A growth system of two-dimensional semiconductor and a growth method thereof

Abstract

The application provides a growth system of two-dimensional semiconductor and a growth method thereof, and the growth system comprises a high-temperature tube furnace, a solid source movable sealing disc, an air extraction sealing disc, a quartz tube supporting bracket, a supporting frame and a gas path panel. The application relates to a novel chemical vapor deposition system for growing 8-inch wafer scale two-dimensional transition metal chalcogenide semiconductor materials, the device is provided with multiple gaseous and solid sources in the upstream, and the opening and closing of each source and the component proportion of the carrier gas can be independently controlled, the device solves the neck problem of poor thin film uniformity in large-area thin film growth, breaks through the technical bottleneck of controllable growth of large-area layers, realizes the 8-inch uniform growth of molybdenum disulfide and the layer-by-layer epitaxial growth of a homostructure of a multilayer two-dimensional transition metal chalcogenide, and provides a technical basis for the large-scale application of wafer-level two-dimensional semiconductor materials on devices.

Description

Technical Field

[0001] This invention belongs to the field of novel low-dimensional semiconductor material preparation, specifically relating to a growth system and method for a two-dimensional semiconductor. Background Technology

[0002] For the semiconductor industry, materials and equipment are the cornerstones, the engines driving the continuous development of integrated circuits. Wafer manufacturing is a crucial link in the semiconductor industry, and semiconductor wafer sizes (measured by diameter) mainly include 4 inches and below, 6 inches, 8 inches, and 12 inches. The larger the diameter of a semiconductor wafer, the more chips can be manufactured on a single wafer, thus reducing the cost per chip. For this reason, semiconductor wafers are continuously developing towards larger sizes. Two-dimensional semiconductor materials, represented by transition metal chalcogenides, are promising new electronic materials in the post-Moore's Law era, and are expected to achieve breakthroughs in applications such as novel optoelectronics, information devices, and flexible electronics. Currently, the mainstream methods for synthesizing two-dimensional semiconductor materials include chemical vapor deposition (CVD), molecular beam epitaxy (MBE), and atomic layer deposition (ALD). CVD mainly includes metal-organic chemical vapor deposition (MOCVD) and thermochemical vapor deposition (CVD). MOCVD (Metal-Organic Chemical Vapor Deposition) is a chemical vapor deposition system that uses a gaseous source as a precursor. Compared to other methods, it has several advantages, making it the most common method for growing wafer-level two-dimensional semiconductor materials: 1) Its growth rate is stable and tunable. 2) By controlling the composition of the gas path, the composition and doping properties of the epitaxial layer can be precisely controlled. 3) It offers high throughput, stable conditions, and well-controlled wafer uniformity. These advantages make MOCVD stand out as a strong candidate for two-dimensional semiconductor epitaxial systems. Currently, MOCVD is mainly used for the large-scale production of III-V group compounds, while its application in the preparation of two-dimensional semiconductor materials is still in the laboratory research stage. Most reported work involves wafers of 4 inches or smaller, and the epitaxial films are mostly composed of polycrystalline materials with disordered grain orientation, resulting in numerous grain boundaries. The most significant problem is that the unavoidable carbon deposition contamination from the metal-organic source makes it difficult to meet the quality requirements of large-area integrated devices. Furthermore, the high cost and complex maintenance of this equipment also limit its development to some extent.

[0003] Thermochemical vapor deposition (CVD) is a chemical vapor deposition system that uses a solid-state source as a precursor. This type of equipment is inexpensive and cost-effective, making it a commonly used system for nanomaterial growth. Current laboratory research shows that CVD can achieve the growth of highly oriented two-dimensional semiconductor materials through substrate and van der Waals epitaxy. Because crystal orientation is controllable, the impact of grain boundaries on carrier mobility is greatly reduced; moreover, the solid-state source is relatively stable and does not pose a carbon contamination problem. Therefore, this growth system shows potential for growing high-quality continuous molybdenum disulfide (MoD) films. However, during the growth of high-quality wafer-level MoD films using CVD, the uneven distribution of source concentration and temperature field can easily create growth gradients, resulting in inhomogeneities in different regions of the final wafer. This significantly hinders the application of wafer-level MoD films in large-scale integrated circuits.

[0004] Currently, the wafer fabrication of two-dimensional semiconductor materials still faces the following challenges: 1. How to achieve large-grain, single-orientation two-dimensional semiconductor materials. 2. How to ensure the uniformity of the thin film. 3. How to control the number of thin film layers. 4. How to achieve equipment versatility. Summary of the Invention

[0005] Therefore, the purpose of this invention is to overcome the deficiencies in the prior art and provide a two-dimensional semiconductor growth system and method thereof. Compared with similar equipment, the growth system of this invention has a novel equipment structure and function.

[0006] Before describing the content of this invention, the following terms are defined as follows:

[0007] The term "high-purity quartz" refers to quartz with a purity of 99.9% and a long-term operating temperature of 1100-1200℃.

[0008] The term "CVD" refers to thermochemical vapor deposition.

[0009] To achieve the above objectives, a first aspect of the present invention provides a two-dimensional semiconductor growth system, the growth system comprising: a high-temperature tube furnace, a solid-state source movable sealing plate, a vacuum sealing plate, a quartz tube support, a support frame, and a gas path panel; wherein the solid-state source movable sealing plate comprises: a vacuum gauge, a sealing plate, a parallel plate, a corrugated pipe, and an inlet pipe;

[0010] Preferably, the wafer size of the two-dimensional semiconductor is 2 to 8 inches, more preferably 4 to 8 inches, and most preferably 8 inches; and / or

[0011] Preferably, the material of the two-dimensional semiconductor is selected from one or more of the following: transition metal sulfides, transition metal selenides, transition metal tellurides, and more preferably molybdenum disulfide, tungsten disulfide, tungsten diselenide, and molybdenum diselenide.

[0012] According to the first aspect of the present invention, a two-dimensional semiconductor growth system is provided, wherein,

[0013] The high-temperature tube furnace is a resistance-type high-temperature tube furnace with three heating zones and temperature control, comprising: a furnace body, a main cavity quartz tube, and a heat insulation plate; wherein...

[0014] The furnace body is a hinged, upper and lower type, with each part including an insulation layer and a heating zone. The insulation layer comprises a first insulation layer, a second insulation layer, a third insulation layer, and a fourth insulation layer. The heating zone comprises a first heating zone, a second heating zone, and a third heating zone. The first insulation layer is preferably located at the edge of the furnace body, with a thickness of 20–40 mm, more preferably 25–35 mm. The second insulation layer is preferably located between the first and second heating zones, with a thickness of 500–700 mm, more preferably 550–650 mm. The third insulation layer is preferably located between the second and third heating zones, with a thickness of 100–200 mm, more preferably 120–160 mm. The fourth insulation layer is preferably located at the edge of the third heating zone, with a thickness of 60–120 mm, more preferably 80–100 mm.

[0015] The main cavity quartz tube has flanges on both sides and a quartz sand core plate in the middle, with the end faces of the flanges mirror-polished; the number of quartz sand core plates is preferably 1 to 5, more preferably 1 to 3, and even more preferably 2; the material of the main cavity quartz tube is preferably high-purity quartz; and / or the operating temperature of the main cavity quartz tube is preferably 1100℃ to 1200℃, most preferably 1200℃; and / or

[0016] The heat insulation plate includes a first heat insulation plate and a second heat insulation plate; wherein, the first heat insulation plate is located between the first heating zone and the second heating zone, and the second heat insulation plate is located outside the third heating zone; the material of the heat insulation plate is preferably ceramic, and the ceramic is more preferably one or more of the following: alumina ceramic, zirconium oxide ceramic, silicon carbide ceramic, and more preferably alumina ceramic and zirconium oxide ceramic;

[0017] Preferably, the first heating zone is located between the first insulation layer and the second insulation layer, and its length is more preferably 500-700 mm, and even more preferably 550-650 mm; and / or the temperature is more preferably 120°C-150°C, and even more preferably 130°C-150°C.

[0018] Preferably, the second heating zone is located between the second and third insulation layers and heats the metal source; the length is more preferably 500-700 mm, and even more preferably 550-650 mm; and / or the temperature is more preferably 500°C-600°C, and even more preferably 550°C-600°C.

[0019] Preferably, the third heating zone is located between the third insulation layer and the fourth insulation layer, and its length is more preferably 800-1200 mm, and even more preferably 950-1100 mm; and / or its temperature is more preferably 900℃-950℃, and even more preferably 900℃-930℃.

[0020] Preferably, the quartz sand core plate has a porous microstructure; and / or

[0021] Preferably, the first heat insulation plate includes a ceramic plate, a ceramic connecting pipe and a ceramic bolt, and the second heat insulation plate is a ceramic plate with multiple through holes; the type of holes in the ceramic plate of the first heat insulation plate is more preferably selected from one or more of the following: bolt holes, vent holes, and air-proof holes; and / or the thickness of the second heat insulation plate is more preferably 20% to 60% of its diameter, and even more preferably 25% to 50%.

[0022] According to the two-dimensional semiconductor growth system of the first aspect of the present invention, the solid-state source movable sealing plate further includes: a longitudinally moving base, a transverse linear module, a first sealing plate, a vacuum gauge, a bellows parallel plate, a butterfly vacuum bellows, a central composite air inlet pipe, a high-temperature source air inlet pipe, a first sealing plate support leg, a bellows parallel plate support leg, a second sealing plate, and a second sealing plate support leg; and the air inlet type of the solid-state source movable sealing plate is selected from one or more of the following: high-temperature source air inlet, main cavity air inlet, and low-temperature source air inlet; wherein:

[0023] Preferably, the central composite air intake pipe is for main cavity air intake and / or low temperature source air intake; the central composite air intake pipe is preferably located at the center of the solid source movable sealing plate; and / or the axis of the central composite air intake pipe is preferably the same as the axis of the main cavity quartz tube.

[0024] Preferably, the high-temperature source air inlet pipe is a high-temperature source air inlet; the high-temperature source air inlet pipe is preferably arranged on the circumference of the solid source movable sealing plate; the number of high-temperature source air inlet pipes is preferably 4 to 12, more preferably 4 to 10; and / or the distance from the high-temperature source air inlet pipe to the center of the solid source movable sealing plate is preferably 60 to 80 mm, more preferably 70 to 80 mm, and most preferably 75 mm;

[0025] Preferably, the vacuum gauge is mounted on the first sealing plate; most preferably, it is a thin-film gauge; and / or

[0026] Preferably, the front of the bellows parallel plate includes a front hole and a connecting hole for the support leg, and the side includes a side hole. The front hole of the bellows parallel plate is preferably used to mount the support piece of the butterfly vacuum bellows, and the front hole is perpendicular to the axis of the front hole. And / or a set screw is installed on the front hole of the bellows parallel plate to connect the bellows parallel plate and the butterfly vacuum bellows.

[0027] According to the first aspect of the present invention, a two-dimensional semiconductor growth system is provided, wherein,

[0028] The longitudinal moving base includes: a first slider of the longitudinal moving base, a base plate of the longitudinal moving base, a linear guide rail of the longitudinal moving base, and a second slider of the longitudinal moving base.

[0029] The transverse linear module includes: a linear module base plate, a lead screw assembly, a transverse linear module linear guide rail, a transverse linear module first slider, a transverse linear module first slider adapter seat, a transverse linear module second slider, and a transverse linear module second slider adapter seat;

[0030] The front side of the first sealing plate includes: a sealing groove for the first sealing plate, a central air inlet hole for the first sealing plate, an outer ring air inlet hole for the first sealing plate, and a vacuum gauge connection hole; and / or the back side of the first sealing plate includes: a threaded hole for the outer ring air inlet hole for the first sealing plate, a threaded hole for the central air inlet hole for the first sealing plate, and a locking hole for the support leg of the first sealing plate.

[0031] The butterfly vacuum bellows includes: a second sealing flange for the butterfly vacuum bellows, a bellows telescopic unit, a telescopic unit connecting plate, and a first sealing flange for the butterfly vacuum bellows.

[0032] The central composite air inlet pipe includes: a central composite air inlet pipe flange cavity, a quartz tube holder, a first vacuum connector, a second vacuum connector, and a low-temperature solid-state source quartz tube;

[0033] The high-temperature sample inlet tube includes: a quartz tube holder, an extension tube, and a high-temperature solid-state source quartz tube; and / or

[0034] The second sealing plate includes: a main plate, a shaped sealing ring, a secondary plate, a vacuum connector, and a sealing ring for the high-temperature sample inlet pipe; wherein:

[0035] Preferably, the second slider of the longitudinal moving base is connected to the connecting transverse linear module; the base plate of the transverse linear module is connected to the longitudinal moving base; the first slider adapter is connected to the second sealing plate support leg; the second slider adapter is connected to the bellows parallel plate; the threaded hole of the outer ring air inlet of the first sealing plate is connected to the butterfly vacuum bellows; the threaded hole of the center air inlet of the first sealing plate is connected to the center composite air inlet pipe; the locking hole of the first sealing plate support leg is connected to the first sealing plate support leg; the second sealing flange of the butterfly vacuum bellows is sealed to the second vacuum sealing plate; the first sealing flange of the butterfly vacuum bellows is sealed to the first vacuum sealing plate; and / or the vacuum connector of the second sealing plate is connected to the gas path panel through a vacuum pipe.

[0036] According to the first aspect of the present invention, a two-dimensional semiconductor growth system is provided, wherein,

[0037] The quartz tube holder is vacuum-sealed with the central composite inlet flange cavity; the quartz tube holder preferably includes: a quartz tube holder main tube, a polytetrafluoroethylene fastening tube, a compression tube, a compression tube sealing ring on the side, a quartz tube sealing ring, a movable compression tube, and a compression nut.

[0038] The side of the central composite air inlet flange cavity is a first vacuum connector; and / or

[0039] The front end of the quartz tube holder is connected to the main cavity quartz tube, and its rear end is sealed to the second vacuum connector; wherein:

[0040] Preferably, the bottom of the main tube of the quartz tube holder has a through hole, and the other end has an external thread. Its inner wall and the inner side of the bottom surface have a chamfer. The angle of the chamfer is preferably 45° to 70°, more preferably 50° to 65°, and most preferably 60°.

[0041] Preferably, the polytetrafluoroethylene (PTFE) fastening tube includes a first PTFE fastening tube and a second PTFE fastening tube;

[0042] Preferably, the extrusion tube includes a first extrusion tube and a second extrusion tube;

[0043] Preferably, the side of the first extrusion tube has a sealing ring mounting groove, one end of which has a raised blade in the middle and the other end has a chamfer. The angle of the chamfer is preferably 10° to 60°, more preferably 20° to 50°, and most preferably 30°.

[0044] Preferably, the structure of the second extrusion tube is the same as that of the first extrusion tube, but the installation direction is opposite;

[0045] Preferably, a quartz tube sealing ring is provided between the first extrusion tube and the second extrusion tube, and the quartz tube sealing ring is in chamfer contact with the first extrusion tube and the second extrusion tube; and / or

[0046] Preferably, the structure of the second PTFE fastening tube is the same as that of the first PTFE fastening tube, but the installation direction is opposite.

[0047] According to the first aspect of the present invention, a two-dimensional semiconductor growth system is provided, wherein,

[0048] The front side of the second sealing plate main board has four sets of holes: the first threaded blind hole of the second sealing plate main board, the second threaded blind hole of the second sealing plate main board, the threaded through hole of the second sealing plate main board, and the first sealing groove of the second sealing plate main board.

[0049] The back of the second sealing plate main board has a circular groove on the back of the second sealing plate main board, a second sealing groove on the second sealing plate main board, and a third threaded blind hole on the second sealing plate main board;

[0050] The second sealing plate main board is sealed to the second sealing plate secondary board via the irregularly shaped sealing ring; and / or

[0051] The second sealing plate vacuum connector is connected to the gas path panel via the vacuum pipe; wherein:

[0052] Preferably, the first threaded blind hole of the second sealing plate main board is connected to the support leg of the second sealing plate, the second threaded blind hole of the second sealing plate main board is connected to the butterfly vacuum bellows, the threaded through hole of the second sealing plate main board is connected to the high-temperature sample inlet pipe, and after the high-temperature sample inlet pipe sealing ring is installed in the first sealing groove of the second sealing plate main board, the high-temperature sample inlet pipe is sealed to the second sealing plate main board; and / or

[0053] Preferably, the second sealing plate secondary plate is positioned and installed in the circular groove on the back of the second sealing plate main plate, and a special-shaped sealing ring is installed in the second sealing groove of the second sealing plate main plate; the third threaded blind hole of the second sealing plate main plate is connected to the second sealing plate secondary plate.

[0054] According to the first aspect of the present invention, a two-dimensional semiconductor growth system is provided, wherein,

[0055] The suction end sealing plate includes: a suction end sealing plate, a suction end sealing plate support leg, a suction end sealing plate longitudinal slider, a suction end sealing plate longitudinal linear guide rail, a suction end sealing plate base plate, and a suction end sealing plate transverse slider; wherein, the suction end sealing plate is connected to a vacuum pump via a vacuum bellows, and its back is connected to the suction end sealing plate support leg; the suction end sealing plate support leg is connected to the suction end sealing plate longitudinal slider, the suction end sealing plate longitudinal slider is mounted on the suction end sealing plate longitudinal linear guide rail, and the suction end sealing plate longitudinal linear guide rail is connected to the suction end sealing plate base plate;

[0056] The quartz tube support includes: a support plate, an optical axis, an optical axis fixing seat, a quartz tube support drag plate, and a quartz tube support drag block; wherein, the optical axis is fixed on the support plate, the quartz tube support drag block and the optical axis fixing seat are fixed on the quartz tube support drag plate, and the quartz tube support drag plate is fixed on the support frame;

[0057] The support frame includes wheels, linear guide rails, sliders, and door panels; wherein the wheels are movably located at the bottom, the linear guide rails are located at the top center, the sliders are located on the linear guide rails, and the door panels are located on the left, right, rear, and top sides of the support frame and are openable and closable; and / or

[0058] The gas path panel includes mass flow meters, valves, pipe fittings, stainless steel pipe assemblies, and a mounting plate; wherein the mass flow meters are, in sequence, a first mass flow meter, a second mass flow meter, a third mass flow meter, a fourth mass flow meter, and a fifth mass flow meter, and the valves are a first valve, a second valve, and a third valve; wherein:

[0059] Preferably, the material of the support frame is selected from one or more of the following: aluminum profile support, welded square tube support, optical platform, preferably aluminum profile support or optical platform;

[0060] Preferably, the door panel is made of one or more of the following materials: iron plate, stainless steel plate, acrylic plate, and aluminum plate;

[0061] Preferably, the pipe fitting and the stainless steel pipe assembly connect the mass flow meter and the valve; and / or

[0062] Preferably, the air passage panel is mounted on the support frame.

[0063] According to a first aspect of the present invention, a two-dimensional semiconductor growth system further includes: a vacuum pump, an exhaust gas treatment system, and a control host; wherein,

[0064] The vacuum pump is a corrosion-resistant oil-sealed rotary vane pump or a dry scroll pump, most preferably a corrosion-resistant oil-sealed rotary vane pump; and / or

[0065] The exhaust gas treatment system is an alkaline solution tank, and the alkaline solution is selected from one or more of the following: NaOH solution, KOH solution, and NaHCO3 solution.

[0066] A second aspect of the present invention provides a method for growing a two-dimensional semiconductor, the method using the growth system described in the first aspect, and comprising the following steps:

[0067] (1) Pre-treat the substrate by placing the pre-treated substrate in the third heating zone;

[0068] (2) Place the solid source in the first heating zone, place the metal source at the front end of the quartz tube, introduce the carrier gas, and raise the temperature;

[0069] (3) After the temperatures of the three zones stabilize, the metal source is moved to the second heating zone for growth to obtain the first two-dimensional semiconductor layer. The carrier gas supply is stopped, and the first two-dimensional semiconductor layer is moved to the first heating zone; and

[0070] (4) Heat the material until it stabilizes, then introduce a carrier gas to move the first layer of the two-dimensional semiconductor back to the second heating zone for growth. After cooling to room temperature, the two-dimensional semiconductor is obtained; wherein:

[0071] Preferably, in step (1), after pretreating the substrate, the method further includes: placing the annealed substrate on a tray, and placing the tray containing the sapphire substrate in a third heating zone. The substrate is preferably selected from one or more of the following: sapphire, silicon, silicon dioxide, quartz, mica, silicon carbide; and / or

[0072] Preferably, step (2) further includes pressing the metal source into a sheet and placing it at the front end of a quartz tube evenly distributed around it, ensuring that it is far away from the second heating zone; the amount of the solid source is preferably 8-12g, more preferably 9-11g, and even more preferably 10g; and / or the amount of the metal source is preferably 40-60mg, more preferably 45-55mg, and even more preferably 50mg.

[0073] According to the method of the second aspect of the present invention, wherein,

[0074] In step (3), the carrier gases in the first heating zone, the second heating zone, and the third heating zone are different; and / or

[0075] In step (3), the time for moving the metal source to the second heating zone for growth is 25-50 minutes, preferably 25-45 minutes, more preferably 30-40 minutes; and / or

[0076] In step (4), the time for moving the first layer of two-dimensional semiconductor to the second heating zone for growth is 35 to 70 minutes, preferably 30 to 65 minutes, and more preferably 40 to 60 minutes.

[0077] According to a specific embodiment of the present invention, the present invention mainly provides a low-cost growth apparatus for 8-inch two-dimensional semiconductor molybdenum disulfide, which is easy to maintain and use. Addressing the issue of large-area uniformity, there are two main reasons for large-area non-uniformity in chemical vapor deposition (CVD): firstly, the spatial non-uniformity of the source concentration in the gas phase, especially for growth using solid-state sources; secondly, when the wafer size is large, the temperature is prone to uneven distribution in different areas of the wafer, resulting in different growth temperatures in different regions. Therefore, it is necessary to ensure uniform and stable temperature within the growth heating zone. Since the substrate may be placed at different angles and in different ways during growth, the sample tray requires multiple functions. Furthermore, since different sources are needed at different stages of growth, independent control of different sources and independent control of the source carrier gas composition are required. The main technical design concept is as follows:

[0078] This invention describes a novel chemical vapor deposition system for growing 8-inch wafer-scale two-dimensional transition metal sulfide compound semiconductor materials. The system comprises the following components: a high-temperature tube furnace, a solid-state source movable sealing plate, a evacuation sealing plate, a quartz tube support, a support frame, a gas path panel, a vacuum pump, an exhaust gas treatment system, and a control unit. Specific details will be described in detail in the embodiments. The core design is as follows:

[0079] 1. The heating system is a resistance-type high-temperature tube furnace with three heating zones of varying lengths and precise temperature control, enabling separate heating of multiple solid-state sources and high-temperature growth of the sample chamber. The entire high-temperature tube furnace is divided into a first insulation layer, a first heating zone, a second insulation layer, a second heating zone, a third insulation layer, a third heating zone, and a fourth insulation layer, each with a different length. Furthermore, due to the large area of ​​the 8-inch system and the significant thermal radiation effect, two ceramic insulation plates were designed. The first insulation plate consists of a ceramic plate, ceramic connecting pipes, and ceramic bolts. It is positioned between the first and second heating zones to prevent thermal radiation from the higher-temperature second heating zone to the lower-temperature second heating zone. The second insulation plate is a ceramic plate with numerous through-holes, placed outside the third heating zone, and is made of alumina or zirconia ceramic. This multi-hole ceramic plate effectively mimics thermal radiation. Simultaneously, these holes allow for uniform airflow, resulting in a more uniform flow field within the chamber.

[0080] 2. Sample Chamber: The main chamber quartz tube is made of high-purity quartz, capable of operating at temperatures up to 1100℃. The inner wall of the tube is polished to ensure stable gas flow. Flanges are located on both sides of the quartz tube, with mirror-polished flange faces for excellent vacuum sealing and low leakage. One or more quartz sand core plates are welded into the center of the quartz tube. These quartz sand core plates have a porous microstructure that hinders gas molecule flow, eliminating vector differences in velocity before the gas enters the quartz sand core plate. After passing through the porous quartz sand core, the gas flow path tends to be parallel to the axis of the quartz tube. The quartz sand core plate has a certain reflective effect on the incident gas flow; the reflected gas forms vortices in front of the quartz sand core plate, which can more uniformly mix the high-temperature and low-temperature sources. The main chamber quartz tube is easy to clean and does not contaminate the growth process.

[0081] 3. Multiple independent carrier gas inputs were designed, ensuring thorough mixing of the multiple carrier gases only before they reach the sample chamber to avoid solid-state source poisoning. The carrier gas system utilizes high-precision stainless steel gas path assembly components from Swagelok (USA) to reduce system leakage. Combined with a high-precision mass flow meter from MKS (USA), it effectively controls the stable airflow input, achieving uniform film formation. There are three types of gas inlets: main chamber inlet, high-temperature source inlet, and low-temperature source inlet. The main chamber inlet and low-temperature source inlet are located in the middle of the movable sealing plate of the solid-state source, with their inlet channel axes aligned with the quartz tube axis. There are 4-10 high-temperature source inlet pipes arranged on the circumference of the sealing plate, positioned approximately 75mm from the center of the sealing plate.

[0082] 4. A movable solid-state source separation device is used, with 5-11 independent solid-state source tubes fixed at the flange connection point of the carrier gas inlet. This allows for the separation of solid-state sources, improving solid-state source utilization, increasing growth rate, and enabling controllable growth. This shower-like multi-source supply design ensures a relatively uniform cross-sectional supply of the high-temperature source after evaporation, which is crucial for growing uniform 8-inch wafers. Most importantly, each solid-state source can be controlled by longitudinal movement to switch it on and off, allowing for on-demand control of evaporation. This enables layer-by-layer growth and in-situ multi-element epitaxial heterojunction growth.

[0083] The technical problem this invention aims to solve is that two-dimensional semiconductor materials are direct bandgap materials with high on / off ratios, compatible with silicon-based fabrication processes, and easy to process and miniaturize for device integration, showing great application potential in the fields of electronics and optoelectronic devices. However, the wafer fabrication of two-dimensional semiconductor materials still faces several challenges:

[0084] 1. How to achieve large-grain, single-orientation two-dimensional semiconductor materials?

[0085] Although CVD can now fabricate large-area continuous monolayer films, the grain size is relatively small and there are many grain boundaries. The challenges include controlling the nucleation density; controlling growth to ensure consistent grain orientation; and eliminating grain boundary formation during growth and splicing.

[0086] 2. How to ensure the uniformity of the thin film?

[0087] Uniformity mainly includes the uniformity between wafers, between different wafers, and between wafers in the same batch.

[0088] 3. How to control the number of film layers?

[0089] How to control the growth pattern to ensure strictly monolayer growth, preventing the nucleation and growth of the second layer before the first layer is fully grown? How to achieve controllable growth in single-layer, double-layer, and multi-layer configurations.

[0090] 4. How to achieve equipment versatility?

[0091] This equipment is designed to achieve the epitaxial growth of two-dimensional semiconductor materials, including molybdenum disulfide (MoS2), tungsten disulfide (WS2), tungsten diselenide (WSe2), and molybdenum diselenide (MoSe2). Different sources will be used for different materials; the challenge is to ensure that the sources do not contaminate each other during the growth process.

[0092] Two-dimensional semiconductor materials, represented by molybdenum disulfide (MoD), are promising new electronic materials in the post-Moore's Law era. Wafer-scale MoD fabrication technology is the engine driving innovation in two-dimensional semiconductors in integrated circuit technology. This invention relates to a novel chemical vapor deposition system for growing 8-inch wafer-scale two-dimensional transition metal chalcogenide semiconductor materials. This equipment places multiple gaseous and solid sources upstream, and each source's switching and carrier gas composition ratio can be independently controlled. This solves the bottleneck problem of poor film uniformity in large-area thin film growth, and breaks through the technical bottleneck of controllable growth of large-area layers. It enables uniform 8-inch growth of MoD and layer-by-layer epitaxial growth of multilayer two-dimensional transition metal chalcogenide homogeneous and heterogeneous structures, providing a technical foundation for the large-scale application of wafer-level two-dimensional semiconductor materials in devices.

[0093] The two-dimensional semiconductor growth system of the present invention may have, but is not limited to, the following beneficial effects:

[0094] 1. The equipment is simple and quick to operate, uses inexpensive and readily available raw materials, grows quickly, has good controllability of growth conditions, and does not pollute the environment.

[0095] 2. This equipment can grow molybdenum disulfide samples at the wafer level, such as 8 inches, and the resulting samples are large-area monolayer films with high quality and good uniformity.

[0096] 3. This equipment can also be used for real-time concentration controllable adjustment of various solid sources, enabling the layer-by-layer growth of two-dimensional semiconductor materials and the growth of in-situ epitaxial heterostructures.

[0097] 4. This equipment is also suitable for the growth of other transition metal chalcogenide thin films, including two-dimensional materials such as tungsten disulfide, molybdenum diselenide, tungsten diselenide, molybdenum distelluride, and tungsten distelluride, with substrates including sapphire, silicon, silicon dioxide, quartz, mica, and silicon carbide. Attached Figure Description

[0098] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings, wherein:

[0099] Figure 1 A schematic diagram of the composition and structure of the high-temperature tube furnace reaction chamber in the two-dimensional semiconductor growth system of the present invention is shown.

[0100] Figure 2 The diagrams show the flow field distribution inside a quartz tube with and without a quartz sand core plate in the two-dimensional semiconductor growth system of the present invention; wherein, Figure 2 A shows the flow field distribution inside a quartz tube with a quartz sand core plate; Figure 2 B shows the flow field distribution inside the quartz tube without a quartz core plate; the area within the dashed box is the location of the third heating zone (1-1-6), which is the location of the substrate.

[0101] Figure 3 A schematic diagram of the first heat insulation plate structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0102] Figure 4 A schematic diagram of the second heat insulation plate structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0103] Figure 5 A schematic diagram of a movable sealing disk for a solid-state source in the growth system of a two-dimensional semiconductor of the present invention is shown.

[0104] Figure 6 The diagram shows a simulation of the flow field uniformity in the two-dimensional semiconductor growth system of the present invention under a multi-solid-state source distribution air intake mode; wherein, Figure 6 A shows the air intake method of the main cavity air intake pipe, a high-temperature source air intake pipe and a central composite air intake pipe. The simulation diagram of the flow field uniformity inside the quartz tube is also shown. Figure 6 B shows a simulation diagram of the flow field uniformity inside the quartz tube, illustrating the intake method of a ring of high-temperature source intake pipes and a central composite intake pipe.

[0105] Figure 7 This diagram illustrates a simulation of the flow field uniformity under different high-temperature source inlet pipe locations within the two-dimensional semiconductor growth system of this invention; wherein, Figure 7A through E show simulation diagrams of the flow field uniformity inside the quartz tube when the distance from the high-temperature source inlet pipe to the center of the sealing plate is 20, 35, 55, 75, and 95 mm, respectively.

[0106] Figure 8 A schematic diagram of the longitudinally moving base structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0107] Figure 9 A schematic diagram of the transverse linear module structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0108] Figure 10 A schematic diagram of the first sealing plate structure in the two-dimensional semiconductor growth system of the present invention is shown; wherein, Figure 10 A shows a schematic diagram of the front structure of the first sealing plate; Figure 10 B shows a schematic diagram of the back structure of the first sealing plate.

[0109] Figure 11 A schematic diagram of the corrugated tube parallel plate structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0110] Figure 12 A schematic diagram of the butterfly vacuum bellows structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0111] Figure 13 A schematic diagram of the central composite air inlet pipe structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0112] Figure 14 A schematic diagram of the quartz tube holder structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0113] Figure 15 A schematic diagram of the high-temperature sample inlet pipe structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0114] Figure 16 A schematic diagram of the second sealing plate structure in the two-dimensional semiconductor growth system of the present invention is shown; wherein, Figure 16 A shows a schematic diagram of the second sealing plate structure; Figure 16 B shows a schematic diagram of the front structure of the second sealing plate mainboard; Figure 16 C shows a schematic diagram of the front structure of the second sealing plate mainboard.

[0115] Figure 17 A schematic diagram of the gas extraction end sealing disk structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0116] Figure 18 A schematic diagram of the quartz tube support structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0117] Figure 19A schematic diagram of the support frame structure in the growth system of the two-dimensional semiconductor of the present invention is shown.

[0118] Figure 20 A schematic diagram of the gas path panel structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0119] Figure 21 A schematic diagram of the furnace structure in the two-dimensional semiconductor growth system of the present invention is shown.

[0120] Figure 22 A schematic diagram of the structure of the two-dimensional semiconductor growth system of the present invention is shown.

[0121] Explanation of reference numerals in the attached figures:

[0122] 1. High-temperature tubular furnace; 2. Solid-state source movable sealing plate; 3. Vacuum sealing plate; 4. Quartz tube support bracket; 5. Support frame; 6. Gas circuit panel; 7. Alkali tank; 8. Vacuum pump; 9. Control host; 1-1. Furnace body; 1-2. Main cavity quartz tube; 1-3. First heat insulation plate; 1-4. Second heat insulation plate; 1-1-1. First heat insulation layer; 1-1-2. First heating zone; 1-1-3. Second heat insulation layer; 1-1-4. Second heating zone; 1-1-5. Third heat insulation layer; 1-1-6. Third heating zone; 1-1-7. Fourth heat insulation layer; 1-3-1. Ceramic connecting pipe; 1-3-2. Ceramic plate; 1-3-3. Ceramic bolt; 2-1. Longitudinal moving base; 2-2. Transverse linear module; 2-3. 2-4. Sealing plate; 2-5. Vacuum gauge; 2-6. Corrugated pipe parallel plate; 2-7. Butterfly-type vacuum corrugated pipe; 2-8. Central composite air inlet pipe; 2-9. High-temperature source air inlet pipe; 2-10. First sealing plate support leg; 2-11. Corrugated pipe parallel plate support leg; 2-12. Second sealing plate support leg; 2-1-1. First slider of longitudinal moving base; 2-1-2. Base plate of longitudinal moving base; 2-1-3. Linear guide rail of longitudinal moving base; 2-1-4. Second slider of longitudinal moving base; 2-2-1. Base plate of transverse linear module; 2-2-2. Mounting screw set; 2-2-3. Mounting linear guide rail; 2-2-4. First slider; 2-2-5. First slider adapter of transverse linear module. 2-2-6, Second slider of the transverse linear module; 2-2-7, Second slider adapter seat of the transverse linear module; 2-3-1, Sealing groove of the first sealing plate; 2-3-2, Central air inlet of the first sealing plate; 2-3-3, Outer ring air inlet of the first sealing plate; 2-3-4, Vacuum gauge connection hole; 2-3-6, Threaded hole of the central air inlet of the first sealing plate; 2-3-7, Locking hole of the support leg of the first sealing plate; 2-5-1, Front hole of the bellows parallel plate; 2-5-2, Side hole of the bellows parallel plate; 2-5-3, Support leg connection hole of the bellows parallel plate; 2-6-1, Second sealing flange of the butterfly vacuum bellows; 2-6-2, Bellows telescopic unit; 2-6-3, Telescopic unit connecting plate; 2-6-4, First sealing method 2-7-1, Central composite air inlet flange cavity; 2-7-2, Quartz tube holder; 2-7-3, First vacuum connector; 2-7-4, Second vacuum connector; 2-7-5, Low-temperature solid-state source quartz tube; 2-7-2-1, Quartz tube holder main pipe; 2-7-2-2, First PTFE fastening tube; 2-7-2-3, First extrusion tube; 2-7-2-4, Extrusion tube sealing ring on the side; 2-7-2-5, Quartz tube sealing ring; 2-7-2-6, Second extrusion tube; 2-7-2-7, Second PTFE fastening tube; 2-7-2-8, Movable extrusion tube; 2-7-2-9, Extrusion nut; 2-8, High-temperature sample air inlet pipe; 2-8-1, High-temperature solid-state source quartz tube; 2-8-2, Extension tube;2-11-1 Second sealing plate main board; 2-11-2 Irregularly shaped sealing ring; 2-11-3 Second sealing plate secondary plate; 2-11-4 Second sealing plate vacuum connector; 2-11-5 High-temperature sample inlet pipe sealing ring; 2-11-1-6 Second sealing groove of the second sealing plate main board; 2-11-5-7 Third threaded blind hole of the second sealing plate main board; 3-1 Extraction end sealing plate; 3-3 Extraction end sealing plate support leg; 3-4 Extraction end sealing disc longitudinal slider; 3-5 Extraction end sealing disc longitudinal... 3-6. Linear guide rail; 3-7. Base plate of the suction end sealing plate; 4-1. Horizontal slider of the suction end sealing plate; 4-2. Optical axis; 4-3. Optical axis fixing seat; 4-4. Quartz tube support drag plate; 4-5. Quartz tube support drag slider; 6-1. First mass flow meter; 6-2. Second mass flow meter; 6-3. Third mass flow meter; 6-4. Fourth mass flow meter; 6-5. Fifth mass flow meter; 6-6. First valve; 6-7. Second valve; 6-8. Third valve. Detailed Implementation

[0123] The present invention will be further illustrated below with specific embodiments. However, it should be understood that these embodiments are merely for more detailed and specific illustration and should not be construed as limiting the present invention in any way.

[0124] This section provides a general description of the materials and testing methods used in the experiments of this invention. While many of the materials and methods of operation used to achieve the objectives of this invention are well known in the art, the invention is still described in as much detail as possible herein. It will be apparent to those skilled in the art that, unless otherwise stated in the context, the materials and methods of operation used in this invention are well known in the art.

[0125] Example 1

[0126] This embodiment is used to illustrate the growth system of the two-dimensional semiconductor of the present invention.

[0127] This embodiment uses the method of preparing single-layer and multi-layer molybdenum disulfide coatings on 8-inch wafers as an example.

[0128] A novel chemical vapor deposition system for growing 8-inch wafer-scale two-dimensional transition metal sulfide compound semiconductor materials, as shown in the attached figure. Figure 22 As shown, its structure includes the following parts: high temperature tube furnace (1), solid source movable sealing plate (2), gas extraction sealing plate (3), quartz tube support bracket (4), support frame (5), gas circuit panel (6), alkali tank (7), vacuum pump (8), and control host (9), wherein the control host is inside the frame.

[0129] Figure 1A schematic diagram of the composition and structure of the high-temperature tube furnace reaction chamber in the two-dimensional semiconductor growth system of the present invention is shown. See Appendix. Figure 1 The high-temperature tubular furnace (1) comprises the following parts: furnace body (1-1), main cavity quartz tube (1-2), first heat insulation plate (1-3), and second heat insulation plate (1-4).

[0130] Figure 21 A schematic diagram of the furnace structure in the two-dimensional semiconductor growth system of the present invention is shown. (See attached diagram) Figure 21 As shown, the furnace body is a top-and-bottom opening furnace body, and both the top and bottom parts include a heat insulation layer and a heating zone; wherein, the heat insulation layer includes a first heat insulation layer (1-1-1), a second heat insulation layer (1-1-3), a third heat insulation layer (1-1-5), and a fourth heat insulation layer (1-1-7); the heating zone includes a first heating zone (1-1-2), a second heating zone (1-1-4), and a third heating zone (1-1-6).

[0131] The first insulation layer (1-1-1) is located at the edge of the furnace (1-1) and has a relatively small thickness of 30mm ± 5mm, facilitating heat dissipation from the first heating zone (1-1-2) by radiation. The second insulation layer is located between the first and second heating zones and has a thickness of 600mm ± 5mm. The third insulation layer is located between the second and third heating zones and has a thickness of 150mm ± 5mm. The fourth insulation layer is located at the edge of the third heating zone and has a thickness of 90mm ± 5mm.

[0132] The first heating zone (1-1-2) is a low-temperature zone, located between the first insulation layer (1-1-1) and the second insulation layer (1-1-3), with a length of 300mm ± 10mm. Its function is to heat the sulfur source, and its maximum operating temperature is 1200℃, while the operating temperature during growth is approximately 200℃. In this embodiment, the operating temperature is 200℃.

[0133] The second insulation layer (1-1-3) is a relatively thick insulation layer located between the first heating zone (1-1) and the second heating zone (1-3). Its thickness is 600mm ± 30mm, and its function is to minimize the impact of the high temperature of the second heating zone (1-1-4) on the temperature of the first heating zone (1-1-2). In this embodiment, the length of the second insulation layer is 120mm ± 10mm, and the length of the third insulation layer is 100mm ± 10mm.

[0134] The second heating zone (1-1-4) heats the metal source (such as Mo, W, Se, etc.). The evaporation temperature of the metal source is relatively high, around 800-1000℃. Due to the large size of the cavity, thermal radiation has a significant impact on the low-temperature zone. Therefore, the length of the second insulation layer needs to be made as long as possible to prevent the power of thermal radiation received by the first heating zone (1-1-2) from the second heating zone (1-1-4) from being too high. When the power received by the first heating zone (1-1-2) from the second heating zone (1-1-4) exceeds the power it radiates outward, the temperature of the first heating zone (1-1-2) will be beyond the control of the temperature controller. In this embodiment, the metal source used is MoO3.

[0135] The third heat insulation layer (1-1-5) has a moderate thickness, and its function is to reduce the impact of thermal radiation from the second heating zone (1-1-4) on the second heating zone (1-6). Since the operating temperatures of the second heating zone (1-1-4) and the third heating zone (1-1-6) are close, the heat insulation zone between them does not need to be too long; otherwise, the heat source would not be able to reach the substrate. In this embodiment, the length of the third heat insulation layer is 120±10 mm.

[0136] The main quartz tube (1-2) is made of high-purity quartz and can operate at temperatures up to 1100℃. The quartz tube has flanges on both sides, with mirror-polished flange ends. One or more quartz sand core plates are welded into the middle of the quartz tube. In this embodiment, two quartz sand core plates are used.

[0137] Figure 2 The diagrams show the flow field distribution inside a quartz tube with and without a quartz sand core plate in the two-dimensional semiconductor growth system of the present invention; wherein, Figure 2 A shows the flow field distribution inside a quartz tube with a quartz sand core plate; Figure 2 B shows the flow field distribution inside the quartz tube without a quartz core plate; the area within the dashed box is the location of the third heating zone (1-1-6), which is also the location of the substrate. (See attached diagram) Figure 2A simplified comparison of the flow field distribution inside a quartz tube with and without a quartz core plate is shown (top: with quartz core plate; without quartz core plate). The dashed box indicates the location of the third heating zone (1-1-6), which is the substrate location. It is easy to see that the flow field in the substrate area of ​​the quartz tube with the quartz core plate is more uniform than that of the quartz tube without the quartz core plate. A uniform flow field is crucial for the growth of large-size wafers. The reason why the quartz core plate can make the flow field uniform is because the quartz core plate has a porous microstructure. This microstructure has a certain obstruction effect on gas molecules, which eliminates the vector difference in velocity before entering the quartz core plate. After the airflow passes through the quartz core, it is rectified by the porous quartz core, and the flow path of the airflow passing through the quartz core plate will tend to be parallel to the axis of the quartz tube. Quartz sand core plates have a certain reflective effect on incident airflow. The reflected gas will form vortices in front of the quartz sand core plate. These vortices can make the high-temperature source and the low-temperature source mix more evenly.

[0138] Figure 3 A schematic diagram of the first heat insulation plate structure in the two-dimensional semiconductor growth system of the present invention is shown. See Appendix. Figure 3 The first heat insulation plate (1-3) consists of the following parts: a ceramic connecting tube (1-3-1), a ceramic plate (1-3-2), and ceramic bolts (1-3-3). The ceramic plate has three types of holes: bolt holes for connecting the ceramic connecting tube, air passage holes, and clearance holes. The clearance holes allow the quartz tube of the high-temperature sample inlet pipe (2-8) to pass through. The ceramic connecting tube (1-3-1) is a ceramic tube with multiple threaded holes on one end face, which match the bolt holes on the ceramic plate (1-3-2).

[0139] The first heat insulation plate (1-3) is placed in the middle of the first heating zone (1-1-2) and the second heating zone (1-1-4). Its function is to prevent the heat radiation from the higher-temperature second heating zone (1-1-4) from radiating to the lower-temperature second heating zone (1-1-4).

[0140] Figure 4 A schematic diagram of the second heat insulation plate structure in the two-dimensional semiconductor growth system of the present invention is shown. See Appendix. Figure 4 The second heat insulation plate (1-4) is a ceramic plate with many through-holes, and its thickness is approximately 25%-50% of its diameter. It is positioned outside the third heating zone (1-1-6) and is made of alumina ceramic or zirconia ceramic. This multi-hole ceramic plate provides excellent heat radiation protection. Simultaneously, these holes allow for uniform airflow, resulting in a more uniform flow field within the cavity. In this embodiment, the second heat insulation plate is made of alumina ceramic and has a thickness of 120mm ± 10mm.

[0141] Figure 5 A schematic diagram of a movable sealing disk for a solid-state source in the growth system of a two-dimensional semiconductor according to the present invention is shown. See Appendix. Figure 5 The solid source movable sealing plate (2) includes the following parts: longitudinal moving base (2-1), transverse straight module (2-2), first sealing plate (2-3), vacuum gauge (2-4), bellows parallel plate (2-5), butterfly vacuum bellows (2-6), central composite air inlet pipe (2-7), high temperature source air inlet pipe (2-8), first sealing plate support leg (2-9), bellows parallel plate support leg (2-10), second sealing plate (2-11), and second sealing plate support leg (2-12).

[0142] The solid source movable sealing plate (2) has three types of air intake: main cavity air intake, high temperature source air intake, and low temperature source air intake. The air intake positions of the main cavity air intake and the low temperature source air intake are located in the middle of the solid source movable sealing plate (2), and the axis of their air intake channels is the same as the axis of the quartz tube.

[0143] Figure 6 The diagram shows a simulation of the flow field uniformity in the two-dimensional semiconductor growth system of the present invention under a multi-solid-state source distribution air intake mode; wherein, Figure 6 A shows the air intake method of the main cavity air intake pipe, a high-temperature source air intake pipe and a central composite air intake pipe. The simulation diagram of the flow field uniformity inside the quartz tube is also shown. Figure 6 B shows a simulation diagram of the flow field uniformity inside the quartz tube, illustrating the intake method of a ring of high-temperature source intake pipes and a central composite intake pipe. See appendix. Figure 6 Fluid analysis revealed that, compared to three intake pipes (main chamber intake pipe, one high-temperature source intake pipe, and central composite intake pipe), the flow field inside the quartz tube is more uniform with the addition of a single high-temperature source intake pipe and a central composite intake pipe in this invention.

[0144] Figure 7 This diagram illustrates a simulation of the flow field uniformity under different high-temperature source inlet pipe locations within the two-dimensional semiconductor growth system of this invention; wherein, Figure 7 Figures A through E show the simulated flow field uniformity inside the quartz tube when the distance from the high-temperature source inlet pipe to the center of the sealing plate is 20, 35, 55, 75, and 95 mm, respectively. (See also...) Figure 7There are 4-10 high-temperature source inlet pipes (2-8) arranged on the circumference of the sealing plate. Fluid analysis was used to calculate the flow field inside the quartz tube at different distances of the high-temperature source inlet pipes (2-8) from the center of the sealing plate. The flow field states of the six high-temperature source inlet pipes (2-8) are shown from top to bottom at approximately 20, 35, 55, 75, and 95 mm. It can be seen that the flow field uniformity is best at 75 mm. Therefore, the high-temperature source inlet pipes (2-8) are placed at approximately 75 mm from the center of the sealing plate. Fluid simulation revealed that a greater distance between the high-temperature source inlet pipes (2-8) and the center of the sealing plate is more conducive to a uniform flow field inside the quartz tube. In this embodiment, there are six high-temperature source inlet pipes (2-8), placed at a distance of 75 mm from the center of the sealing plate.

[0145] Figure 8 A schematic diagram of the longitudinally moving base structure in the two-dimensional semiconductor growth system of the present invention is shown. See also Figure 8 The longitudinal moving base (2-1) comprises the following parts: the first slider of the longitudinal moving base (2-1-1), the base plate of the longitudinal moving base (2-1-2), the linear guide rail of the longitudinal moving base (2-1-3), and the second slider of the longitudinal moving base (2-1-4).

[0146] Two sets of first sliders (2-1-1) of the longitudinal moving base are installed side by side at the bottom of the longitudinal moving base base plate (2-1-2). Their function is to install the longitudinal moving base (2-1) onto the guide rail of the support frame (5). At least one guide rail, namely the longitudinal moving base linear guide rail (2-1-3), is installed above the longitudinal moving base base plate (2-1-2). The installation direction of the longitudinal moving base linear guide rail (2-1-3) is perpendicular to the movement direction of the first slider (2-1-1) of the longitudinal moving base. Above each longitudinal moving base linear guide rail (2-1-3) there is at least one second slider (2-1-4) of the longitudinal moving base. The function of the second slider (2-1-4) of the longitudinal moving base is to connect the transverse linear module (2-2). In addition to the countersunk hole of the initial connecting slider of the longitudinal moving base plate (2-1-2), there is a threaded hole above the first slider (2-1-1) of each longitudinal moving base in a place other than the slider connecting hole. The function of these threaded holes is to install set screws to finely adjust the height and level of the longitudinal moving base plate (2-1-2). Figure 9 A schematic diagram of the transverse linear module structure in the two-dimensional semiconductor growth system of the present invention is shown. See also Figure 9The horizontal linear module (2-2) includes the following parts: linear module base plate (2-2-1), lead screw assembly (2-2-2), horizontal linear module linear guide rail (2-2-3), horizontal linear module first slider (2-2-4), horizontal linear module first slider adapter seat (2-2-5), horizontal linear module second slider (2-2-6), and horizontal linear module second slider adapter seat (2-2-7).

[0147] The bottom of the horizontal linear module base plate (2-2-1) has multiple sets of mounting holes, including countersunk threaded holes for mounting and connecting the longitudinal moving base (2-1), threaded holes for mounting the linear guide rail (2-2-3), and threaded holes for mounting the lead screw assembly (2-2-2).

[0148] The horizontal linear module linear guide rails (2-2-3) are installed on both sides of the upper surface of the horizontal linear module base plate (2-2-1).

[0149] The lead screw assembly (2-2-2) includes an end lead screw support, a lead screw nut, a lead screw nut adapter block, a motor mount, a coupling, and a motor. The lead screw assembly (2-2-2) is installed in the center of the linear module base plate (2-2-1).

[0150] The first slider adapter (2-2-5) has three sets of threaded holes, which are used to connect the nut of the lead screw assembly (2-2-2), the first slider (2-2-4), and the second sealing plate support leg (2-10), respectively. When the motor rotates, the first slider adapter (2-2-5) will move linearly together with the nut of the lead screw assembly (2-2-2), thereby driving the bellows parallel plate (2-5) to move linearly.

[0151] There are multiple second slider adapters (2-2-7), and each second slider adapter (2-2-7) has a set of countersunk holes and a set of threaded holes. The countersunk holes are used to connect the second slider (2-2-6), and the threaded holes are used to connect the bellows parallel plate (2-5).

[0152] Figure 10 A schematic diagram of the first sealing plate structure in the two-dimensional semiconductor growth system of the present invention is shown; wherein, Figure 10 A shows a schematic diagram of the front structure of the first sealing plate; Figure 10 B shows a schematic diagram of the rear structure of the first sealing plate. See also Figure 10The front of the first sealing plate (2-3) is provided with a groove, namely the first sealing plate sealing groove (2-3-1). The surface finish of the three surfaces of the groove is better than 1.6. There are multiple through holes on the inner side of the groove, namely the first sealing plate central air inlet hole (2-3-2) located in the center, a ring of holes located outside the first sealing plate central air inlet hole (2-3-2), the first sealing plate outer ring air inlet hole (2-3-3), and the vacuum gauge connection hole (2-3-4) located between the first sealing plate outer ring air inlet hole (2-3-3) and the first sealing plate sealing groove (2-3-1). The back of the first sealing plate (2-3) has multiple sets of non-penetrating threaded holes. The threaded holes (2-3-6) around the central air inlet hole (2-3-2) of the first sealing plate are used to lock the central composite air inlet pipe (2-7). The locking holes (2-3-7) of the bottom first sealing plate support leg are used to lock the first sealing plate (2-3) and the first sealing plate support leg (2-9) together.

[0153] The vacuum gauge (2-4) is a thin-film gauge, which is installed on the first sealing plate (2-3).

[0154] Figure 11 A schematic diagram of the bellows parallel plate structure in the two-dimensional semiconductor growth system of the present invention is shown. See also Figure 11 The front of the bellows parallel plate (2-5) has multiple through holes (one in the center and six around it), namely the bellows parallel plate front hole (2-5-1), which are used to install the support plate of the butterfly bellows (2-6). The lower part of the front of the bellows parallel plate (2-5) has a set of threaded holes, namely the bellows parallel plate support leg connection holes (2-5-3). The side of the bellows parallel plate (2-5) has a ring of threaded holes, namely the bellows parallel plate side holes (2-5-2). The axis of these holes is perpendicular to the axis of the bellows parallel plate front hole (2-5-1), and their function is to install set screws to connect the bellows parallel plate (2-5) and the butterfly vacuum bellows (2-6).

[0155] Figure 12 A schematic diagram of a butterfly vacuum bellows structure in the two-dimensional semiconductor growth system of the present invention is shown. See also Figure 12The butterfly vacuum bellows (2-6) has the following features: a second sealing flange (2-6-1), a bellows expansion unit (2-6-2), an expansion unit connecting plate (2-6-3), and a first sealing flange (2-6-4). The second sealing flange (2-6-1) has a ring of holes on its end face, used for mounting bolts to lock the butterfly vacuum bellows (2-6) to the second vacuum sealing plate (2-11). The second sealing flange (2-6-1) also has a sealing groove on its end face, used for installing a sealing ring. This sealing ring allows for a sealed connection between (2-6) and the second vacuum sealing plate (2-11). The butterfly-type vacuum bellows (2-6) comprises multiple bellows expansion units (2-6-2). A connecting plate (2-6-3) is welded between two bellows expansion units (2-6-2), which provides support points for the bellows expansion units (2-6-2). The first sealing flange (2-6-4) of the butterfly-type vacuum bellows has a ring of holes on its end face, which are used to install bolts to lock the butterfly-type vacuum bellows (2-6) to the first vacuum sealing plate (2-5). There is also a sealing groove on the end face, which is used to install a sealing ring, thereby sealingly connecting (2-6) to the second vacuum sealing plate (2-5).

[0156] Figure 13 A schematic diagram of the central composite inlet pipe structure in the two-dimensional semiconductor growth system of the present invention is shown. See also Figure 13 The central composite air inlet pipe (2-7) includes the following parts: central composite air inlet pipe flange cavity (2-7-1), quartz tube holder (2-7-2), first vacuum connector (2-7-3), second vacuum connector (2-7-4), and low-temperature solid-state source quartz tube (2-7-5).

[0157] The flange face of the central composite air intake pipe flange cavity (2-7-1) is provided with a sealing ring mounting groove and a through hole. After the sealing ring is installed on the sealing ring mounting groove, the central composite air intake pipe flange cavity (2-7-1) is pressed onto the first sealing plate (2-3) by bolts through the through hole on the flange, thereby realizing the sealing connection between the central composite air intake pipe (2-7) and the first sealing plate (2-3).

[0158] The gap between the quartz tube holder (2-7-2) and the central composite inlet flange cavity (2-7-1) is completely welded together, achieving a vacuum seal. The central composite inlet flange cavity (2-7-1) has a through-hole on its side, on which a vacuum connector, the first vacuum connector (2-7-3), is sealed and welded. The quartz tube holder (2-7-2) has a quartz tube mounting hole at its front end and a vacuum connector mounting hole at its rear end, which communicates with the quartz tube mounting hole. The rear vacuum connector mounting hole is sealed and welded together with the second vacuum connector (2-7-4).

[0159] Figure 14 A schematic diagram of the quartz tube holder structure in the two-dimensional semiconductor growth system of the present invention is shown. See also Figure 14 The quartz tube holder (2-7-2) comprises the following parts: quartz tube holder main tube (2-7-2-1), first PTFE fastening tube (2-7-2-2), first extrusion tube (2-7-2-3), extrusion tube sealing ring (2-7-2-4), quartz tube sealing ring (2-7-2-5), second extrusion tube (2-7-2-6), second PTFE fastening tube (2-7-2-7), movable extrusion tube (2-7-2-8), and extrusion nut (2-7-2-9).

[0160] The inner wall and the inner side of the bottom surface of the quartz tube holder main tube (2-7-2-1) have a chamfer of angle b, where b is 110°±2°. The bottom is provided with a through hole, and the other end is externally threaded.

[0161] The first PTFE fastening tube (2-7-2-2) is made of a relatively soft PTFE material and is shaped as a round tube with a chamfer at one end. The angle of this chamfer is 'a', where 'a' is 120°±2°. The value of chamfer 'a' is greater than the chamfer 'b' between the inner wall and the inner bottom surface of the main tube of the quartz tube holder. Therefore, when the first PTFE fastening tube (2-7-2-2) is not compressed, the edge of its bottom is in contact with the chamfer at the bottom of the main tube of the quartz tube holder (2-7-2-1), rather than their bottom surfaces touching. When subjected to compression along the axial direction, their bottom surfaces gradually come into contact. Due to the difference in their chamfers, the inner diameter of the side of the first PTFE fastening tube (2-7-2-2) that contacts the chamfer is easily deformed, eventually fitting tightly against the quartz tube, thus locking the quartz tube in place.

[0162] The first extrusion tube (2-7-2-3) is a circular tube with a raised edge at the center of one end and a 45° chamfer at the other end. A sealing ring mounting groove is located on the side of the tube. The edged end of the first extrusion tube (2-7-2-3) contacts the first PTFE fastening tube (2-7-2-2). When the first extrusion tube (2-7-2-3) is subjected to axial force, the edge cuts into the first PTFE fastening tube (2-7-2-2), deforming it and reducing its inner diameter and increasing its outer diameter. This results in the inner side of the first PTFE fastening tube (2-7-2-2) being tightly fitted to the quartz tube, and the outer wall being tightly fitted to the inner wall of the quartz tube holder main tube (2-7-2-1). The outer wall of the first extrusion tube (2-7-2-3) has a groove for installing an O-ring. Installing the O-ring in this groove has two benefits: ① It seals the first extrusion tube (2-7-2-3) and the main tube of the quartz tube holder (2-7-2-1) together. ② It improves the coaxiality of the first extrusion tube (2-7-2-3) and the main tube of the quartz tube holder (2-7-2-1) during installation.

[0163] A sealing ring, namely a quartz tube sealing ring (2-7-2-5), is provided between the first extrusion tube (2-7-2-3) and the second extrusion tube (2-7-2-6). During installation, the quartz tube sealing ring (2-7-2-5) contacts the first extrusion tube (2-7-2-3) and the second extrusion tube (2-7-2-6) at a 45° chamfer. When the second extrusion tube (2-7-2-3) is subjected to axial compressive force, the quartz tube sealing ring will deform. Due to the chamfered contact between the quartz tube sealing ring and the first extrusion tube (2-7-2-3) and the second extrusion tube (2-7-2-6), the deformation direction of the quartz tube sealing ring is away from the inner wall of the main tube of the quartz tube holder (2-7-2-1) and closer to the outer wall of the quartz tube. When the deformation reaches a certain amount, the first extrusion tube (2-7-2-3) and the second extrusion tube (2-7-2-6) will directly contact each other. The quartz tube sealing ring (2-7-2-5) is squeezed into the gap between the chamfers of the first extrusion tube (2-7-2-3) and the second extrusion tube (2-7-2-6). This structure has two advantages: ① The extrusion pressure on the quartz tube sealing ring (2-7-2-5) will not increase after reaching a certain value, because the force required for the first PTFE fastening tube (2-7-2-2) and the second PTFE fastening tube (2-7-2-7) to adhere tightly to the quartz tube and the main tube of the quartz tube holder (2-7-2-1) is greater than the maximum load of the sealing ring. If the first extrusion tube (2-7-2-3) and the second extrusion tube (2-7-2-6) do not have a chamfer structure, the pressure on the quartz tube sealing ring (2-7-2-5) will be the same as the axial force on the first extrusion tube (2-7-2-3) and the second extrusion tube (2-7-2-6). With the presence of the chamfered structure, the maximum force on the quartz tube sealing ring (2-7-2-5) is only related to the size of the chamfer between the first extrusion tube (2-7-2-3) and the second extrusion tube (2-7-2-6).

[0164] The second extrusion tube (2-7-2-6) has the same structure as the first extrusion tube (2-7-2-3), but is installed in the opposite direction.

[0165] The second PTFE fastening tube (2-7-2-7) has the same structure as the first PTFE fastening tube (2-7-2-2), but is installed in the opposite direction. Its un-beveled end contacts the bladed end of the second extruded tube (2-7-2-6).

[0166] The chamfer c of the active extrusion tube (2-7-2-8) is 150°±5°, which is greater than the chamfer a of the second PTFE fastening tube (2-7-2-7). 2-7-2-2 and 2-7-2-7 have the same structure, but different installation positions. Figure 14Further details are provided in the supplementary document. The chamfer extends to the outer wall of the movable extrusion tube (2-7-2-8), forming a cutting edge on the outer ring. When the movable extrusion tube (2-7-2-8) is compressed, the cutting edge on its outer ring presses inward against the second PTFE fastening tube (2-7-2-7), causing the second PTFE fastening tube (2-7-2-7) to fit tightly against the quartz tube.

[0167] The inner ring of the compression nut (2-7-2-9) has an internal thread that matches the external thread of the quartz tube holder main tube (2-7-2-1). The compression nut (2-7-2-9) provides axial compression force to the movable compression tube (2-7-2-8) through the threaded structure of the quartz tube holder main tube (2-7-2-1), and this compression force is transmitted axially all the way to the first PTFE fastening tube (2-7-2-2).

[0168] Figure 15 A schematic diagram of the high-temperature sample inlet pipe structure in the two-dimensional semiconductor growth system of the present invention is shown. See also... Figure 15 The high-temperature sample inlet tube (2-8) includes the following parts: quartz tube holder (2-7-2), extension tube (2-8-2), and high-temperature solid-state source quartz tube (2-8-1).

[0169] The extension tube (2-8-2) is a stainless steel tube with an external thread at one end, which matches the thread on the main board of the second sealing plate (2-11-1). The connecting tube's function is to seal the quartz tube holder (2-7-2) and the extension tube (2-8-2) together by welding. The delay tube (2-7-2) extends the quartz tube holder (2-7-2) to facilitate the installation of the high-temperature sample quartz tube (2-8-1) during experiments.

[0170] Figure 16 A schematic diagram of the second sealing plate structure in the two-dimensional semiconductor growth system of the present invention is shown; wherein, Figure 16 A shows a schematic diagram of the second sealing plate structure; Figure 16 B shows a schematic diagram of the front structure of the second sealing plate mainboard; Figure 16 C shows a schematic diagram of the front structure of the second sealing plate mainboard. See also Figure 16 The second sealing plate (2-11) consists of the following three parts: the main plate of the second sealing plate (2-11-1), the irregular sealing ring (2-11-2), the secondary plate of the second sealing plate (2-11-3), the vacuum connector of the second sealing plate (2-11-4), and the sealing ring of the high-temperature sample inlet pipe (2-11-5).

[0171] The main plate of the second sealing plate (2-11-1) is sealed together with the secondary plate of the second sealing plate (2-11-3) by a special-shaped sealing ring (2-11-2). The vacuum connector of the second sealing plate (2-11-4) is connected to the outlet of the third valve (6-9) of the gas circuit panel (6) through a vacuum pipe.

[0172] The front of the second sealing plate main board (2-11-1) has four sets of holes: the first threaded blind hole (2-11-1-1), the second threaded blind hole (2-11-1-2), the threaded through hole (2-11-1-3), and the first sealing groove (2-11-1-4). The back of the second sealing plate main board (2-11-1) has a circular groove (2-11-1-5), a shaped sealing ring groove (2-11-1-6), and multiple threaded blind holes (2-11-5-7). The first threaded blind hole (2-11-1-1) on the main board of the second sealing plate is used to lock and install the second sealing plate support leg (2-12). The second threaded blind hole (2-11-1-2) on the main board of the second sealing plate is used to lock and install the butterfly vacuum bellows (2-6). The threaded through hole (2-11-1-3) on the main board of the second sealing plate is used to install the high-temperature sample inlet pipe (2-8). The first sealing groove (2-11-1-4) on the main board of the second sealing plate is used to install the high-temperature sample inlet pipe sealing ring (2-11-5). These sealing rings seal the high-temperature sample inlet pipe (2-11-5) with the main board of the second sealing plate (2-11-1). The circular groove (2-11-1-5) on the back of the main board of the second sealing plate is used to position and install the second sealing plate secondary plate (2-11-3). The second sealing groove (2-11-1-6) on the main board of the second sealing plate is used to install the irregularly shaped sealing ring (2-11-2). The function of the third threaded blind hole (2-11-5-7) on the main board of the second sealing plate is to lock the secondary board (2-11-3) of the second sealing plate with bolts. The overall structure of the main board of the second sealing plate (2-11-1) enables the uniform and equal supply of air to the high-temperature sample inlet pipe (2-8) through one air intake, after passing through the main board of the second sealing plate (2-11-1).

[0173] Figure 17 A schematic diagram of the gas extraction end sealing disk structure in the two-dimensional semiconductor growth system of the present invention is shown. See also... Figure 17The suction end sealing plate (3) consists of the following parts: suction end sealing plate (3-1), suction end sealing plate support leg (3-3), suction end sealing plate longitudinal slider (3-4), suction end sealing plate longitudinal linear guide rail (3-5), suction end sealing plate base plate (3-6), and suction end sealing plate transverse slider (3-7).

[0174] The front of the suction end sealing plate (3-1) has a mounting groove for a sealing ring. The surface finish of the three sides of the mounting groove is better than 1.6. A through hole is provided in the middle, and a flange is welded to the through hole. The flange is connected to the vacuum pump (7) through a vacuum bellows. The back of the suction end sealing plate (3-1) has a set of threaded holes. These threaded holes are used to lock the suction end sealing plate (3-1) and the suction end sealing plate support leg (3-3) together. The lower part of the suction end sealing plate support leg (3-3) has multiple countersunk holes. Through these countersunk holes, the suction end sealing plate support leg (3-3) can be bolted to the longitudinal slider (3-4) of the suction end sealing plate. The longitudinal slider (3-4) of the suction end sealing plate is mounted on the longitudinal linear guide (3-5) of the suction end sealing plate. The longitudinal linear guide (3-5) of the suction end sealing plate is bolted to the base plate (3-6) of the suction end sealing plate. The base plate has two sets of countersunk holes and two sets of threaded holes. The countersunk holes are used to connect the transverse slider (3-7) of the suction end sealing plate, and the two sets of threaded holes are used to fine adjust the level and height of the sealing plate.

[0175] Figure 18 A schematic diagram of the quartz tube support structure in the two-dimensional semiconductor growth system of the present invention is shown. See also... Figure 18 The quartz tube support bracket (4) consists of the following parts: a semi-circular support plate (4-1), an optical axis (4-2), an optical axis fixing seat (4-3), a quartz tube support base plate (4-4), and a quartz tube support slider (4-5). The semi-circular support plate (4-1) has a semi-circular groove, which is slightly larger than the diameter of the main cavity quartz tube. The bottom surface of the semi-circular support plate (4-1) has two optical axis mounting holes, and the side of the semi-circular support plate (4-1) has a row of threaded holes at the position corresponding to the optical axis mounting. The function of this row of threaded holes is to install bolts to tightly press the optical axis to fix the optical axis (4-2) on the semi-circular support plate (4-1). The quartz tube support base plate (4-4) has two sets of threaded holes and four sets of countersunk holes. The purpose of these two sets of threaded holes is to install the optical axis support. Two sets of countersunk holes are used to install the quartz tube support slide block (4-5), and the other two sets of countersunk holes are used to fix the quartz tube support base plate (4-4), fixing the quartz tube support base plate (4-4) on the aluminum profile of the support frame (5).

[0176] Figure 19 A schematic diagram of the support frame structure in the growth system of the two-dimensional semiconductor of the present invention is shown. See also Figure 19The support frame (5) is constructed of aluminum profiles. The bottom of the frame has movable wheels, and linear guide rails are installed on the two aluminum profiles in the middle of the top. Corresponding sliders are mounted on the linear guide rails, and the holes on these sliders correspond to the threaded holes at the bottom of the tubular furnace. The tubular furnace can be locked onto these sliders for flexible movement. Sheet metal panels secured with bolts are installed on the left, right, rear, and top sides of the support frame, and there is an openable sheet metal door panel at the front. These openable doors allow for convenient operation of the gas path panel, vacuum pump, exhaust gas treatment box, and other components inside the support frame.

[0177] Figure 20 A schematic diagram of the gas path panel structure in the two-dimensional semiconductor growth system of the present invention is shown. See also Figure 20 The gas circuit panel (6) mainly consists of 5 mass flow meters, 3 valves, pipe joints connecting the mass flow meters and valves, stainless steel pipe assemblies, and mounting plates.

[0178] The five mass flow meters are, in order: first mass flow meter (6-1), second mass flow meter (6-2), third mass flow meter (6-3), fourth mass flow meter (6-4), and fifth mass flow meter (6-5). The three valves are: first valve (6-6), second valve (6-7), and third valve (6-8). The outlets of the first mass flow meter (6-1) and the second mass flow meter (6-2) converge and connect to the first valve (6-6), then to the second vacuum connector (2-7-4) of the central composite inlet pipe (2-7). Therefore, the first mass flow meter (6-1) can control the carrier gas flow into the low-temperature solid-state source quartz tube (2-7-5), thereby adjusting the evaporation rate of the low-temperature solid-state source. The first mass flow meter (6-1) is connected to the high-purity hydrogen source. The pipeline from the high-purity argon source branches into three paths after passing through a four-way connector, leading to the second mass flow meter (6-2), the third mass flow meter (6-3), and the fourth mass flow meter (6-4), respectively. The fifth mass flow meter (6-5) is connected to a high-purity oxygen source. The outlet of the third mass flow meter (6-3) is directly connected to the inlet of the second valve (6-7) via a vacuum tube connector, then connected to the first vacuum connector (2-7-3) of the central composite gas inlet pipe (2-7). Therefore, the third mass flow meter (6-3) can control the amount of gas entering the main chamber quartz tube (1-2), thereby controlling the vacuum level within the main chamber quartz tube (1-2). The outlets of the fourth mass flow meter (6-4) and the fifth mass flow meter (6-5) are connected together via a tee and then connected to the inlet of the third valve (6-8), and then connected to the vacuum connector (2-11-3) of the second sealing plate (2-11). Therefore, the amount of oxygen and argon entering the high-temperature sample inlet pipe (2-8) can be controlled by the fourth mass flow meter (6-4) and the fifth mass flow meter (6-5).

[0179] The mounting plate of the air circuit panel (6), namely the air circuit panel mounting plate (6-9), is an L-shaped sheet metal with multiple holes along its edge. These holes can be used to secure the air circuit panel to the aluminum profile inside the support frame (5).

[0180] The vacuum pump (8) is a corrosion-resistant oil-sealed plate pump, and the tail gas treatment system is an alkaline tank (7). The alkaline solution is a mixture of NaOH and KOH, and the ratio of their material flow is 1:1.

[0181] Example 2

[0182] This embodiment is used to illustrate the growth method of the two-dimensional semiconductor growth system of the present invention.

[0183] This embodiment uses a method for preparing single-layer and multi-layer molybdenum disulfide coatings on 8-inch wafers as an example. The composition and features of the CVD equipment can be found in Example 1 and its appendix. Figure 1-22 To understand.

[0184] Step 1, Preparation Stage: Place a single-crystal sapphire substrate in the CVD system, introduce an argon-oxygen mixture or high-purity oxygen, and anneal the substrate at a high temperature (900℃-1000℃) to create periodic and atomically flat steps, which is beneficial for nucleation in the early stages of growth and for uniform control of epitaxial growth. In this embodiment, an argon-oxygen mixture is used as the carrier gas at a temperature of 1000℃.

[0185] Step 2: Place 8-12g of 99% pure sulfur powder in the quartz tube at the center of the movable multi-solid source and place it in the first heating zone. Then, press 20-50mg of molybdenum oxide powder into thin sheets and place them at the front ends of six evenly distributed quartz tubes around it, ensuring they are far away from the second heating zone. Note that the amount of sulfur powder should be much greater than the amount of molybdenum oxide powder. In this embodiment, 10g of sulfur powder and 50mg of molybdenum oxide powder are used.

[0186] Step 3: Place the annealed sapphire wafer onto a tray. The tray can be a rectangular tray or a three-dimensional tray with other wafer holding capacities. The tray size can be set and adjusted according to the cavity size. Then, place the tray containing the sapphire substrate into the third heating zone—the high-temperature zone—of the three-heating-zone chemical vapor deposition system. In this embodiment, a three-dimensional tray is used.

[0187] Step 4: Different carrier gases are introduced sequentially: 100 sccm of argon in the main chamber, 120 sccm of argon in the sulfur source quartz tube, and an argon-oxygen mixture (240 sccm Ar + 4 sccm O) in the six molybdenum oxide source quartz tubes, maintaining the chamber pressure between 1 and 3 Torr. Oxygen here protects the molybdenum oxide from sulfidation and poisoning by the returning sulfur vapor, thus ensuring a relatively stable evaporation rate of the molybdenum source during growth and effectively controlling the stability of the growth rate. In this embodiment, the chamber pressure is 1.3 Torr.

[0188] Step 5: Raise the temperatures of the three heating zones to specific ranges: 120℃-150℃, 540℃-600℃, and 900℃-930℃. After the temperatures stabilize, introduce the movable solid-state source molybdenum oxide into the second heating zone and maintain growth for approximately 30-40 minutes. The first layer of molybdenum disulfide is then complete. In this embodiment, the temperatures of the three heating zones are 130℃, 540℃, and 930℃, with a growth time of 30 minutes.

[0189] Step 6: After the first layer growth is complete, stop the oxygen supply and move the molybdenum oxide source to the low-temperature zone. Simultaneously, change the growth conditions by increasing the substrate growth temperature from 930℃ to 960℃ and the molybdenum oxide source temperature from 540℃ to 560℃, keeping other growth parameters unchanged. After the temperature stabilizes, move the molybdenum oxide source back to the second heating zone and introduce oxygen carrier gas to begin the growth of the second layer of molybdenum sulfide, which takes 40-60 minutes. Immediately stop the oxygen carrier gas supply after the growth process is complete and allow the sample to cool naturally to room temperature under argon carrier gas protection before removing it. In this embodiment, the growth time is 40 minutes.

[0190] In step 2 of the method, sulfur powder can be replaced with selenium powder, tellurium powder, etc., and molybdenum oxide powder can be replaced with tungsten oxide, vanadium oxide, titanium oxide, etc.

[0191] In step 2, the method can also simultaneously and evenly place six quartz tubes into two oxide sources, and switch the two sources in step 6 to achieve the growth of epitaxial heterojunctions.

[0192] The method also includes a cavity oxygen cleaning process, which is performed after growth is complete to provide a cleaner environment for the next batch and eliminate cross-contamination between process cycles.

[0193] This invention enables uniform growth of 8-inch molybdenum disulfide and controlled epitaxial growth of multilayer two-dimensional semiconductor samples or van der Waals heterojunctions, which can greatly save equipment investment costs, reduce material consumption costs, and improve the competitiveness of equipment and two-dimensional semiconductor materials.

[0194] Although the invention has been described to a certain extent, it is apparent that appropriate variations can be made to the various conditions without departing from the spirit and scope of the invention. It is understood that the invention is not limited to the described embodiments, but falls within the scope of the claims, which include equivalent substitutions for each of the elements.

Claims

1. A two-dimensional semiconductor growth system, characterized in that, The two-dimensional semiconductor growth system includes: a high-temperature tube furnace, a solid-state source movable sealing plate, a suction end sealing plate, a quartz tube support, a support frame, and a gas path panel; wherein, the wafer size of the two-dimensional semiconductor is 2-8 inches, and the solid-state source movable sealing plate includes: a vacuum gauge, a sealing plate, a parallel plate, a bellows, and an inlet pipe; and: The high-temperature tube furnace is a resistance high-temperature tube furnace with three heating zones and temperature control, comprising: a furnace body, a main cavity quartz tube, and a heat insulation plate; wherein, the furnace body is an upper and lower opening furnace body, and both the upper and lower parts of the furnace body include a heat insulation layer and a heating zone; wherein, the heat insulation layer includes a first heat insulation layer, a second heat insulation layer, a third heat insulation layer, and a fourth heat insulation layer; the heating zone includes a first heating zone, a second heating zone, and a third heating zone; The main cavity quartz tube has flanges on both sides and a quartz sand core plate in the middle, which has a porous microstructure. The heat insulation plate includes a first heat insulation plate and a second heat insulation plate; wherein, the first heat insulation plate is located between the first heating zone and the second heating zone, and the second heat insulation plate is located outside the third heating zone; The solid-state source movable sealing disc further includes: a longitudinally moving base, a transverse linear module, a first sealing plate, a bellows parallel plate, a butterfly vacuum bellows, a central composite air inlet pipe, a high-temperature source air inlet pipe, a first sealing plate support leg, a bellows parallel plate support leg, a second sealing plate, and a second sealing plate support leg. The central composite air inlet pipe is located at the center of the solid-state source movable sealing disc; and / or the axis of the central composite air inlet pipe is the same as the axis of the main cavity quartz tube.

2. The two-dimensional semiconductor growth system according to claim 1, characterized in that: The wafer size of the two-dimensional semiconductor is 4 to 8 inches; and / or The material of the two-dimensional semiconductor is selected from one or more of the following: transition metal sulfides, transition metal selenides, and transition metal tellurides; The first heat insulation layer is located at the edge of the furnace body and has a thickness of 20-40mm; the second heat insulation layer is located between the first heating zone and the second heating zone and has a thickness of 500-700mm; the third heat insulation layer is located between the second heating zone and the third heating zone and has a thickness of 100-200mm; the fourth heat insulation layer is located at the edge of the third heating zone and has a thickness of 60-120mm. The flange end face is mirror polished; the number of quartz sand core plates is 1 to 5; the main cavity quartz tube is made of high-purity quartz; and / or the operating temperature of the main cavity quartz tube is 1100℃ to 1200℃; and / or The insulation board is made of ceramic, and the ceramic is selected from one or more of the following: alumina ceramic, zirconium oxide ceramic, and silicon carbide ceramic.

3. The two-dimensional semiconductor growth system according to claim 2, characterized in that: The wafer size of the two-dimensional semiconductor is 8 inches; and / or The material of the two-dimensional semiconductor is selected from one or more of the following: molybdenum disulfide, tungsten disulfide, tungsten diselenide, and molybdenum diselenide; The thickness of the first heat insulation layer is 25~35mm; the thickness of the second heat insulation layer is 550~650mm; the thickness of the third heat insulation layer is 120~160mm; and the thickness of the fourth heat insulation layer is 80~100mm. The number of quartz sand core plates is 1 to 3; and / or the operating temperature of the main cavity quartz tube is 1200℃; and / or The insulation board is made of ceramic, specifically alumina ceramic and / or zirconium oxide ceramic.

4. The two-dimensional semiconductor growth system according to claim 3, characterized in that, The number of quartz sand core boards is 2.

5. The growth system for a two-dimensional semiconductor according to any one of claims 1-4, characterized in that: The first heating zone is located between the first insulation layer and the second insulation layer; The second heating zone is located between the second insulation layer and the third insulation layer; The third heating zone is located between the third insulation layer and the fourth insulation layer; and / or The first heat insulation plate includes a ceramic plate, a ceramic connecting pipe and a ceramic bolt, and the second heat insulation plate is a ceramic plate with multiple through holes.

6. The two-dimensional semiconductor growth system according to claim 5, characterized in that: The length of the first heating zone is 500~700mm; and / or the temperature of the first heating zone is 120℃~150℃; The length of the second heating zone is 500~700mm; and / or the temperature of the second heating zone is 500℃~600℃; The length of the third heating zone is 800~1200mm; and / or the temperature of the third heating zone is 900℃~950℃; and / or The type of holes in the ceramic plate of the first heat insulation board is selected from one or more of the following: bolt holes, vent holes, and air-proof holes; and / or the thickness of the second heat insulation board is 20% to 60% of its diameter.

7. The two-dimensional semiconductor growth system according to claim 6, characterized in that: The length of the first heating zone is 550~650mm; and / or the temperature of the first heating zone is 130℃~150℃; The length of the second heating zone is 550~650mm; and / or the temperature of the second heating zone is 550℃~600℃; The length of the third heating zone is 950~1100mm; and / or the temperature of the third heating zone is 900℃~930℃; and / or The thickness of the second insulation board is 25% to 50% of its diameter.

8. The growth system for a two-dimensional semiconductor according to any one of claims 1-4, characterized in that, The air intake type of the solid-state source movable sealing disc is selected from one or more of the following: high-temperature source air intake, main cavity air intake, and low-temperature source air intake; wherein: The central composite air intake pipe has the following air intake types: main cavity air intake and / or low temperature source air intake. The high-temperature source air intake pipe is of the type of high-temperature source air intake; the high-temperature source air intake pipe is arranged on the circumference of the solid source movable sealing plate; the number of high-temperature source air intake pipes is 4 to 12; and / or the distance from the high-temperature source air intake pipe to the center of the solid source movable sealing plate is 60 to 80 mm. The vacuum gauge is mounted on the first sealing plate; and / or The front of the bellows parallel plate includes a front hole and a connecting hole for the support leg, and the side includes a side hole. The support piece of the butterfly vacuum bellows is installed in the front hole of the bellows parallel plate, and the front hole of the bellows parallel plate is perpendicular to the axis of the front hole. And / or a set screw is installed on the front hole of the bellows parallel plate to connect the bellows parallel plate and the butterfly vacuum bellows.

9. The two-dimensional semiconductor growth system according to claim 8, characterized in that: The number of high-temperature source inlet pipes is 4 to 10; and / or the distance from the high-temperature source inlet pipe to the center of the solid source movable sealing plate is 70 to 80 mm.

10. The two-dimensional semiconductor growth system according to claim 9, characterized in that: The distance from the high-temperature source inlet pipe to the center of the solid-state source movable sealing plate is 75mm; and / or The vacuum gauge is a thin-film gauge.

11. The growth system for a two-dimensional semiconductor according to any one of claims 1-4, characterized in that: The longitudinal moving base includes: a first slider of the longitudinal moving base, a base plate of the longitudinal moving base, a linear guide rail of the longitudinal moving base, and a second slider of the longitudinal moving base. The transverse linear module includes: a transverse linear module base plate, a lead screw assembly, a transverse linear module linear guide rail, a transverse linear module first slider, a transverse linear module first slider adapter seat, a transverse linear module second slider, and a transverse linear module second slider adapter seat; The front side of the first sealing plate includes: a sealing groove for the first sealing plate, a central air inlet hole for the first sealing plate, an outer ring air inlet hole for the first sealing plate, and a vacuum gauge connection hole; and / or the back side of the first sealing plate includes: a threaded hole for the outer ring air inlet hole for the first sealing plate, a threaded hole for the central air inlet hole for the first sealing plate, and a locking hole for the support leg of the first sealing plate. The butterfly vacuum bellows includes: a second sealing flange for the butterfly vacuum bellows, a bellows telescopic unit, a telescopic unit connecting plate, and a first sealing flange for the butterfly vacuum bellows. The central composite air inlet pipe includes: a central composite air inlet pipe flange cavity, a quartz tube holder, a first vacuum connector, a second vacuum connector, and a low-temperature solid-state source quartz tube; The high-temperature sample inlet tube includes: a quartz tube holder, an extension tube, and a high-temperature solid-state source quartz tube; and / or The second sealing plate includes: a main body of the second sealing plate, a shaped sealing ring, a secondary plate of the second sealing plate, a vacuum connector of the second sealing plate, and a sealing ring for the high-temperature sample inlet pipe.

12. The two-dimensional semiconductor growth system according to claim 11, characterized in that, The second slider of the longitudinal moving base is connected to the transverse linear module; the base plate of the transverse linear module is connected to the longitudinal moving base; the first slider adapter is connected to the second sealing plate support leg; the second slider adapter is connected to the bellows parallel plate; the threaded hole of the outer ring air inlet of the first sealing plate is connected to the butterfly vacuum bellows; the threaded hole of the center air inlet of the first sealing plate is connected to the center composite air inlet pipe; the locking hole of the first sealing plate support leg is connected to the first sealing plate support leg; the second sealing flange of the butterfly vacuum bellows is sealed to the second sealing plate; the first sealing flange of the butterfly vacuum bellows is sealed to the first sealing plate; and / or the vacuum connector of the second sealing plate is connected to the gas path panel through a vacuum pipe.

13. The two-dimensional semiconductor growth system according to claim 11, characterized in that: The quartz tube holder and the central composite air inlet flange cavity are vacuum sealed; the quartz tube holder includes: a quartz tube holder main tube, a polytetrafluoroethylene fastening tube, a compression tube, a side sealing ring of the compression tube, a quartz tube sealing ring, a movable compression tube, and a compression nut. The side of the central composite air inlet flange cavity is a first vacuum connector; and / or The front end of the quartz tube holder is connected to the main cavity quartz tube, and its rear end is sealed to the second vacuum connector.

14. The two-dimensional semiconductor growth system according to claim 13, characterized in that: The bottom of the main tube of the quartz tube holder has a through hole, and the other end has an external thread. Its inner wall and the inner side of the bottom surface have chamfers. The polytetrafluoroethylene (PTFE) fastening tube includes a first PTFE fastening tube and a second PTFE fastening tube. The extrusion tube includes a first extrusion tube and a second extrusion tube; The first extrusion tube has a sealing ring mounting groove on its side, a raised blade in the middle of one end, and a chamfer at the other end; The structure of the second extrusion tube is the same as that of the first extrusion tube, but the installation direction is opposite. A quartz tube sealing ring is provided between the first extrusion tube and the second extrusion tube, and the quartz tube sealing ring is in chamfer contact with the first extrusion tube and the second extrusion tube; and / or The second PTFE fastening tube has the same structure as the first PTFE fastening tube, but is installed in the opposite direction.

15. The two-dimensional semiconductor growth system according to claim 14, characterized in that: The angle between the inner wall of the main tube of the quartz tube holder and the inner chamfer of the bottom surface is 45°~70°; and / or The chamfer angle at the other end of the side sealing ring mounting groove of the first extrusion tube is 10°~60°.

16. The two-dimensional semiconductor growth system according to claim 15, characterized in that: The angle between the inner wall of the main tube of the quartz tube holder and the inner chamfer of the bottom surface is 50°~65°; and / or The chamfer angle at the other end of the side sealing ring mounting groove of the first extrusion tube is 20°~50°.

17. The two-dimensional semiconductor growth system according to claim 16, characterized in that: The angle between the inner wall of the main tube of the quartz tube holder and the inner chamfer of the bottom surface is 60°; and / or The chamfer angle at the other end of the side sealing ring mounting groove of the first extrusion tube is 30°.

18. The two-dimensional semiconductor growth system according to claim 11, characterized in that: The front side of the second sealing plate main board has four sets of holes: the first threaded blind hole of the second sealing plate main board, the second threaded blind hole of the second sealing plate main board, the threaded through hole of the second sealing plate main board, and the first sealing groove of the second sealing plate main board. The back of the second sealing plate main board has a circular groove on the back of the second sealing plate main board, a second sealing groove on the second sealing plate main board, and a third threaded blind hole on the second sealing plate main board; The second sealing plate main board is sealed to the second sealing plate secondary board via the irregularly shaped sealing ring; and / or The second sealing plate vacuum connector is connected to the gas path panel via a vacuum pipe.

19. The two-dimensional semiconductor growth system according to claim 18, characterized in that: The first threaded blind hole of the second sealing plate main board is connected to the support leg of the second sealing plate; the second threaded blind hole of the second sealing plate main board is connected to the butterfly vacuum bellows; the threaded through hole of the second sealing plate main board is connected to the high-temperature sample inlet pipe; after the high-temperature sample inlet pipe sealing ring is installed in the first sealing groove of the second sealing plate main board, the high-temperature sample inlet pipe is sealed to the second sealing plate main board; and / or The second sealing plate is positioned and installed in the circular groove on the back of the main board of the second sealing plate, and a special-shaped sealing ring is installed in the second sealing groove of the main board of the second sealing plate. The third threaded blind hole of the main plate of the second sealing plate is connected to the secondary plate of the second sealing plate.

20. The growth system for a two-dimensional semiconductor according to any one of claims 1-4, characterized in that: The suction end sealing plate includes: a suction end sealing plate, a suction end sealing plate support leg, a suction end sealing plate longitudinal slider, a suction end sealing plate longitudinal linear guide rail, a suction end sealing plate base plate, and a suction end sealing plate transverse slider; wherein, the suction end sealing plate is connected to a vacuum pump via a vacuum bellows, and its back is connected to the suction end sealing plate support leg; the suction end sealing plate support leg is connected to the suction end sealing plate longitudinal slider, the suction end sealing plate longitudinal slider is mounted on the suction end sealing plate longitudinal linear guide rail, and the suction end sealing plate longitudinal linear guide rail is connected to the suction end sealing plate base plate; The quartz tube support includes: a support plate, an optical axis, an optical axis fixing seat, a quartz tube support base plate, and a quartz tube support slider; wherein, the optical axis is fixed on the support plate, the quartz tube support slider and the optical axis fixing seat are fixed on the quartz tube support base plate, and the quartz tube support base plate is fixed on the support frame; The support frame includes wheels, linear guide rails, sliders, and door panels; wherein the wheels are movably located at the bottom, the linear guide rails are located at the top center, the sliders are located on the linear guide rails, and the door panels are located on the left, right, rear, and top sides of the support frame and are openable and closable; and / or The gas circuit panel includes a mass flow meter, valves, pipe fittings, stainless steel pipe assemblies, and a mounting plate; wherein the mass flow meters are, in sequence, a first mass flow meter, a second mass flow meter, a third mass flow meter, a fourth mass flow meter, and a fifth mass flow meter, and the valves are a first valve, a second valve, and a third valve.

21. The two-dimensional semiconductor growth system according to claim 20, characterized in that: The support frame is made of one or more of the following materials: aluminum profile support, welded square tube support, optical platform; The door panel is made of one or more of the following materials: iron plate, stainless steel plate, acrylic plate, and aluminum plate; The pipe fitting and the stainless steel pipe assembly connect the mass flow meter and the valve; and / or The gas passage panel is mounted on the support frame.

22. The two-dimensional semiconductor growth system according to claim 21, characterized in that, The support frame is an aluminum profile bracket or an optical platform.

23. The growth system for a two-dimensional semiconductor according to any one of claims 1-4, characterized in that, The two-dimensional semiconductor growth system further includes: a vacuum pump, an exhaust gas treatment system, and a control unit; wherein, The vacuum pump is a corrosion-resistant oil-sealed rotary vane pump or a dry scroll pump; and / or The exhaust gas treatment system is an alkaline solution tank, and the alkaline solution is selected from one or more of the following: NaOH solution, KOH solution, and NaHCO3 solution.

24. The two-dimensional semiconductor growth system according to claim 23, characterized in that, The vacuum pump is a corrosion-resistant oil-sealed rotary vane pump.

25. A method for growing a two-dimensional semiconductor, characterized in that, The method uses the growth system of any one of claims 1-24 and includes the following steps: (1) Pre-treat the substrate, and place the pre-treated substrate in the third heating zone; (2) Place the solid source in the first heating zone, place the metal source at the front end of the quartz tube, introduce carrier gas, and heat up; (3) After the temperatures of the three zones stabilize, the metal source is moved to the second heating zone for growth to obtain the first two-dimensional semiconductor layer. The carrier gas supply is stopped, and the first two-dimensional semiconductor layer is moved to the first heating zone; and (4) Heat up and wait for the temperature to stabilize. Then introduce carrier gas and move the first layer of two-dimensional semiconductor to the second heating zone for growth. After cooling to room temperature, the two-dimensional semiconductor is obtained.

26. The method according to claim 25, characterized in that: In step (1), after pre-treating the substrate, the method further includes: placing the annealed substrate on a tray, and placing the tray containing the sapphire substrate in the third heating zone; and / or Step (2) further includes pressing the metal source into a sheet and placing it at the front end of a quartz tube that is evenly distributed around it, ensuring that it is far away from the second heating zone.

27. The method according to claim 26, characterized in that: In step (1), the substrate is selected from one or more of the following: sapphire, silicon, silicon dioxide, quartz, mica, silicon carbide; and / or In step (2), the amount of the solid source is 8~12g; and / or the amount of the metal source is 40~60mg.

28. The method according to claim 27, characterized in that, In step (2), the amount of the solid source is 9~11g; and / or the amount of the metal source is 45~55mg.

29. The method according to claim 28, characterized in that, In step (2), the amount of the solid source is 10g; and / or the amount of the metal source is 50mg.

30. The method according to any one of claims 25-29, characterized in that: In step (3), the carrier gases in the first heating zone, the second heating zone, and the third heating zone are different; and / or In step (3), the time for moving the metal source to the second heating zone for growth is 25-50 minutes; and / or In step (4), the time for moving the first layer of two-dimensional semiconductor to the second heating zone for growth is 35 to 70 minutes.

31. The method according to claim 30, characterized in that: In step (3), the time for moving the metal source to the second heating zone for growth is 25-45 minutes; and / or In step (4), the time for moving the first layer of two-dimensional semiconductor to the second heating zone for growth is 30 to 65 minutes.

32. The method according to claim 31, characterized in that: In step (3), the time for moving the metal source to the second heating zone for growth is 30-40 minutes; and / or In step (4), the time for moving the first layer of two-dimensional semiconductor to the second heating zone for growth is 40 to 60 minutes.

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