the growth process. The lack of in-depth understanding of the reaction mechanism during the growth process fundamentally limits the preparation of high-performance two-dimensional semiconductor materials. In terms of characterization technology, in-situ observation based on optical characterization technology provides an important real-time monitoring method that can reflect the instant feedback brought about by the adjustment of various variables in the reaction process, thereby helping researchers to better understand the growth mechanism of the material and prepare materials with special functions accordingly. However, due to structural limitations, the traditional vapor deposition growth chamber is not compatible with a variety of in-situ characterizations represented by X-ray diffraction detection.

[0005] Therefore, it is urgent to design and develop new vapor deposition growth devices to meet the needs of in-situ observation of material growth and real-time dynamic and refined regulation, so as to promote the high-quality development and application of two-dimensional semiconductor materials and their devices. Summary of the invention

[0006] The purpose of the present invention is to provide a vapor deposition growth device to improve the uniformity and quality of thin film growth and meet the needs of in-situ observation of the thin film growth structure and mechanism under different working conditions.

[0007] In order to achieve the above-mentioned objectives, the present invention provides a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device, comprising a drum-type chamber shell installed on an X-ray experimental detection device, a plurality of air inlet pipes inserted into the drum-type chamber shell, a central heating module in the form of a platform arranged inside the drum-type chamber shell, and two side heating modules in the form of heating sleeves, and an experimental sample table arranged below the drum-type chamber shell; the central heating module is provided with a sample growth substrate, each air inlet pipe is respectively connected to the corresponding two side heating modules, and different air inlet pipes are used to introduce different precursors and transport gases.

[0008] The drum-shaped cavity shell is a hollow cylinder with closed end faces, and comprises a cylindrical side structure and an end face sealing structure covering the end faces of the cylindrical side structure to serve as X-ray transmission windows.

[0009] The diameter of the end face sealing structure is greater than the distance between the end faces on both sides of the drum-shaped cavity shell.

[0010] The cylindrical side structure is made of stainless steel, and the material of the end face sealing structure can withstand the conditions of an inner cavity temperature of >1200°C and an inner cavity pressure of <1×10 -5 Torr, and its X-ray transmittance is >80%.

[0011] A stainless steel base is fastened to the bottom of the drum-shaped cavity shell, and is connected to the experimental sample table of the X-ray experimental detection device through a clamp or a bolt fastening device.

[0012] The air inlet pipe matches the inner diameter of the heating sleeve and is fastened to the heating sleeve; the bottoms of the heating modules on both sides are respectively provided with translation components.

[0013] The central heating module and the heating modules on both sides are equipped with independent temperature sensors.

[0014] The top of the drum-shaped cavity shell is provided with a quartz observation window which is transparent to visible light; and / or the side of the drum-shaped cavity shell is provided with an air inlet for an air inlet pipe to pass through and a multifunctional flange interface, and the multifunctional flange interface includes an exhaust port.

[0015] The cavity of the drum-shaped cavity shell is communicated with a water cooling device.

[0016] A fastening device is installed on the side of the central heating module for fixing the sample growth substrate; and / or a heat shielding material coating layer is provided on the side of the central heating module.

[0017] A drum-shaped multi-temperature zone vapor deposition growth and in-situ characterization cavity device of the present invention adopts a drum-shaped cavity structure design. According to the isoperimetric theorem, compared with other cavity shapes, the vapor deposition cavity is designed as a drum-shaped cavity structure to ensure the maximization of the cavity space under the same cavity shell mass, thereby ensuring the compact integration of the vapor deposition cavity and ensuring the cavity's tolerance to high vacuum. The lightweight and compact characteristics brought by the drum-shaped design enable the cavity to be integrated into various X-ray experimental detection devices using a stainless steel base. The special structural design enables the front and rear side X-ray transmission window end face sealing structures to cover a wide range of X-ray detection angles, thereby effectively ensuring the real-time and effective extraction of multi-dimensional diffraction information during the growth and preparation of thin film materials in the cavity. In addition, the high vacuum environment that can be achieved by the drum-shaped cavity structure is indispensable for achieving extremely high purity and precise control of the deposition process, and is particularly important for various semiconductor devices that require high-quality thin film materials.

[0018] The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device of the present invention adopts a dual air inlet pipe design, allowing different precursors to be introduced into the chamber through different heating channels and to be temperature-modulated by different heating modules. The independent temperature zone design allows each heating module to perform fine temperature control, thereby effectively avoiding the quenching phenomenon caused by the temperature difference between precursors that is common in traditional technologies, and ensuring the flatness and uniformity of the film during the growth process. This precise control not only improves the crystallization integrity of the material, but also optimizes the electrical and mechanical properties of the film, significantly improves the quality of film growth in the chamber, and is of great significance to improving the reliability and performance of the final product. Using the in-situ characterization information during the growth process, the operator can read various microscopic growth mechanisms of the corresponding thin film material, thereby providing accurate guidance for the high-quality growth of the thin film material inside the cavity.

[0019] In addition, the side heating module of the drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device of the present invention adopts a translation component. By finely adjusting the specific position of the heating module, the optimization of the precursor vapor distribution is achieved, the controllability of the growth environment during the vapor deposition process is enhanced, and the overall quality of thin film growth can be further improved; by dynamically adjusting the heating module, the supply of the precursor can be adjusted according to the real-time monitoring data to achieve the optimal vapor distribution state, thereby ensuring the environmental stability during the thin film growth process in the cavity and improving the growth quality and efficiency of the thin film material. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a front view of a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to one embodiment of the present invention.

[0021] Figure 2It is a schematic diagram of the operating principle of a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device in thin film growth according to the present invention.

[0022] Figure 3 It is a schematic diagram of the operating principle of a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device of the present invention when performing in-situ characterization of the thin film growth state in the chamber.

[0023] Figure 4 It is a schematic structural diagram of three independently controlled heating modules of a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device of the present invention.

[0024] Figure 5 It is a side cross-sectional view of the heating modules on both sides of a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device of the present invention.

[0025] Figure 6 A front view of a central heating module of a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to the present invention is shown.

[0026] Figure 7 Shown is a top view of a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device of the present invention. DETAILED DESCRIPTION

[0027] In order to more clearly illustrate the technical solution in the embodiment of the present invention, a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device proposed by the present invention is further introduced below in combination with the embodiments and drawings.

[0028] The following description of at least one exemplary embodiment is actually only illustrative and is by no means intended to limit the present invention and its application or use. 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.

[0029] Figure 1 A drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to an embodiment of the present invention is shown. The device is installed on an X-ray experimental detection device such as a six-circle diffractometer, and can realize real-time characterization of the material growth process under high vacuum and high temperature environment. It is suitable for the preparation and performance research of high-quality thin film materials.

[0030] like Figure 1As shown, the drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device specifically includes: a drum-type chamber shell 1 installed on the X-ray experimental detection device, a plurality of air inlet pipes 31, 32 inserted on the drum-type chamber shell 1, a central heating module 21 in the form of a platform arranged inside the drum-type chamber shell 1, and heating modules 22, 23 on both sides in the form of heating sleeves, and an experimental sample table arranged below the drum-type chamber shell 1. Among them, a sample growth substrate is arranged on the central heating module 21 for sample growth, each air inlet pipe 31, 32 is respectively connected to the corresponding heating modules 22, 23 on both sides, and the side of the drum-type chamber shell 1 is provided with air inlets 131, 132 for the air inlet pipes 31, 32 to pass through.

[0031] Figure 2 The present invention is a schematic diagram of the operating principle of a drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device in thin film growth. In this embodiment, while the drum-type chamber housing 1 grows thin film materials in a high vacuum environment, it can effectively be compatible with X-ray in-situ detection, thereby gaining a deep understanding of the material growth mechanism and further ensuring high-quality semiconductor film growth. The drum-type chamber adopts dual air inlet pipes 31 and 32, and different air inlet pipes 31 and 32 are used to introduce different precursors and transport gases to achieve the introduction of different precursor components.

[0032] Preferably, the inside of the air inlet pipes 31 and 32 is filled with precursors, which are converted into steam when heated and transported to the central heating temperature zone to achieve vapor deposition. The transport gas can be hydrogen, oxygen, nitrogen, argon, etc. The air inlet pipes 31 and 32 can selectively output hydrogen, oxygen, nitrogen, argon and other transport gases from the multi-channel gas mixing system and introduce them into the drum-shaped cavity. When the transport gas passes through the heating modules 22 and 23 on both sides, it carries the independently heated precursor molecules to the central heating module 21, and realizes the deposition growth of thin film materials on the sample growth substrate at the central heating module 21.

[0033] See also Figure 1 and Figure 3 The drum-shaped cavity shell 1 is a hollow cylinder with closed two end faces, which includes a cylindrical side structure 11 made of stainless steel and an end face sealing structure (not shown) covering the two end faces of the cylindrical side structure 11 to serve as an X-ray transmission window.

[0034] Figure 3The present invention is a schematic diagram of the operating principle of a drum-type multi-temperature zone vapor deposition growth and in-situ characterization cavity device for in-situ characterization of the growth state of a thin film in the cavity. Among them, the X-rays of the X-ray experimental detection device penetrate from the end face sealing structure on one side of the drum-type cavity shell 1 and exit from the end face sealing structure on the other side. In this embodiment, the X-ray or synchrotron radiation beam is emitted from the light source, and after being collimated by the beam line collimation system, it is irradiated onto the thin film material growing inside the cavity through the end face sealing structure, and the emitted X-rays carrying the diffraction information of the material structure will be emitted through the end face sealing structure on the other side of the cavity, and then captured by the integrated detection system of the X-ray experimental detection device, converted into an electronic signal of signal data, and transmitted to the visualization data analysis system of the X-ray experimental detection device.

[0035] According to the prior art, the X-ray experimental detection device integrated detection system includes X-ray down-conversion elements (scintillator crystals, amorphous silicon or amorphous selenium, etc.), light spot detection sensors (CMOS, CCD or TFT flat panels, etc.), analog-to-digital conversion elements, and corresponding lens groups and signal transmission circuits, etc. The visual data analysis system will analyze the real-time structural information of the material based on the signal data obtained by the integrated detection system, which is helpful to deeply explore the growth mechanism of each material, thereby providing further refined guidance for the corresponding material growth.

[0036] The isoperimetric theorem shows that a circle can achieve the maximum area of ​​all figures under the same circumference limit. Similarly, for stainless steel frames of the same mass, the cylindrical drum structure ensures the maximum X-ray transmission surface, and in X-ray diffraction detection, such a design ensures the maximum detectable diffracted light angle.

[0037] The diameter of the end face sealing structure is greater than the thickness of the drum-shaped cavity represented by the distance between the two end faces of the drum-shaped cavity shell 1, thereby ensuring wide X-ray detection angle coverage. This special structural design enables the cavity to receive multi-dimensional diffraction structure information in real time within a large angle range during the material growth process in the cavity when used in conjunction with a variety of X-ray experimental detection devices, and is suitable for in-situ characterization research on thin film structures and their corresponding growth mechanisms during material preparation. The diameter of the end face sealing structure is such that after the X-rays pass through the end face sealing structure of the drum-shaped cavity shell 1 and hit the central heating module (and the growing sample thereon), the detectable scattered light beam has an upper limit angle of ≥62° with the plane of the sample growth substrate in the vertical direction, and the total left and right divergence angle of the central heating module 21 in the horizontal direction is ≥100°. The above-mentioned wide X-ray detection angle coverage range (vertical direction>62°, horizontal direction>100°) ensures that the cavity can effectively be compatible with a variety of X-ray real-time detection methods such as θ-2θ method X-ray diffraction detection and grazing incidence thin film surface structure characterization, and record material growth information in real time, thereby helping researchers to accurately understand the real-time structural changes and corresponding microscopic growth mechanisms in the process of thin film material preparation inside the cavity, and provide effective guidance for the preparation of higher quality films.

[0038] The end face sealing structure allows X-rays to be transmitted to the central heating module 21, thereby capturing the growth status information of the sample by X-ray diffraction. The material of the end face sealing structure has high heat resistance and high mechanical strength (the material can withstand the conditions of the chamber temperature > 1200°C and the chamber pressure < 1×10 -5 Torr) and high X-ray transmittance (X-ray transmittance>80%), thereby ensuring that the cavity is suitable for high-purity vapor deposition growth of thin film materials in a high vacuum and high temperature environment inside the cavity. In this embodiment, the end face sealing structure is a polyimide (Kapton) film.

[0039] like Figure 1 and Figure 3 As shown, the bottom curved surface of the drum-shaped cavity shell 1 is fastened with a stainless steel base 15 for maintaining the stability of the cavity itself, and at the same time, the experimental sample table 101 of the X-ray experimental detection device below the drum-shaped cavity shell 1 can be connected by a clamp or a bolt fastening device.

[0040] In the present invention, in order to realize X-ray in-situ detection, the sample stage of the six-circle diffractometer can be used as the experimental sample stage 101, and provide the drum-shaped cavity shell 1 with spatial rotational freedom for X-ray diffraction characterization detection, which can realize real-time characterization of the growth state of the thin film material in the drum-shaped cavity shell 1. In order to ensure the display degree of the operation diagram, the experimental sample stage 101 with rotational freedom is drawn as a substitute for the six-circle diffractometer. In other embodiments, the experimental sample stage 101 can be replaced by a sample stage of other X-ray experimental detection devices, which is suitable for in-situ characterization research of its performance during the material preparation process.

[0041] In order to install the drum-shaped cavity shell 1 on the six-circle diffractometer, the total weight of the drum-shaped cavity shell 1 and its accessories is required to be less than 6 kg. The specific size depends on the size of different diffractometers and is not strictly required. Generally speaking, the radius of the end face (i.e., the bottom face of the cylinder) of the drum-shaped cavity shell 1 is ≤20 cm, and the end face spacing (i.e., the height of the cylinder) is ≤25 cm.

[0042] like Figure 1 , Figure 4 and Figure 5 As shown, the interior of the drum-shaped cavity shell 1 can be equipped with three independent heating modules arranged in a horizontal straight line: a central heating module 21 in the form of a platform and two side heating modules 22, 23 in the form of heating sleeves. The three heating modules 21, 22, 23 are distributed along a horizontal straight line on the cavity support platform 24, and the direction of the horizontal straight line is parallel to the connection direction of the air inlet pipes 31, 32 on both sides. The central heating module 21 can be used to provide sample growth temperature and is the core area of ​​material growth; the two side heating modules 22, 23 can be used to respectively control the temperature and distribution of precursor vapors of different components to further optimize the reaction environment during material growth.

[0043] The three heating modules 21, 22, and 23 are all heated by electric heating, and the heating materials used by the heating modules 21, 22, and 23 can be nickel-chromium or iron-chromium-aluminum alloys, refractory metals (molybdenum, platinum, tungsten, etc.) or non-metallic graphite fibers, etc. Among them, for the central heating module 21, the central heating module can adopt a circular or rectangular platform mode, and the heating material is in the form of a sheet and directly located at the bottom of the platform, which can provide the highest heating temperature upper limit for the material growth substrate, thereby ensuring the main temperature conditions for sample growth; for the heating modules 22 and 23 on both sides, the heating materials can be arranged in the form of electric heating wires on the inner side of the heating sleeve.

[0044] like Figure 4 and Figure 6As shown, the central heating module 21 is configured to place the material growth substrate 213, and through its own temperature control, provides environmental conditions that facilitate the deposition of the sample molecules after the reaction on the material growth substrate 213 and the growth of the film. The central heating module 21 is located at the center of the drum-shaped cavity shell 1. The central heating module 21 can be installed with the corresponding material growth substrate 213 according to the growth requirements of the specific material, and can be heated to a maximum of 1150°C for the growth of thin film materials.

[0045] A fastening device is installed on the side of the central heating module 21 to fix the material growth substrate 213, so as to avoid the large-angle rotation of the cavity during the in-situ multi-dimensional detection process, which may cause the position of the material growth substrate 213 to shift and affect the detection accuracy. In this embodiment, the fastening device is a small ceramic fixture 212 arranged on the side of the heating platform.

[0046] In order to prevent the heat radiated from the central heating module 21 from affecting the temperature control of the heating platforms on both sides, a heat shielding material coating layer 211 is provided on the side of the central heating module 21 to prevent the heat radiated from the central high-temperature heating platform from affecting the temperature control of the heating platforms on both sides, thereby ensuring that the three heating modules are independently adjustable from each other. In this embodiment, the heat shielding material is specifically silicon oxide.

[0047] The heating modules 22 and 23 on both sides adopt heating sleeves, and the heating modules 22 and 23 on both sides are respectively sleeved on the outside of the corresponding air inlet pipes. Among them, the centers of the three heating modules 21, 22, and 23 are in the same straight line, and the air inlet pipes 31 and 32 are parallel to the straight line where the centers of the three heating modules are located and are at the same height as the heating sleeves, and are respectively inserted into the interior of the drum-shaped cavity shell 1 through the air inlets 131 and 132, and inserted into the heating sleeves of the heating modules 22 and 23 on both sides, so that the air inlet pipe is in the center position of the heating sleeve and is evenly heated, effectively transporting the heated volatilized precursor molecules to the central heating platform, and realizing independent and adjustable heating of precursors of different components. Preferably, the air inlet pipes 31 and 32 match the inner diameter of the heating sleeves and are fastened to the heating sleeves so that they can move with the heating sleeves.

[0048] The bottom of the heating modules 22 and 23 on both sides are respectively provided with translation components 221 and 231, which are used to drive the heating modules 22 and 23 on both sides and the air intake pipes 31 and 32 with the precursor placed inside to approach or move away from the central heating module 21. The heating modules 22 and 23 on both sides are directly fixed on the translation components 221 and 231, and the connection method can be bolts, buckles, etc. The translation components 221 and 231 can be manually adjusted or driven by high-precision servo motors, and are fixed on the intracavity support platform 24; by using manual or high-precision servo motors as power sources, accurate and controllable horizontal linear motion can be provided.

[0049] The functions of the translation components 221 and 231 are as follows: 1. If the temperature of the central heating zone is too high relative to the heating zones on both sides, the translation component can drive the heating sleeves on both sides away to avoid the influence of thermal radiation that may leak from the central heating platform; 2. In the initial stage of the precursor being converted into steam by heating in the air inlet pipes on both sides, there will be an imbalance in the steam concentration gradient in the pipes, which will affect the quality of sample growth. According to the real-time temperature and steam concentration data, the position of the translation components 221 and 231 can be adjusted to control the transmission distance of the precursor steam in the pipe, ensuring that the precursor steam is in a state of balanced concentration when it is fed into the central heating zone. This dynamic adjustment helps to achieve a more uniform precursor supply, thereby optimizing the uniformity and overall quality of the prepared thin film material.

[0050] In this embodiment, each heating module 21, 22, 23 is equipped with an independent temperature sensor for real-time monitoring of the temperature of the corresponding heating module, and the sensor is connected to the driver of each heating module, so as to interact through a negative feedback mechanism. The above-mentioned fine feedback adjustment device design ensures that the temperature control accuracy of each temperature zone can be within 1°C. This fine temperature control is the key to achieving high-quality growth of deposited thin films. In this embodiment, the maximum heating temperature of the heating modules 22 and 23 on both sides can reach 950°C respectively.

[0051] In addition to temperature sensors, sensors can also include pressure sensors. Therefore, during the real-time growth process of the material, the sensor detects the temperature, pressure and other intra-cavity indicators of each heating module in real time and transmits the data to the computer for analysis. The specific operation instructions are transmitted to the heating module and translation motor inside the cavity through the heating module control program and the sleeve translation driver program on the computer side (such as the visual data analysis system of the X-ray experimental detection device) to accurately control the growth environment of the thin film material inside the cavity and ensure the growth of high-quality thin films.

[0052] Therefore, during the sample vapor deposition preparation process, different precursors are arranged inside the air intake pipes 31 and 32 on the left and right sides, and each generates gas molecules at different heating temperatures through the heating sleeves of the heating modules 22 and 23 on both sides and is transmitted to the central heating module 21 via the transport gas in the air intake pipe. The special layout design of the central heating module 21, the heating modules 22 and 23 on both sides and the air intake pipes 31 and 32 ensures that the steam can be evenly transported from the air intake pipes 31 and 32 on both sides to the material growth substrate 213. At the same time, by adjusting the translation components 221 and 231 of the heating modules 22 and 23 on both sides, the stability of the material growth environment inside the cavity is ensured, and the distribution of the precursor vapor is further optimized.

[0053] Specifically, different precursor materials have different effects on the growth of semiconductor materials. By simultaneously introducing multiple precursor materials and mixing them in the central heating module 21, precise control of the growth conditions can be achieved. This control can adjust key parameters such as the composition, structure, and thickness of the film, thereby optimizing the performance of the material. When multiple precursor materials are mixed from both sides under different heating conditions, they can fully contact and interact with each other, thereby helping to form a uniform and high-quality film on the material growth substrate 213. Compared to introducing precursor materials separately, introducing multiple precursor materials at the same time helps to simplify the operation process, reduce the time for equipment switching and cleaning, improve production efficiency, and reduce production costs. At the same time, the independently controlled heating modules on both sides can meet the heating requirements of precursor materials with different boiling points. On the one hand, the precise temperature control of the heating modules on both sides can effectively control the thermal evaporation rate of the precursor, thereby adjusting the flow of precursor gas molecules into the central heating module, and accurately controlling the concentration of each precursor component during the material growth process to avoid defects in crystal growth; on the other hand, it avoids the physical quenching of high-temperature precursor vapor by low-temperature precursor vapor before the precursor vapor reaches the heating material growth substrate 213 in the central temperature zone, thereby ensuring the purity and crystallinity of the grown sample.

[0054] like Figure 1 and Figure 7 As shown, the top of the drum-shaped cavity housing 1 is provided with a quartz observation window 12. The quartz observation window 12 has high transmittance to visible light.

[0055] In order to ensure the accuracy of X-ray in-situ detection, the quartz observation window 12 on the top of the drum-shaped cavity can use visible light to achieve leveling of the material growth substrate 213 before the experiment. At the same time, the quartz observation window 12 provides visualization of the internal environment of the cavity during the thin film material growth preparation process, which is convenient for the operator to observe the growth of the corresponding material on the material growth substrate 213 and the vapor state of the precursor in real time during the experiment. Specifically, before the vapor deposition thin film material growth step begins, the operator can inject the collimated laser into the cavity through the quartz observation window 12, and use the material growth substrate 213 to reflect the collimated laser, transmit the reflected collimated laser to the correction plane outside the cavity through the quartz observation window 12, adjust the plane rotation angle of the material growth substrate 213, correct the position of the reflected light spot, and when the reflected light spot coincides with the preset calibration point on the correction plane, it is considered that the leveling is achieved, thereby achieving optical leveling of the material growth substrate 213 in the cavity, avoiding the adverse effects of dynamic factors such as airflow inclination angle and gravity effect on thin film growth preparation.

[0056] In addition, the side of the drum-shaped cavity shell 1 is provided with multifunctional flange interfaces 141, 142, 143, 144, which can be used as exhaust ports, water cooling pipe interfaces and other functions. Among them, the air inlet, exhaust port and multifunctional flange interface can all be sealed. The outlet pipe can be set at the multifunctional flange interfaces 141, 142, 143, 144. This design ensures the smooth discharge of residual gas after participating in the growth process, avoids excessive internal pressure and gas residue, and maintains environmental stability during the vapor deposition process.

[0057] The cavity of the drum-shaped cavity shell 1 is connected to a water cooling device, which is used to reduce the heat radiation of the non-heating area, thereby improving the temperature control accuracy of each heating module, extending the service life of the material of the stainless steel frame and the end face sealing structure, and being compatible with the integrated equipment outside the cavity. In this embodiment, the housing of the water cooling device is installed outside the cavity, and the cooling water is input and output from the cavity of the drum-shaped cavity shell 1 through the transmission pipeline of the water cooling device. The transmission pipeline of the water cooling device can be connected to the cavity of the drum-shaped cavity shell 1 through the multifunctional flange interfaces 141, 142, 143, 144.

[0058] A drum-shaped multi-temperature zone vapor deposition growth and in-situ characterization cavity device of the present invention adopts a drum-shaped cavity structure design. According to the isoperimetric theorem, compared with other cavity shapes, the vapor deposition cavity is designed as a drum-shaped cavity structure to ensure the maximization of the cavity space under the same cavity shell mass, thereby ensuring the compact integration of the vapor deposition cavity and ensuring the tolerance of the cavity to high vacuum. The lightweight and compact characteristics brought by the drum-shaped design enable the cavity to be integrated into various X-ray experimental detection devices using a stainless steel base. The special structural design enables the front and rear side X-ray transmission window end face sealing structure to cover a wide range of X-ray detection angles, thereby effectively ensuring the real-time and effective extraction of multi-dimensional diffraction information during the growth and preparation of thin film materials in the cavity. In addition, the high vacuum environment that can be achieved by the drum-shaped cavity structure is indispensable for achieving extremely high purity and precise control of the deposition process, and is particularly important for various semiconductor devices that require extremely high-quality thin film materials.

[0059] The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device of the present invention adopts a dual air inlet pipe design, allowing different precursors to be introduced into the chamber through different heating channels and to be temperature-modulated by different heating modules. The independent temperature zone design allows each heating module to perform fine temperature control, thereby effectively avoiding the quenching phenomenon caused by the temperature difference between precursors that is common in traditional technologies, and ensuring the flatness and uniformity of the film during the growth process. This precise control not only improves the crystallization integrity of the material, but also optimizes the electrical and mechanical properties of the film, significantly improves the quality of film growth in the chamber, and is of great significance to improving the reliability and performance of the final product. Using the in-situ characterization information during the growth process, the operator can read various microscopic growth mechanisms of the corresponding thin film material, thereby providing accurate guidance for the high-quality growth of the thin film material inside the cavity.

[0060] In addition, the side heating module in the device of the present invention adopts a translation component, which optimizes the precursor vapor distribution by finely adjusting the specific position of the heating module, enhances the controllability of the growth environment during the vapor deposition process, and can further improve the overall quality of thin film growth; by dynamically adjusting the heating module, the supply of precursor can be adjusted according to real-time monitoring data to achieve the optimal vapor distribution state, thereby ensuring the environmental stability during the thin film growth process in the cavity and improving the growth quality and efficiency of thin film materials.

[0061] In summary, the drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device of the present invention improves the growth quality of two-dimensional semiconductor thin films through a unique drum-type chamber design and independent and precise control of multiple heating modules, and meets the needs of in-situ observation of thin film growth structure and mechanism under different working conditions, thereby gaining an in-depth understanding of the growth mechanism of thin film materials and providing guidance for the preparation of higher quality two-dimensional semiconductor thin films. This device can achieve real-time characterization of the material growth process in a vacuum and high temperature environment, and is suitable for the preparation and performance research of high-quality thin film materials.

[0062] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device, characterized in that: It includes a drum-shaped cavity shell installed on an X-ray experimental detection device, a plurality of air inlet pipes inserted into the drum-shaped cavity shell, a central heating module in the form of a platform arranged inside the drum-shaped cavity shell, and two side heating modules in the form of heating sleeves, and an experimental sample table arranged below the drum-shaped cavity shell; the central heating module is provided with a sample growth substrate, each air inlet pipe is respectively connected to the corresponding two side heating modules, and different air inlet pipes are used to introduce different precursors and transport gases.

2. The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to claim 1, characterized in that: The drum-shaped cavity shell is a hollow cylinder with closed end faces, and comprises a cylindrical side structure and an end face sealing structure covering the end faces of the cylindrical side structure to serve as X-ray transmission windows.

3. The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to claim 2, characterized in that: The diameter of the end face sealing structure is greater than the distance between the end faces on both sides of the drum-shaped cavity shell.

4. The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to claim 1, characterized in that: The cylindrical side structure is made of stainless steel, and the material of the end face sealing structure can withstand the conditions of an inner cavity temperature of >1200°C and an inner cavity pressure of <1×10 -5 Torr, and its X-ray transmittance is >80%.

5. The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to claim 1, characterized in that: A stainless steel base is fastened to the bottom of the drum-shaped cavity shell, and is connected to the experimental sample table of the X-ray experimental detection device through a clamp or a bolt fastening device.

6. The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to claim 1, characterized in that: The air inlet pipe matches the inner diameter of the heating sleeve and is fastened to the heating sleeve; the bottoms of the heating modules on both sides are respectively provided with translation components.

7. The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to claim 1, characterized in that: The central heating module and the heating modules on both sides are equipped with independent temperature sensors.

8. The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to claim 1, characterized in that: A quartz observation window is provided on the top of the drum-shaped cavity shell, and the observation window is transparent to visible light; and / or An air inlet for an air inlet pipe to pass through and a multifunctional flange interface are arranged on the side of the drum-shaped cavity shell, and the multifunctional flange interface includes an exhaust port.

9. The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to claim 1, characterized in that: The cavity of the drum-shaped cavity shell is communicated with a water cooling device.

10. The drum-type multi-temperature zone vapor deposition growth and in-situ characterization chamber device according to claim 1, characterized in that: A fastening device is installed on the side of the central heating module for fixing the sample growth substrate; and / or a heat shielding material coating layer is provided on the side of the central heating module.

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