A MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN
By employing the synergistic effect of a gradient magnetic field confinement module and an Ar isolation gas curtain module within the MOCVD reaction chamber, combined with a four-layer gradient composite coating, the problems of atmosphere compatibility and cross-contamination in the in-situ heterogeneous integration of Ga2O3 and GaN were solved, achieving efficient atmosphere isolation and improved device performance.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- XIDIAN UNIV
- Filing Date
- 2026-03-20
- Publication Date
- 2026-06-05
AI Technical Summary
Existing MOCVD equipment is difficult to be compatible with in-situ heterogeneous integration of Ga2O3 and GaN, resulting in poor atmosphere compatibility, safety risks, carbon contamination, cross-contamination, and the inability to achieve in-situ heterogeneous integration, leading to poor device performance consistency and high production costs.
A MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN was designed. The gradient magnetic field confinement module and Ar isolation gas curtain module work together to achieve intrinsic spatial partitioning and physical barrier of the atmosphere. Combined with a four-layer gradient composite coating, the atmosphere is isolated and cross-contamination is prevented.
It achieves permanent and stable isolation between H2 and O2 atmospheres with a separation efficiency of ≥99.9%, completely eliminating the risk of explosion and cross-contamination from hydrogen-oxygen contact, improving device performance consistency and production efficiency, and reducing equipment investment and production costs.
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Figure CN122147515A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of semiconductor technology, specifically relating to an MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN. Background Technology
[0002] Ultra-wide bandgap semiconductor material Ga2O3 possesses excellent high-voltage resistance, low leakage current, and high breakdown field strength, while wide bandgap semiconductor material GaN exhibits outstanding high-frequency, low-loss, and high thermal conductivity. In-situ heterogeneous integration of these two materials is a core technological path for breaking through performance bottlenecks in next-generation high-end semiconductor devices, possessing strong industrial necessity and irreplaceable technological advantages. Through in-situ heterogeneous integration of GaN and Ga2O3, devices can simultaneously achieve high-frequency and high-voltage performance, significantly improving power density, energy efficiency, and operational reliability, while significantly reducing device size and system integration complexity, perfectly meeting the application needs of high-end fields such as 5G communication, new energy power generation, and aerospace.
[0003] Typically, GaN epitaxial growth requires a reducing atmosphere of NH3 / H2 at 900-1200℃, while Ga2O3 epitaxial growth requires a strong oxidizing atmosphere of O2 at 400-800℃. These two atmospheres not only present completely contradictory requirements for the chemical stability of the chamber coating but also pose a safety risk due to hydrogen-oxygen mixing. Existing MOCVD equipment is difficult to integrate Ga2O3 and GaN in situ, thus necessitating a MOCVD reaction chamber compatible with both Ga2O3 and GaN in situ heterogeneous integration. Summary of the Invention
[0004] To address the aforementioned problems in the prior art, this invention provides an MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN. The technical problem to be solved by this invention is achieved through the following technical solution: This invention provides an MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN, including a reaction chamber, an atmosphere isolation system and a sample translation base inside the reaction chamber, the atmosphere isolation system including a gradient magnetic field confinement module and an Ar isolation gas curtain module; The Ar isolation gas curtain module is located in the middle of the reaction chamber and is used to form an isolation gas curtain in the reaction chamber to divide the reaction chamber into a left chamber and a right chamber. The gradient magnetic field confinement module is located on the side of the right chamber away from the Ar isolation gas curtain module, and is used to generate a magnetic effect on the gas in the right chamber. The left chamber is equipped with a GaN spray head, which is connected to a TMGa gas path, an NH3 gas path, an H2 gas path, and a TMAl doping gas path. The right chamber is equipped with a Ga2O3 spray head, which is connected to a TEGa gas path, an Ar gas path, a doping gas path, and an O2 / O3 gas path. The sample translation base is used to support the sample and move it between the left and right chambers.
[0005] In one embodiment of the present invention, the inner wall of the reaction chamber is provided with four layers of gradient composite coating, the four layers of gradient composite coating including a first layer, a second layer, a third layer and a fourth layer stacked sequentially from the outside to the inside; The first layer is a low surface energy, fully amorphous, multi-component metal oxynitride composite passivation layer; the second layer is a high-density SiC covalent ceramic corrosion-resistant layer; the third layer is a lattice-free carbon nitride / oxynitride-based carbon diffusion barrier layer; and the fourth layer is a high-purity isostatically pressed carbon matrix layer.
[0006] In one embodiment of the present invention, the material of the first layer includes one of the following: rare earth-aluminum-based amorphous oxynitride system, rare earth-silicon-aluminum-based amorphous oxynitride system, high melting point transition metal-aluminum-based amorphous oxynitride system, and alkaline earth metal-aluminum-based amorphous oxynitride system. Rare earth-aluminum based amorphous oxynitride systems include the following: amorphous Y-Al-ON, amorphous Sc-Al-ON, amorphous La-Al-ON, amorphous Gd-Al-ON, and amorphous Yb-Al-ON.
[0007] In one embodiment of the present invention, the material of the third layer includes one of the following: a binary nitride system, a ternary or higher composite nitride system, a rare earth composite oxynitride system, and a transition metal composite oxynitride system; Binary nitride systems include the following: nanocrystalline α-Si3N4, nanocrystalline β-Si3N4, and nanocrystalline AlN.
[0008] In one embodiment of the present invention, the gradient magnetic field confinement module includes multiple permanent magnets arranged in an array, wherein the surface remanence of a single permanent magnet is greater than or equal to 1.45T, the surface magnetic field of the gradient magnetic field confinement module is greater than or equal to 1.4T, and the magnetic field gradient of the effective working area of the right chamber is greater than or equal to 150T / m. The exterior of the multiple permanent magnets is sequentially fitted with a non-magnetic stainless steel protective cover and a water-cooled heat dissipation sleeve.
[0009] In one embodiment of the present invention, the Ar isolation air curtain module includes multiple linear nozzle assemblies, the nozzle gap width of the linear nozzle assembly is 0.3mm-0.5mm, and the outlet pressure of the linear nozzle assembly is 0.02mbar-0.05mbar higher than the cavity pressure in the left and right chambers.
[0010] In one embodiment of the present invention, both the left and right chambers are provided with air extraction ports on the side away from the Ar isolation air curtain module, and the air extraction ports are connected to external air extraction pumps.
[0011] In one embodiment of the present invention, an NH3 preheating unit is provided in the left chamber, and the temperature control range of the NH3 preheating unit is 900-1200℃.
[0012] In one embodiment of the present invention, an O2 concentration stabilization unit is provided in the right chamber, and the temperature control range of the O2 concentration stabilization unit is 400-1000℃.
[0013] In one embodiment of the present invention, the sample translation base includes a linear drive assembly and a base body. The linear drive assembly is arranged along the length direction of the reaction chamber. The base body is mounted on the linear drive assembly. The base body is provided with a thermocouple and two Cr-Mo-Si alloy heating tapes. The thermocouple is located between the two Cr-Mo-Si alloy heating tapes. The outer side of the base body is also provided with a heat insulation layer. The heat insulation layer is provided with a spiral cooling pipe. The base body is also equipped with a magnetohydrodynamic sealing rotation mechanism.
[0014] Compared with the prior art, the beneficial effects of the present invention are as follows: In the above-described scheme of this application, the MOCVD reaction chamber includes a reaction chamber, within which an atmosphere isolation system and a sample translation base are provided. The atmosphere isolation system includes a gradient magnetic field confinement module and an Ar isolation gas curtain module. The Ar isolation gas curtain module is located in the middle of the reaction chamber and is used to form an isolation gas curtain within the reaction chamber to divide the reaction chamber into a left chamber and a right chamber. The gradient magnetic field confinement module is located in the right chamber on the side away from the Ar isolation gas curtain module and is used to generate a magnetic attraction effect on the gas in the right chamber. A GaN spray head is provided in the left chamber, and the GaN spray head is connected to a TMGa gas path, an NH3 gas path, an H2 gas path, and a TMAl doping gas path. A Ga2O3 spray head is provided in the right chamber, and the Ga2O3 spray head is connected to a TEGa gas path, an Ar gas path, a doping gas path, and an O2 / O3 gas path. The sample translation base is used to carry the sample and move the sample between the left and right chambers. This structure, firstly, utilizes the intrinsic magnetic susceptibility difference between the strong paramagnetism of O2 and the weak diamagnetics of H2 / NH3, allowing the gradient magnetic field confinement module to generate directional volume forces on the paramagnetic gas, achieving intrinsic spatial partitioning confinement of the two atmospheres and suppressing lateral diffusion at the source of gas characteristics. Secondly, the gas curtain ejected by the Ar isolation gas curtain module forms a physical barrier, preventing gas contact between the left and right chambers. Through the synergistic cooperation of the gradient magnetic field confinement module and the Ar isolation gas curtain module, non-contact, permanent, and stable isolation between H2-based and O2-based atmospheres is achieved, with a separation efficiency ≥99.9%, completely eliminating the explosion risk and cross-contamination associated with hydrogen-oxygen contact, and realizing in-situ heterogeneous integration compatible with Ga2O3 and GaN.
[0015] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description
[0016] Figure 1 This is a schematic diagram of the MOCVD reaction chamber provided in an embodiment of the present invention; Figure 2 This is a schematic diagram of the air path system and spray head system in an embodiment of the present invention; Figure 3 This is a schematic diagram of the sample translation base in an embodiment of the present invention; Figure 4 This is a schematic diagram of the gradient magnetic field constraint module in an embodiment of the present invention; Figure 5 This is a schematic diagram of the Ar isolation air curtain module in an embodiment of the present invention; Figure 6 This is a schematic diagram of a four-layer gradient composite coating in an embodiment of the present invention.
[0017] Reference numerals: 10-Ar isolation gas curtain module, 11-sample translation base, 12-graphite concave stage, 13-graphite protrusion, 14-movable base, 15-four-layer gradient composite coating, 16-reaction chamber, 17-gradient magnetic field confinement module, 18-extraction port, 19-graphite tray, 20-heating tube, 21-thermocouple, 22-magnetic fluid sealing rotation mechanism, 23-insulation layer, 24-spiral cooling pipeline, 25-movable gear shaft seat. Detailed Implementation
[0018] The present invention will be further described in detail below with reference to specific embodiments, but the implementation of the present invention is not limited thereto.
[0019] Ultra-wide bandgap semiconductor material Ga2O3 (bandgap ~4.8eV) possesses excellent high voltage resistance, low leakage current, and high breakdown field strength, while wide bandgap semiconductor material GaN (bandgap ~3.4eV) exhibits outstanding high frequency, low loss, and high thermal conductivity. In-situ heterogeneous integration of these two materials is a core technological path for breaking through performance bottlenecks in next-generation high-end semiconductor devices, possessing strong industrial necessity and irreplaceable technological advantages. Through in-situ heterogeneous integration of GaN and Ga2O3, devices can simultaneously achieve high-frequency and high-voltage performance, significantly improving power density, energy efficiency, and operational reliability, while significantly reducing device size and system integration complexity, perfectly meeting the application needs of high-end fields such as 5G communication, new energy power generation, and aerospace.
[0020] MOCVD technology is the core equipment for achieving high-quality epitaxial growth and in-situ heterogeneous integration of GaN and Ga2O3. The reaction chamber, as a core component of MOCVD equipment, directly determines the purity, thickness uniformity, and interface quality of the epitaxial film through its structural design, atmosphere isolation capability, coating performance, and temperature control accuracy, thus affecting device performance and the yield of in-situ heterogeneous integration. However, current MOCVD equipment and reaction chamber structures generally suffer from the following insurmountable core technological bottlenecks, severely hindering the industrialization of GaN / Ga2O3 in-situ heterogeneous integration technology: First, the atmosphere compatibility and isolation capabilities are extremely poor, posing a fatal safety risk. GaN epitaxial growth requires a reducing atmosphere of NH3 / H2 at 900-1200℃, while Ga2O3 epitaxial growth requires a strong oxidizing atmosphere of O2 at 400-800℃. These two atmospheres not only completely contradict the chemical stability requirements of the cavity coating, but also pose a fatal safety risk of hydrogen-oxygen mixture explosion. Existing single-chamber equipment can only reduce residual atmosphere through conventional processes such as repeated vacuuming and high-purity Ar purging. This not only results in a long switchover time of 1-2 hours and extremely low mass production efficiency, but also fails to completely eliminate the possibility of hydrogen-oxygen contact, without any structural innovation or isolation effect. Existing dual-chamber discrete equipment requires removing the substrate from the chamber and transferring it to another device, which not only introduces atmospheric pollution and damages the cleanliness of the heterogeneous interface, but also has the problems of large equipment investment, large footprint, and high production threshold. Existing physical gate and single gas curtain isolation solutions have problems such as gate sealing failure and poor gas curtain anti-disturbance ability, which cannot achieve long-term stable atmosphere isolation, and have not formed a dual synergistic system of "intrinsic constraint plus physical barrier", resulting in insufficient isolation reliability.
[0021] Secondly, carbon contamination in the graphite matrix cannot be completely eliminated, severely damaging the performance of Ga2O3 materials. Current MOCVD reaction chambers mostly use graphite as both the chamber and substrate. At high temperatures, carbon elements in graphite readily diffuse outwards, directly incorporating into the Ga2O3 epitaxial film, causing severe carbon doping contamination. This leads to Ga2O3 lattice distortion, increased leakage current, and a sharp decrease in breakdown field strength, completely failing to meet the intrinsic purity requirements of high-end devices. Existing technologies only coat the graphite matrix with a SiC coating, but the SiC lattice itself contains 50% carbon. At high temperatures, carbon exhibits intrinsic self-diffusion behavior, which cannot completely block the outward migration of carbon elements, thus failing to address the carbon contamination problem at its root.
[0022] Third, cross-contamination and memory effect are prominent, resulting in poor device performance consistency. The cavity walls and gas paths of existing single-cavity devices are prone to adsorbing organometallic precursors such as TMGa and TEGa, forming a serious process memory effect. Cross-contamination is easily generated when switching between the growth of the two materials, resulting in large fluctuations and poor consistency in the performance of epitaxial films. The yield of in-situ heterogeneous integration is less than 30%, which is completely unsuitable for industrial mass production requirements.
[0023] Fourth, true in-situ heterogeneous integration cannot be achieved. Current technologies cannot achieve continuous in-situ growth of GaN and Ga2O3 within the same cavity without opening or changing the cavity. Instead, heteroepitaxial growth followed by bonding is used. This method not only introduces problems such as interface contamination and exacerbated lattice mismatch, significantly reducing device reliability and performance limits, but also increases process complexity and production costs, completely failing to leverage the technological advantages of in-situ heterogeneous integration.
[0024] The aforementioned bottlenecks, coupled with the necessity of in-situ heterogeneous integration, result in particularly prominent comprehensive consequences: On the one hand, companies need to invest huge sums of money to purchase two independent machines, significantly increasing equipment investment, floor space, and production barriers. Moreover, they cannot achieve continuous in-situ growth of both, and can only use heteroepitaxial growth followed by bonding as an alternative. This method not only introduces problems such as interface contamination and exacerbated lattice mismatch, significantly reducing the reliability and performance limits of devices, but also increases process complexity and production costs. On the other hand, even if attempts are made to modify single-cavity equipment for compatible growth, problems such as contamination and temperature control imbalance will lead to a significant decline in product qualification rate, further restricting the industrialization process of Ga2O3 and GaN in-situ heterogeneous integration technology. This makes it impossible to meet the market's demand for large-scale high-end integrated devices and limits the upgrading and breakthrough of the wide-bandgap semiconductor industry towards high-value-added fields.
[0025] Therefore, developing an MOCVD reaction chamber structure that can achieve stable and compatible growth of GaN and Ga2O3 in a single chamber, support in-situ heterogeneous integration, and solve the core pain points of hydrogen-oxygen atmosphere isolation, carbon contamination, and cross-contamination from the structural root through the synergistic effect of gradient magnetic field and linear isolation gas curtain has become a technical challenge that the wide bandgap semiconductor industry urgently needs to solve.
[0026] Based on the above issues, please refer to Figures 1 to 6This invention provides an MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN, including a reaction chamber 16. The reaction chamber 16 is equipped with an atmosphere isolation system and a sample translation base 11. The atmosphere isolation system includes a gradient magnetic field confinement module 17 and an Ar isolation gas curtain module 10. The Ar isolation gas curtain module 10 is located in the middle of the reaction chamber 16 and is used to form an isolation gas curtain within the reaction chamber 16 to divide the reaction chamber 16 into a left chamber and a right chamber. The gradient magnetic field confinement module 17 is located in the right chamber. The side furthest from the Ar isolation gas curtain module 10 is used to generate a magnetic effect on the gas in the right chamber; the left chamber is equipped with a GaN spray head, which is connected to a TMGa gas path, an NH3 gas path, an H2 gas path, and a TMAl doped gas path; the right chamber is equipped with a Ga2O3 spray head, which is connected to a TEGa gas path, an Ar gas path, a doped gas path, and an O2 / O3 gas path; the sample translation base 11 is used to carry the sample and move the sample between the left and right chambers.
[0027] In some embodiments of this application, the cavity is integrally formed from 316L non-magnetic austenitic stainless steel, and the use of ferromagnetic materials is strictly prohibited to avoid magnetic field distortion and ensure uniform and stable magnetic field distribution of the gradient magnetic field confinement module. The cavity adopts a flat rectangular structure with a cross-sectional width-to-height ratio ≥4:1, which can enhance the uniform coverage of the magnetic field and suppress vertical convection disturbances, providing an optimal cavity environment for laminar flow stability, magnetic field separation, and linear air curtain isolation. The cavity is completely empty, without any built-in physical obstructions, gates, or other structures, which does not affect the lateral translation of the sample base and avoids interference from structural components on atmosphere flow and magnetic field distribution. All opening and closing parts of the cavity, gas path inlets, lead wire outlets, and drive mechanisms are sealed with conventional high-vacuum flanges, and the cavity's base vacuum is ≤1×10⁻⁶. -5 mbar ensures the cavity's airtightness and cleanliness.
[0028] In the above-described scheme of this application, the MOCVD reaction chamber includes a reaction chamber 16, which is equipped with an atmosphere isolation system and a sample translation base 11. The atmosphere isolation system includes a gradient magnetic field confinement module 17 and an Ar isolation gas curtain module 10. The Ar isolation gas curtain module 10 is located in the middle of the reaction chamber 16 and is used to form an isolation gas curtain in the reaction chamber 16 to divide the reaction chamber 16 into a left chamber and a right chamber. The gradient magnetic field confinement module 17 is located on the side of the right chamber away from the Ar isolation gas curtain module 10 and is used to generate a magnetic attraction effect on the gas in the right chamber. A GaN spray head is provided in the left chamber, and the GaN spray head is connected to a TMGa gas path, an NH3 gas path, an H2 gas path, and a TMAl doping gas path. A Ga2O3 spray head is provided in the right chamber, and the Ga2O3 spray head is connected to a TEGa gas path, an Ar gas path, a doping gas path, and an O2 / O3 gas path. The sample translation base 11 is used to carry the sample and move the sample between the left and right chambers. This structure, firstly, utilizes the intrinsic magnetic susceptibility difference between the strong paramagnetism of O2 and the weak diamagneticism of H2 / NH3, allowing the gradient magnetic field confinement module 17 to generate directional volume forces on the paramagnetic gas, achieving intrinsic spatial partitioning confinement of the two atmospheres and suppressing lateral diffusion at the source of gas characteristics. Secondly, the gas curtain ejected by the Ar isolation gas curtain module 10 forms a physical barrier, preventing contact between the gases in the left and right chambers. Through the synergistic cooperation of the gradient magnetic field confinement module 17 and the Ar isolation gas curtain module 10, non-contact, permanent, and stable isolation between the H2 and O2 atmospheres is achieved, with a separation efficiency ≥99.9%, completely eliminating the explosion risk and cross-contamination associated with hydrogen-oxygen contact, and realizing in-situ heterogeneous integration compatible with Ga2O3 and GaN.
[0029] In some embodiments of this application, such as Figure 1 , Figure 2 , Figure 4 and Figure 5 As shown, the atmosphere isolation system is the core for achieving stable isolation of hydrogen and oxygen atmospheres and ensuring in-situ heterogeneous integration. It consists of a gradient magnetic field confinement module and a linear Ar isolation gas curtain module. The two work together and complement each other, serving as the core support for atmosphere isolation. Based on the dual effects of the intrinsic properties of the gas and dynamic physical barrier, it achieves complete isolation of the two atmospheres, completely eliminating cross-contamination and safety risks.
[0030] In some embodiments of this application, such as Figure 1 As shown, the gradient magnetic field confinement module 17 includes multiple permanent magnets arranged in an array. The surface remanence of a single permanent magnet is greater than or equal to 1.45T, the surface magnetic field of the gradient magnetic field confinement module 17 is greater than or equal to 1.4T, and the magnetic field gradient of the effective working area of the right chamber is greater than or equal to 150T / m. The multiple permanent magnets are sequentially covered with a non-magnetic stainless steel protective cover and a water-cooled heat dissipation sleeve.
[0031] In some embodiments of this application, the gradient magnetic field confinement module is based on the intrinsic magnetic susceptibility difference between the strong paramagnetism of O2 and the weak diamagneticism of H2 / NH3 (the molar magnetic susceptibility difference between the two is nearly 1000 times). It generates directional volume forces on the paramagnetic gas through a strong gradient magnetic field, achieving intrinsic spatial partitioning confinement of the two atmospheres and suppressing lateral diffusion from the root cause of gas characteristics. The specific structure is as follows: First, a single-sided strong-field Halbach permanent magnet array is adopted, which can maximize the magnetic field on one side and cancel the magnetic field on the back side, maximizing the magnetic field gradient inside the cavity (a core isolation indicator) while avoiding interference from the magnetic field to external equipment; the permanent magnets are made of sintered neodymium iron boron N52 material, with a remanence of ≥1.45T on the surface of a single magnet and a magnetic field of ≥1.4T on the surface of the array as a whole, ensuring magnetic field confinement capability. Secondly, the Halbach permanent magnet array is fixed to the outer right wall of the cavity (on the side of the Ga2O3 dedicated growth area), and runs through the entire cavity along the length of the cavity, covering the entire range of the left and right dual areas, ensuring that the magnetic field constraint covers the entire working area; the strong magnetic field surface of the array faces the inside of the cavity, forming a stable high magnetic field gradient field in the right region of the cavity, and the magnetic field gradient of the effective working area inside the cavity is ≥150T / m, which meets the directional constraint requirements of O2. Furthermore, the magnet array is equipped with a non-magnetic stainless steel protective cover and a water-cooling jacket to prevent the magnets from demagnetizing due to high cavity temperature, ensuring that the magnets operate at a temperature ≤80℃ and that the magnetic field performance remains stable over a long period of time. The magnet array adopts a modular splicing design, which can be flexibly adjusted according to the cavity length to adapt to mass production equipment of different sizes and improve versatility. Furthermore, the strong gradient magnetic field exerts a directional attraction on the paramagnetic O2, firmly confining it to the high magnetic field region on the right (Ga2O3 growth region); at the same time, it exerts a repulsive force on the antimagnetic H2 / NH3, restricting it to the non-magnetic region on the left (GaN growth region). This achieves spatial partitioning based on the intrinsic properties of the gas, laying the foundation for the physical barrier of the subsequent linear gas curtain.
[0032] In some embodiments of this application, such as Figure 1 , Figure 2 , Figure 4 and Figure 5As shown, the gradient magnetic field confinement module is responsible for achieving intrinsic spatial partitioning confinement of the two atmospheres, suppressing lateral diffusion from the root of gas characteristics, and initially separating O2 and H2 / NH3 into two regions on the left and right. The linear Ar isolation gas curtain module is responsible for constructing a physical dynamic isolation barrier, utilizing the inert properties of high-purity Ar and the pressure difference to block the cross-regional diffusion of trace gases. At the same time, a vacuum pump promptly removes any potentially leaked trace gases. Both are important components of the atmosphere isolation system, working synergistically and providing dual protection. Combined with the stable laminar flow state within the cavity to suppress convective mixing, permanent and stable separation of the two atmospheres is achieved in a completely empty cavity, completely eliminating the risk of residual gas cross-regional contamination and hydrogen-oxygen contact, providing core protection for in-situ heterogeneous integration of two materials.
[0033] In some embodiments of this application, the Ar isolation air curtain module 10 includes multiple linear nozzle assemblies, the nozzle slit width of the linear nozzle assembly is 0.3mm-0.5mm, and the outlet pressure of the linear nozzle assembly is 0.02mbar-0.05mbar higher than the cavity pressure in the left and right chambers.
[0034] In some embodiments of this application, an air extraction port 18 is provided on the side of the left and right chambers away from the Ar isolation air curtain module 10, and an external air extraction pump is connected to the air extraction port 18.
[0035] In some embodiments of this application, an NH3 preheating unit is provided in the left chamber, and the temperature control range of the NH3 preheating unit is 900-1200℃.
[0036] In some embodiments of this application, an O2 concentration stabilization unit is provided in the right chamber, and the temperature control range of the O2 concentration stabilization unit is 400-1000℃.
[0037] In some embodiments of this application, the cavity is divided into a left-side diamagnetic atmosphere growth region (GaN-specific) and a right-side paramagnetic atmosphere growth region (Ga2O3-specific) by an atmosphere isolation system. The two regions are configured as independent systems with full-link physical isolation, without any shared pipelines or components, completely eliminating the possibility of hydrogen-oxygen contact, while simultaneously meeting the different growth process requirements of the two materials, as detailed below: In some embodiments of this application, the left-side GaN-dedicated growth area is equipped with: a GaN-specific retractable spray head, independently connected to the TMGa / NH3 / H2 gas path and the TMAl doping gas path, and equipped with an NH3 preheating unit to ensure stable NH3 gas temperature and improve the quality of the GaN epitaxial layer; the spray height adjustment range is 10~100mm, with an adjustment accuracy of ±0.1mm, which can adapt to different growth process requirements; an independent high-temperature temperature control module is configured to stably maintain 900-1200℃, with regional temperature uniformity ≤±2℃, ensuring the temperature stability of GaN epitaxial growth; a fully independent vacuum pumping system is configured, consisting of an independent turbomolecular pump, a rotary vane forepump, a two-stage isolation valve, and a vacuum monitoring gauge, to ensure stable vacuum; and an independent ammonia-hydrogen-specific exhaust gas treatment system is configured, with the exhaust chimney completely independent from the right-side system to avoid cross-contamination of exhaust gas.
[0038] In some embodiments of this application, the right-side Ga2O3 dedicated growth area is equipped with: a dedicated Ga2O3 retractable spray head, independently connected to the TEGa / O2 / Ar gas path and the Cp2Mg doping gas path, and equipped with an O2 concentration stabilization unit to ensure O2 concentration fluctuation ≤ ±5g / m³, thereby improving the purity of the Ga2O3 epitaxial layer; the spray height adjustment range is 10~100mm, with an adjustment accuracy of ±0.1mm, adapting to different growth processes; an independent medium-low temperature control module is configured to stably maintain 400-1000℃, with regional temperature uniformity ≤ ±2℃, meeting the temperature requirements for Ga2O3 epitaxial growth; a fully independent vacuum pumping system is configured, consisting of an independent turbomolecular pump, an oil-free vortex dry pump, a two-stage isolation valve, and a vacuum monitoring gauge, avoiding oil contamination; and an independent oxygen-enriched dedicated exhaust gas treatment system is configured, with the exhaust chimney completely independent of the left-side system, ensuring safe and compliant exhaust gas treatment.
[0039] In some embodiments of this application, the process gas flow rates in the left and right zones are strictly controlled by high-precision MFC, with flow fluctuations ≤ ±1%, ensuring that the Reynolds number Re < 800 for gas flow within the cavity, maintaining a stable laminar flow state throughout, and avoiding turbulence from damaging the atmosphere partition and air curtain barrier; both the left and right zones adopt a flow field design of "top vertical spray - bottom coaxial independent pumping", after the process gas flows vertically downwards, it is directly pumped away by the independent vacuum pump of the corresponding zone, without lateral diffusion power, further enhancing the constraint effect of the atmosphere isolation system; a three-level hard interlock control is set to ensure the safe operation of the equipment.
[0040] In some embodiments of this application, the sample translation base 11 includes a linear drive assembly and a base body. The linear drive assembly is arranged along the length direction of the reaction chamber 16. The base body is mounted on the linear drive assembly. The base body is provided with a thermocouple 21 and two Cr-Mo-Si alloy heating tapes 20. The thermocouple 21 is located between the two Cr-Mo-Si alloy heating tapes 20. The outer side of the base body is also provided with a heat insulation layer 23. The heat insulation layer 23 is provided with a spiral cooling pipe 24. The base body is also provided with a magnetic fluid sealing rotation mechanism 22.
[0041] In some embodiments of this application, such as Figure 1 and Figure 2 As shown, the base body includes a graphite recess 12, a graphite boss 13, and a movable base 14, with a graphite tray 19 mounted on the graphite recess 12. The sample translation base 11 can also move the gear shaft seat 25.
[0042] In some embodiments of this application, the reaction chamber 16 is fully compatible with the requirements of dual-region in-situ growth, has no design conflict with the atmosphere isolation system, and can realize a smooth switching of the substrate between the two growth regions, avoiding contamination and damage during the substrate transfer process. The specific structure is as follows: First, the translation drive adopts a magnetically coupled non-contact linear drive system, eliminating the risk of dynamic sealing and vacuum leakage, and ensuring stable vacuum in the cavity. A high-precision linear motor module is set on the outer side of the bottom of the cavity, and a translation slide is set on the inner side of the cavity, which is magnetically coupled to the motor. The base is fixed on the slide, and the high-precision guide rail moves linearly along the length of the cavity. The translation stroke completely covers the left and right growth areas, and the translation positioning accuracy is ±0.1mm, ensuring that the substrate and the corresponding spray head are coaxially aligned, thus improving the uniformity of the epitaxial layer thickness.
[0043] Secondly, the base body consists of a top graphite protrusion 13 and a bottom 316L stainless steel nitrided body, balancing heat conduction efficiency and structural stability. The height of the graphite protrusion 13 is interference-fitted with the concave structure of the graphite tray 19, achieving a heat conduction efficiency of ≥90% and ensuring uniform substrate temperature. Two symmetrically arranged Cr-Mo-Si alloy heating tapes 20 are embedded in the surface of the graphite protrusion 13, with a single-section power of 0.8~2.5kW and a temperature resistance of ≥1300℃. The power can be independently adjusted to compensate for heat loss at the substrate edge and improve substrate temperature uniformity. A K-type armored thermocouple 21 is embedded between the two heating tapes 20, integrated with the heating tapes 20, with a temperature measurement range of 400-1200℃, a temperature measurement accuracy of ±1℃, and a response time of ≤5s, realizing single-point zoned temperature control and accurately adapting to the different growth temperature requirements of the two zones.
[0044] And, as Figure 1 and Figure 3As shown, a 1cm thick alumina ceramic heat insulation layer 23 with a thermal conductivity of 1.0~1.5W / (m·K) is tightly attached to the outside of the graphite boss 13 to reduce heat diffusion to the outside of the cavity and reduce energy consumption. The heat insulation layer 23 has an embedded spiral cooling pipe 24, which uses liquid nitrogen and ethylene glycol dual media switching, with a flow rate adjustable from 0 to 5L / min. The cooling pipe is 1cm away from the graphite boss 13 to achieve physical isolation between heating and cooling and avoid temperature interference. The base is equipped with a magnetohydrodynamic sealing rotation mechanism 22 with an adjustable rotation speed of 0~30rpm and a speed accuracy of ±0.1rpm to ensure uniform distribution of process gas on the substrate surface and improve the quality of the epitaxial layer.
[0045] In some embodiments of this application, such as Figure 1 and Figure 6 As shown, the inner wall of the reaction chamber 16 is provided with a four-layer gradient composite coating 15. The four-layer gradient composite coating 15 includes a first layer, a second layer, a third layer and a fourth layer stacked sequentially from the outside to the inside. The first layer is a low surface energy fully amorphous multi-component metal oxynitride composite passivation layer, the second layer is a high-density SiC covalent ceramic corrosion-resistant layer, the third layer is a lattice-free carbon nitride / oxynitride-based carbon diffusion barrier layer, and the fourth layer is a high-purity isostatic carbon matrix layer.
[0046] In some embodiments of this application, such as Figure 1 and Figure 6 As shown, the inner wall of the cavity body and the surfaces of all components in contact with the atmosphere (spray head, base, tray, air curtain nozzle, etc.) are fully covered with four layers of gradient composite coating 15, arranged sequentially from the side of the cavity to the substrate. Each layer is a type of material with uniform functional characteristics. The functions of each layer are coordinated and the thermal expansion coefficients are matched. This not only completely solves the problem of carbon pollution in the graphite matrix, but also perfectly accommodates both reducing and oxidizing extreme atmospheres. At the same time, the low surface energy design eliminates the adsorption and memory effect of precursors, and works in conjunction with the atmosphere isolation system to achieve no cross-contamination.
[0047] In some embodiments of this application, the material of the first layer includes one of the following: rare earth-aluminum-based amorphous oxynitride system, rare earth-silicon-aluminum-based amorphous oxynitride system, high melting point transition metal-aluminum-based amorphous oxynitride system, and alkaline earth metal-aluminum-based amorphous oxynitride system; the rare earth-aluminum-based amorphous oxynitride system includes one of the following: amorphous Y-Al-ON, amorphous Sc-Al-ON, amorphous La-Al-ON, amorphous Gd-Al-ON, and amorphous Yb-Al-ON.
[0048] In some embodiments of this application, the first layer is a type of completely amorphous multi-component metal oxynitride ceramic material with low surface energy core characteristics. It is the outermost protective layer that directly contacts the process atmosphere and is also the core layer for solving precursor adsorption, memory effect, and cross-contamination. Its core design priority is: low surface energy > amorphous defect-free structure > dual-atmosphere chemical stability.
[0049] In some embodiments of this application, the surface energy is extremely low (the first core feature): the surface energy at room temperature is ≤30mJ / m², and the optimal surface energy can reach 22~28mJ / m², which is far lower than the surface energy of conventional crystalline SiC coatings (>60mJ / m²). The physical and chemical adsorption effects on MOCVD organometallic precursors such as TMGa, TEGa, TMAl, and Cp2Mg are extremely weak, making them difficult to adhere to and leave residues. Combined with cavity purging, residual precursors can be 100% removed, completely eliminating process memory effects and cross-contamination.
[0050] In some embodiments of this application, the completely amorphous and defect-free structure is free of grain boundaries, grains, pinholes, and dislocations, which structurally eliminates atmospheric erosion channels, particle attachment points, and impurity residue sites, resulting in a smooth, low-particle-content surface and ensuring the cleanliness of the cavity. In some embodiments of this application, dual-atmosphere fully compatible chemical stability is achieved: it can withstand both a high-temperature reducing atmosphere of NH3 / H2 at 900~1200℃ and a strong oxidizing atmosphere of O2 at 400~800℃, without hydrogen corrosion, nitriding, oxidation, or decomposition during repeated switching between the two extreme atmospheres, thus solving the fatal defect of traditional crystalline coatings being unable to be compatible with dual atmospheres. In some embodiments of this application, there is no impurity release at high temperatures: the gas emission rate at high temperatures is ≤1×10⁻⁶. - ¹² mbar·L / (s·cm²), with no release of metal or carbon impurities, and will not cause secondary pollution at the interface between the epitaxial film and the heterojunction; In some embodiments of this application, the interface bonding is stable: the bonding force with the underlying SiC layer is ≥50MPa, and the coefficient of thermal expansion is 3~6×10⁻⁶. -6 / ℃, with gradient matching between SiC layer and graphite matrix, it does not crack, peel, or pulverize during repeated temperature cycles of 400~1200℃.
[0051] In some embodiments of this application, the low surface energy fully amorphous multi-component metal oxynitride composite passivation layer described in this layer includes, but is not limited to, the following four material systems, all of which possess the above-mentioned common core characteristics: rare earth-aluminum based amorphous oxynitride system: amorphous Y-Al-ON, amorphous Sc-Al-ON, amorphous La-Al-ON, amorphous Gd-Al-ON, amorphous Yb-Al-ON (the optimal system is amorphous Y-Al-ON, with a surface energy as low as 22mJ / m²).
[0052] Among them, rare earth-silicon-aluminum-based amorphous oxynitride systems include: amorphous Y-Si-Al-ON, amorphous Sc-Si-Al-ON, and amorphous La-Si-Al-ON; high-melting-point transition metal-aluminum-based amorphous oxynitride systems include: amorphous Zr-Al-ON, amorphous Hf-Al-ON, amorphous Ta-Al-ON, and amorphous Nb-Al-ON; and alkaline earth metal-aluminum-based amorphous oxynitride systems include: amorphous Mg-Al-ON and amorphous Ca-Al-ON. The thickness of this layer is 1~5μm, and it is prepared using reactive magnetron sputtering, plasma spraying, or low-pressure chemical vapor deposition processes. The corresponding material system and preparation process can be selected according to actual mass production requirements.
[0053] In some embodiments of this application, the second layer is a high-density covalently bonded ceramic corrosion-resistant layer. This layer is a high-density covalently bonded corrosion-resistant ceramic material, with SiC as the core material. It is the main structural support layer and the main corrosion-resistant layer of the coating system, with a thickness of 80~150μm, a density of >99%, and a temperature resistance of ≥1600℃.
[0054] The common core characteristics of this type of material are: it is prepared by CVD or plasma spraying process, and has extremely strong resistance to high temperature, NH3 ammonia corrosion and O2 oxygen free radical bombardment. At the same time, it provides a buffer for the thermal expansion coefficient of the upper and lower layers, avoids thermal stress cracking of the coating, and protects the inner carbon diffusion barrier layer and graphite matrix. The interfacial bonding force with the upper passivation layer and the lower carbon diffusion barrier layer is ≥45MPa. It does not deform or crack at high temperature and has a stable structure in long-term operation.
[0055] In some embodiments of this application, the material of the third layer includes one of the following: a binary nitride system, a ternary or higher composite nitride system, a rare earth composite oxynitride system, and a transition metal composite oxynitride system; the binary nitride system includes one of the following: nanocrystalline α-Si3N4, nanocrystalline β-Si3N4, and nanocrystalline AlN.
[0056] In some embodiments of this application, this layer is a ternary or higher nitride / oxynitride ceramic material that contains no carbon elements in the crystal lattice. It is a core innovative layer that blocks carbon pollution in the graphite matrix from the root, and completely solves the essential defect that traditional SiC coatings cannot completely block carbon diffusion. It has a thickness of 2~10μm, a dense nanocrystalline structure, and a grain size of ≤100nm.
[0057] In some embodiments of this application, the common core features of this type of material are: The lattice is essentially carbon-free, completely eliminating carbon self-diffusion channels: The material lattice does not contain any carbon elements, and there is no natural intrinsic carbon self-diffusion behavior of SiC materials, thus blocking the intrinsic path of carbon diffusion from the root of the crystal structure. Superior carbon diffusion blocking capability across the entire temperature range: Within the full operating temperature range of MOCVD (1000~1600℃), the diffusion coefficient of carbon in this type of material is ≤1×10⁻⁶. - ² 0 cm² / s, which is more than 6 orders of magnitude lower than that of SiC materials, can completely block the outward diffusion of carbon from the graphite matrix and completely solve the fatal carbon pollution problem of Ga2O3 epitaxy. Excellent thermal compatibility: coefficient of thermal expansion is 2~5×10 -6 / ℃, highly compatible with graphite matrix and SiC layer, no thermal stress, no cracking, no peeling during high temperature heating and cooling cycles; Dual-atmosphere chemical stability: It can withstand both high-temperature reducing atmosphere and strong oxidizing atmosphere, is not corroded, does not react with the interface between the upper and lower layers, and has a stable structure during long-term operation.
[0058] In some embodiments of this application, the lattice-free carbon nitride / oxynitride-based carbon diffusion barrier layer described herein includes, but is not limited to, the following four major material systems, all of which possess the aforementioned common core characteristics: Binary nitride systems: nanocrystalline α-Si3N4, nanocrystalline β-Si3N4, nanocrystalline AlN (the optimal system is dense nanocrystalline Si3N4, which has the lowest carbon diffusion coefficient). Ternary and higher-order composite nitride systems: nanocrystalline AlN-Si3N4 solid solution, Zr-Si-N, Hf-Si-N, Ta-Si-N, Nb-Si-N, Ti-Si-N; Rare earth composite oxynitride systems: nanocrystalline Y-Si-Al-ON, Sc-Si-Al-ON, Y-Al-ON; Transition metal complex oxynitride systems: nanocrystalline Zr-Al-ON, Hf-Al-ON, Ta-Al-ON.
[0059] In some embodiments of this application, this layer is prepared using low-pressure chemical vapor deposition, reactive sintering, or atomic layer deposition processes to ensure that the coating is dense and defect-free, thereby achieving complete blockage of carbon diffusion.
[0060] In some embodiments of this application, the fourth layer is a high-purity isostatically pressed carbon matrix material, which is fixed with high-purity fine-particle isostatically pressed graphite. It serves as the structural support matrix for the cavity and all coated components, with a thermal conductivity ≥150W / (m·K) and ash content ≤5ppm. It can provide a uniform and stable thermal field distribution for the cavity, and at the same time form a perfect interface bond with the carbon diffusion barrier layer, ensuring the overall stability of the coating system. The surface of the graphite matrix is polished, with a roughness Ra≤0.2μm, providing good substrate conditions for the deposition of the upper carbon diffusion barrier layer.
[0061] Compared with the prior art, the present invention has the following outstanding substantive features and significant beneficial effects: Firstly, this invention pioneers a dual atmosphere isolation scheme combining "intrinsic magnetic field constraint and dynamic isolation with a linear air curtain." It clearly defines the gradient magnetic field and the linear Ar isolation air curtain as crucial components of the atmosphere isolation system, fundamentally addressing the core pain point of hydrogen-oxygen isolation. Based on the intrinsic magnetic susceptibility difference between H2 and O2, this invention constructs a strong gradient magnetic field through an external Halbach permanent magnet array to achieve intrinsic gas partitioning. Simultaneously, it utilizes a through-type linear Ar isolation air curtain at the top of the cavity to create a physical dynamic barrier. The synergistic effect and dual protection of these two elements achieve non-contact, permanent, and stable isolation of H2 and O2 atmospheres within a completely open cavity without internal obstructions, achieving a separation efficiency of ≥99.9%. This completely eliminates the risk of explosion and cross-contamination from hydrogen-oxygen contact. Unlike conventional solutions using physical gates or single air curtains, this scheme has no moving parts, zero continuous energy consumption, no wear, and no risk of seal failure. It exhibits strong resistance to flow fluctuations, and minor disturbances will not disrupt the partitioning. Its innovative nature addresses the reliability issues of existing isolation solutions.
[0062] Furthermore, this invention truly achieves in-situ heterogeneous integration within a single cavity, eliminating the need for cavity opening or replacement. Within a single integrated cavity, a dual-atmosphere isolation system enables dual-atmosphere partitioning. Combined with a movable substrate, continuous in-situ growth of GaN and Ga2O3 can be achieved without opening, replacing, or transferring the substrate. This completely solves the pain point of existing technologies being unable to achieve in-situ heterogeneous integration, ensuring the cleanliness and lattice matching of the heterogeneous interface, significantly improving the upper limit of device performance, while reducing process complexity and lowering production costs.
[0063] Furthermore, the dual-zone fully independent system doubles equipment utilization and significantly improves mass production efficiency. The left and right zones are equipped with fully physically isolated vacuum, spray, temperature control, and exhaust gas systems, which can operate completely independently and in parallel: while the GaN zone on the left is growing normally, the Ga2O3 zone on the right can stably maintain a high vacuum, and simultaneously perform substrate baking, pretreatment, and even simultaneous growth, increasing equipment utilization by 100% and directly doubling production capacity; the process changeover time is shortened from the traditional 1-2 hours to less than 2 minutes, eliminating the need for repeated high vacuum pumping throughout the cavity, significantly improving mass production efficiency, and adapting to the needs of large-scale industrial production.
[0064] Furthermore, the four-layer gradient composite coating 15 completely eradicates carbon contamination, is compatible with both extreme atmospheres, and eliminates the memory effect. This invention, through a lattice-free carbon nitride / oxynitride-based carbon diffusion barrier layer, blocks the outward diffusion of graphite carbon from the lattice source, completely solving the problem that existing SiC coatings cannot completely block carbon contamination. The top layer, a low surface energy amorphous multi-component metal oxynitride passivation layer, significantly reduces surface adsorption capacity, eliminates the memory effect and cross-contamination of organometallic precursors, and, in conjunction with the SiC corrosion-resistant layer and graphite substrate, forms a gradient-matched coating system compatible with both reducing and oxidizing extreme atmospheres, improving the quality of epitaxial films and the consistency of device performance.
[0065] Furthermore, it offers sufficient safety redundancy, making it fully adaptable to industrial mass production. This invention employs four layers of safety protection: intrinsic magnetic field confinement, dynamic isolation with a linear gas curtain, dual independent vacuum hard isolation, and three-level hard interlock control, completely eliminating the possibility of hydrogen-oxygen contact and significantly improving operational safety. Its fully modular design eliminates vulnerable parts, reduces maintenance costs, and allows for continuous and stable operation 24 hours a day. It is compatible with 2-8 inch large-size substrate growth, offering strong versatility and fully meeting the needs of industrial mass production.
[0066] Furthermore, it has no internal obstructions, resulting in a simple structure and high reliability. The cavity contains no built-in physical obstructions, gates, or other structures, has no moving parts or dynamic seals, and has an extremely low risk of vacuum leakage, leading to a low failure rate during long-term operation. Simultaneously, it does not affect the translation of the base or the placement and removal of the substrate, making operation convenient, maintenance simple, and reducing equipment operating costs.
[0067] use Figure 1 The reaction chamber structure is used for in-situ growth of Ga2O3 / GaN heterojunctions, which is completed entirely within the same chamber without the need for opening or changing chambers. The specific process is as follows, which verifies the feasibility and superiority of the invention and demonstrates the synergistic effect of each system and coating: First, the preparation stage: the 2-inch c-plane sapphire substrate is ultrasonically cleaned sequentially with acetone, ethanol, and deionized water for 15 minutes each time (5 minutes each time), dried with high-purity N2, and then placed in a graphite tray 19 and fixed on the translation base; the quick-release door of the cavity is closed, and the flange is tightened evenly; the independent vacuum units of the left and right zones are started separately, and the background vacuum is evacuated to ≤5×10 -6mbar; Start the atmosphere isolation system, turn on the Halbach magnetic field system and water cooling jacket, and confirm that the magnetic field gradient is 162T / m and the magnet temperature is ≤60℃; Start the linear Ar isolation gas curtain, introduce high-purity Ar, adjust the gas curtain outlet pressure to 0.12mbar, start the vacuum pump in the middle evacuation tank, and confirm that the gas curtain is stable; Introduce high-purity Ar (flow rate 30sccm) into the left and right zones respectively, and adjust the flow rate to ensure that the Reynolds number Re=650 in the cavity, maintain a stable laminar flow state, and the cleanliness of the atmosphere inside the cavity meets the standard (particle number ≤10 / cm³); At this time, the coating system has completed preheating, there is no impurity adsorption on the surface, and the low surface energy characteristics begin to play a role.
[0068] Secondly, the GaN epitaxial layer growth stage: the translational substrate is moved along the track to the left GaN-specific region and coaxially aligned with the GaN spray head, with an alignment accuracy of ≤±0.3mm; the two heating elements of the substrate are activated at 20°C, heated to 1100°C, and held at that temperature for 10 minutes, with a substrate surface temperature uniformity of ≤±1.2°C; the spray head height is adjusted to 35mm, and TMGa (55sccm), NH3 (220sccm), and H2 (320sccm) are introduced, while the TMAl doping branch is activated (8sccm), controlling the Al composition to 11%; the substrate rotation is activated at 22rpm, the cavity pressure is stabilized at 0.09mbar, and the growth time is 65 minutes, completing the growth of a 2.8μm thick AlGaN epitaxial layer.
[0069] During this process, the atmosphere isolation system operated stably: the gradient magnetic field completely confined the diamagnetic H2 / NH3 to the left region, preventing lateral diffusion; the linear Ar gas curtain formed a stable barrier, and the central evacuation trough continuously pumped gas, completely blocking trace amounts of gas from crossing the region; the independent vacuum unit in the Ga2O3 region on the right operated at full load throughout the entire process, stably maintaining ≤3×10 -6 The high vacuum of mbar allows for simultaneous substrate baking and degassing at 600℃, completely unaffected by the operation on the left side, maximizing equipment utilization. The low surface energy characteristics of the coating on the inner wall of the cavity effectively prevent the adsorption of TMGa precursors and eliminate the memory effect. At the same time, the SiC corrosion-resistant layer and the carbon diffusion barrier layer work synergistically to prevent carbon pollution and coating damage.
[0070] Following this, in-situ cross-region switching stage: After GaN growth is completed, all process gas valves on the left side are closed, and high-purity Ar (flow rate 50 sccm) is introduced for 3 purging cycles, 5 minutes each time, followed by vacuuming to ≤9×10⁻⁶. -5mbar; After confirming that all three-level interlocking conditions are met (both process gas valves in both zones are fully closed, purging is completed, vacuum level meets standards, and the atmosphere isolation system is normal), the translation base maintains a rotation of 22 rpm, smoothly passes through the straight gas curtain area along the track, and moves to the right-side Ga2O3 exclusive zone, coaxially aligned with the Ga2O3 spray head. The entire process takes ≤2 minutes. The atmosphere isolation system operates continuously throughout the process, with the magnetic field and gas curtain working together to ensure stable atmosphere partitioning, no hydrogen-oxygen cross-contact, no substrate contamination, and no sudden temperature changes. The dual-atmosphere compatibility of the coating ensures no coating damage or impurity release during the switching process, and the low surface energy characteristics prevent cross-contamination of residual precursors.
[0071] Next, during the Ga2O3 epitaxial layer growth stage: the substrate was cooled to 620℃ and kept at a constant temperature for 10 min, with the substrate surface temperature uniformity ≤ ±1.3℃; the spray head height was adjusted to 50 mm, and TEGa (42 sccm), O2 (155 sccm), and Ar (60 sccm) were introduced, while the Cp2Mg doping branch was activated (5 sccm), and the Mg composition was controlled at 3%; the substrate rotation speed was kept constant at 22 rpm, the cavity pressure was stabilized at 0.09 mbar, and the growth time was 45 min, completing the growth of a 1.5 μm thick Ga2O3 epitaxial layer, ultimately forming an AlGaN / Ga2O3 heterojunction structure.
[0072] During this process, the gradient magnetic field firmly confines the paramagnetic O2 to the Ga2O3 growth region on the right, the linear Ar gas curtain continuously forms an isolation barrier, and the middle gas extraction groove promptly removes any trace amounts of gas that may leak, ensuring that O2 does not diffuse across regions. The GaN region on the left maintains a high vacuum state to avoid contamination of the atmosphere on the right. The four-layer gradient composite coating 15 on the inner wall of the cavity plays a key role. The low surface energy amorphous passivation layer effectively avoids the adsorption of TEGa and Cp2Mg precursors and has no process memory effect. The carbon diffusion barrier layer completely blocks the carbon diffusion of the graphite matrix, and the SiC corrosion-resistant layer is resistant to O2 oxygen free radical bombardment. The coating as a whole is free from cracks and damage, ensuring the purity and quality of the Ga2O3 epitaxial layer.
[0073] Finally, in the growth completion stage: after the Ga2O3 growth is complete, close all process gas valves on the right side, and purge with high-purity Ar (flow rate 50 sccm) three times for 5 minutes each time, and then evacuate to a vacuum level ≤8×10⁻⁶. -5 mbar; shut down the atmosphere isolation system, dual-zone vacuum unit and temperature control system, wait for the substrate to cool down to below 100°C, open the quick-release door of the cavity, remove the substrate, and complete the entire in-situ growth process of the GaN / Ga2O3 heterojunction.
[0074] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," and "counterclockwise," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.
[0075] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly specified.
[0076] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.
[0077] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.
[0078] The above description, in conjunction with specific preferred embodiments, provides a further detailed explanation of the present invention. It should not be construed that the specific implementation of the present invention is limited to these descriptions. For those skilled in the art, various simple deductions or substitutions can be made without departing from the concept of the present invention, and all such modifications and substitutions should be considered within the scope of protection of the present invention.
Claims
1. A MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN, characterized in that, The system includes a reaction chamber, which is equipped with an atmosphere isolation system and a sample translation base. The atmosphere isolation system includes a gradient magnetic field confinement module and an Ar isolation gas curtain module. The Ar isolation gas curtain module is located in the middle of the reaction chamber and is used to form an isolation gas curtain in the reaction chamber to divide the reaction chamber into a left chamber and a right chamber. The gradient magnetic field constraint module is located on the side of the right chamber away from the Ar isolation gas curtain module, and is used to generate a magnetic attraction effect on the gas in the right chamber; The left chamber is equipped with a GaN spray head, which is connected to a TMGa gas path, an NH3 gas path, an H2 gas path, and a TMAl doping gas path. The right chamber is equipped with a Ga2O3 spray head, which is connected to a TEGa gas path, an Ar gas path, a doping gas path, and an O2 / O3 gas path. The sample translation base is used to support the sample and move the sample between the left chamber and the right chamber.
2. The MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN according to claim 1, characterized in that, The inner wall of the reaction chamber is provided with four layers of gradient composite coating, which includes a first layer, a second layer, a third layer and a fourth layer stacked sequentially from the outside to the inside. The first layer is a low surface energy, fully amorphous, multi-component metal oxynitride composite passivation layer; the second layer is a high-density SiC covalent ceramic corrosion-resistant layer; the third layer is a lattice-free carbon nitride / oxynitride-based carbon diffusion barrier layer; and the fourth layer is a high-purity isostatic pressing carbon matrix layer.
3. The MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN according to claim 2, characterized in that, The material of the first layer includes one of the following: rare earth-aluminum-based amorphous oxynitride system, rare earth-silicon-aluminum-based amorphous oxynitride system, high melting point transition metal-aluminum-based amorphous oxynitride system, and alkaline earth metal-aluminum-based amorphous oxynitride system; The rare earth-aluminum based amorphous oxynitride system includes one of the following: amorphous Y-Al-ON, amorphous Sc-Al-ON, amorphous La-Al-ON, amorphous Gd-Al-ON, and amorphous Yb-Al-ON.
4. The MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN according to claim 1, characterized in that, The material of the third layer includes one of the following: a binary nitride system, a ternary or higher composite nitride system, a rare earth composite oxynitride system, and a transition metal composite oxynitride system; The binary nitride system includes one of the following: nanocrystalline α-Si3N4, nanocrystalline β-Si3N4, and nanocrystalline AlN.
5. The MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN according to claim 1, characterized in that, The gradient magnetic field constraint module includes multiple permanent magnets arranged in an array, wherein the surface remanence of a single permanent magnet is greater than or equal to 1.45T, the surface magnetic field of the gradient magnetic field constraint module is greater than or equal to 1.4T, and the magnetic field gradient of the effective working area of the right chamber is greater than or equal to 150T / m. The external parts of the multiple permanent magnets are sequentially fitted with non-magnetic stainless steel protective covers and water-cooled heat dissipation sleeves.
6. The MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN according to claim 5, characterized in that, The Ar isolation air curtain module includes multiple linear nozzle assemblies. The nozzle gap width of the linear nozzle assembly is 0.3mm-0.5mm, and the outlet pressure of the linear nozzle assembly is 0.02mbar-0.05mbar higher than the cavity pressure in the left and right chambers.
7. The MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN according to claim 6, characterized in that, Both the left and right chambers are equipped with air extraction ports on the side away from the Ar isolation air curtain module, and the air extraction ports are connected to external air pumps.
8. The MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN according to claim 1, characterized in that, The left chamber is equipped with an NH3 preheating unit, the temperature control range of which is 900-1200℃.
9. The MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN according to claim 8, characterized in that, The right chamber is equipped with an O2 concentration stabilization unit, the temperature control range of which is 400-1000℃.
10. The MOCVD reaction chamber compatible with in-situ heterogeneous integration of Ga2O3 and GaN according to claim 1, characterized in that, The sample translation base includes a linear drive assembly and a base body. The linear drive assembly is arranged along the length direction of the reaction chamber. The base body is mounted on the linear drive assembly. The base body is provided with a thermocouple and two Cr-Mo-Si alloy heating tapes. The thermocouple is located between the two Cr-Mo-Si alloy heating tapes. The outer side of the base body is also provided with a heat insulation layer. The heat insulation layer is provided with a spiral cooling pipe. The base body is also equipped with a magnetic fluid sealing rotation mechanism.