CN113089089B - Silicon carbide crystal preparation device and growth method thereof - Google Patents

Silicon carbide crystal preparation device and growth method thereof Download PDF

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CN113089089B
CN113089089B CN202110363903.6A CN202110363903A CN113089089B CN 113089089 B CN113089089 B CN 113089089B CN 202110363903 A CN202110363903 A CN 202110363903A CN 113089089 B CN113089089 B CN 113089089B
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chamber
cavity
substrate
growth
crystal
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CN113089089A (en
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王宇
杨田
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Meishan Tianle Semiconductor Material Co ltd
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Meishan Boya New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/36Carbides
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02Epitaxial-layer growth
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02Epitaxial-layer growth
    • C30B25/18Epitaxial-layer growth characterised by the substrate
    • C30B25/186Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08Etching
    • C30B33/10Etching in solutions or melts

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The embodiment of the specification discloses a silicon carbide crystal preparation device and a growth method thereof, wherein the method is carried out in a multi-cavity growth device, and the multi-cavity growth device comprises a plurality of cavities; the method comprises the following steps: sequentially transferring and processing at least one substrate between a plurality of chambers; growing a silicon carbide crystal by vapor deposition in one of the plurality of cavities to obtain at least one combined crystal comprising the substrate and the silicon carbide crystal; etching the combined crystal by using an etching solution in a first temperature range to obtain a basal plane dislocation density of 120-2000cm‑2The silicon carbide crystal of (1). The silicon carbide crystals are prepared by adopting the multi-cavity growing device, and at least one substrate or combined crystal is conveyed among the cavities simultaneously or sequentially, so that the silicon carbide crystals are produced in batch in a production line manner, and the production efficiency is improved.

Description

Silicon carbide crystal preparation device and growth method thereof
Technical Field
The specification relates to the technical field of crystal preparation, in particular to a silicon carbide crystal preparation device and a growth method thereof.
Background
The silicon carbide crystal is used as a semiconductor material, and the single crystal of the silicon carbide crystal has the performances of wide forbidden band, high chemical stability, large thermal conductivity, strong radiation resistance, high breakdown electric field, high electron saturation drift velocity and the like. Therefore, the silicon carbide crystal material can be widely applied to various fields. However, the silicon carbide crystal is one of the hardest known materials, and the hardness and Young modulus of the silicon carbide crystal reach 380-700 Gpa. This poses a challenge to the cutting and polishing of the ingot into wafers.
Therefore, it is necessary to provide a silicon carbide crystal preparation apparatus and a growing method thereof, which can reduce the process of cutting silicon carbide crystal and improve the efficiency of silicon carbide crystal production.
Disclosure of Invention
One aspect of the embodiments of the present description provides a method of preparing a silicon carbide crystal, the method performed in a multi-chamber growth apparatus comprising a plurality of chambers; the method comprises the following steps: sequentially transferring and processing at least one substrate between a plurality of chambers; in thatGrowing a silicon carbide crystal in one of the plurality of cavities by vapor deposition to obtain at least one combined crystal comprising the substrate and the silicon carbide crystal; etching the combined crystal by using an etching solution in a first temperature range to obtain a basal plane dislocation density of 120-2000cm-2The silicon carbide crystal of (1).
In some embodiments, prior to sequentially transferring and processing the at least one substrate between the plurality of chambers, the method further comprises: and carrying out polishing treatment on the at least one substrate.
In some embodiments, prior to sequentially transferring and processing the at least one substrate between the plurality of chambers, the method further comprises: and carrying out cleaning treatment on the at least one substrate.
In some embodiments, the etching the composite crystal with an etching solution comprises: the etching solution is used for carrying out ultrasonic cleaning on the combined crystal for a first time to obtain the basal plane dislocation density of 120-2000cm-2The silicon carbide crystal of (1).
In some embodiments, the multi-chamber growth device comprises at least: the device comprises an in-situ etching cavity, a carbonization cavity, a growth cavity, a buffer cavity and a transmission assembly; and the transmission assembly sequentially processes at least one substrate through the in-situ etching cavity, the carbonization cavity, the growth cavity and the buffer cavity.
In some embodiments, the method further comprises: before the at least one substrate is sequentially transferred and processed among the plurality of cavities, at least one substrate of another batch is started to be transferred and processed among the plurality of cavities, and at least one substrate of the two batches is simultaneously and respectively transferred and processed in different cavities.
In some embodiments, the multi-chamber growth device comprises a vacuum chamber; the method comprises the following steps: placing the at least one substrate in the vacuum chamber prior to processing the at least one substrate in the in-situ etch chamber; adjusting the pressure of the vacuum cavity and the in-situ etching cavity to a first pressure interval; the drive assembly conveys the at least one substrate to the in-situ etch chamber.
In some embodiments, the processing of the at least one substrate in the in-situ etch chamber comprises: keeping the pressure of the in-situ etching cavity in a second pressure interval and the temperature in a second temperature interval within a second time length range; and introducing hydrogen to the in-situ etching cavity to normal pressure, and keeping the temperature of the in-situ etching cavity within a third time range at a third temperature interval for in-situ etching treatment.
In some embodiments, the processing of the at least one substrate in the carbonization chamber comprises: and keeping the pressure of the carbonization cavity in a third pressure interval within a fourth time period, and carrying out carbonization treatment at the fourth temperature interval.
In some embodiments, the carbonizing process comprises: adjusting the temperature of the carbonization cavity to the third temperature interval; and conveying the at least one substrate into the carbonization cavity through the transmission assembly, adjusting the temperature of the carbonization cavity to a fifth temperature interval and the pressure to a fourth pressure interval, simultaneously introducing propane and hydrogen to the third pressure interval, keeping the pressure of the carbonization cavity as the third pressure interval within a fourth time period, and carrying out carbonization treatment at the temperature within the fourth temperature interval.
In some embodiments, the processing of the at least one substrate in the growth chamber comprises: keeping the temperature of the growth cavity in a sixth temperature interval and the pressure in a fourth pressure interval, introducing reaction raw materials, and adjusting the pressure in a fifth pressure interval to perform a crystal growth process.
In some embodiments, the crystal growth process comprises: adjusting the temperature of the growth cavity to the fourth temperature interval and the pressure to the third pressure interval; conveying the at least one substrate into the growth cavity through the transmission assembly, adjusting the temperature of the growth cavity to a sixth temperature interval, introducing silane, propane and hydrogen to a fifth pressure interval at the pressure of the fourth pressure interval, and performing crystal growth; and stopping the crystal growth when the thickness of the silicon carbide crystal reaches the target thickness.
In some embodiments, the multi-chamber growth device comprises a positioner; said transferring said at least one substrate to said growth chamber by said drive assembly comprises: stopping the drive assembly when the positioner determines that the at least one substrate is in a preset position in the growth chamber.
In some embodiments, said processing in said buffer chamber comprises: and cooling within a seventh temperature interval of keeping the temperature of the buffer cavity within the fifth time.
In some embodiments, the cool-down process comprises: adjusting the temperature of the buffer cavity to the sixth temperature interval; conveying the combined crystal into the buffer cavity through the transmission assembly; and adjusting the temperature of the buffer cavity to a seventh temperature interval, and keeping the temperature of the buffer cavity in a fifth time interval as the seventh temperature interval to carry out cooling treatment.
In some embodiments, the multi-lumen growth device comprises a tip lumen; the method further comprises the following steps: maintaining the temperature of the end cavity at room temperature; transferring the composite crystal into the end cavity through the transmission assembly; the combined crystals were cooled to room temperature.
An aspect of embodiments of the present specification provides a multi-chamber growth apparatus for use in a crystal preparation process, the multi-chamber growth apparatus comprising: etching the cavity in situ; carbonizing the cavity; a growth chamber for growing a silicon carbide crystal by vapor deposition, resulting in at least one composite crystal comprising a substrate and a silicon carbide crystal; a buffer cavity; a transmission assembly; the transmission assembly sequentially processes the at least one substrate through the in-situ etching cavity, the carbonization cavity, the growth cavity and the buffer cavity.
In some embodiments, the multi-chamber growth device further comprises a vacuum chamber.
In some embodiments, the multi-lumen growth device further comprises a tip lumen.
In some embodiments, the drive assembly comprises at least two rotatable cylindrical rollers arranged in parallel, the rotatable cylindrical rollers being located side-by-side below each chamber.
In some embodiments, the multi-chamber growth device comprises a tray; the tray is provided with at least one groove, and the at least one groove is used for placing at least one substrate.
In some embodiments, the growth cavity comprises a rotating shaft.
In some embodiments, the multi-chamber growth device comprises a positioner.
In some embodiments, at least one gas inlet conduit is included in each of the in-situ etch chamber, the carbonization chamber, and the growth chamber.
In some embodiments, at least one pumping line is included in each of the vacuum chamber, the in-situ etching chamber, the carbonization chamber, and the growth chamber.
In some embodiments, heating bodies are respectively disposed in the in-situ etching chamber, the carbonization chamber, the growth chamber, and the buffer chamber.
Drawings
FIG. 1 is a schematic diagram of exemplary hardware and/or software of a crystal production system according to some embodiments;
FIG. 2A is an exemplary schematic structural diagram of a multi-chamber growth apparatus according to some embodiments;
FIG. 2B is a top view of an exemplary distribution of cavities in a multi-cavity growth apparatus according to some embodiments;
FIG. 3A is a schematic diagram of an exemplary configuration of a multi-chamber growth apparatus according to further embodiments;
FIG. 3B is a top view of an exemplary distribution of cavities in a multi-cavity growth apparatus according to further embodiments;
FIG. 4 is an exemplary schematic structural view of a first type of cavity according to some embodiments;
FIG. 5 is an exemplary schematic structural diagram of a second type of cavity according to some embodiments;
FIG. 6 is an exemplary schematic structural diagram of a third type of cavity according to some embodiments;
FIG. 7 is an exemplary structural schematic of a tray according to some embodiments;
FIG. 8 is an exemplary schematic structural diagram of a transmission assembly according to some embodiments;
FIG. 9 is a schematic flow chart of an exemplary method for preparing a silicon carbide crystal according to some embodiments;
FIG. 10 is an exemplary flow diagram of a substrate surface treatment process according to some embodiments;
FIG. 11 is an exemplary flow diagram for transferring and processing a substrate between chambers according to some embodiments;
FIG. 12 is an exemplary flow diagram of a vacuum process according to some embodiments;
FIG. 13 is an exemplary flow diagram of an in-situ etch process according to some embodiments;
FIG. 14 is an exemplary flow diagram of a carbonization process according to some embodiments;
FIG. 15 is a schematic view of an exemplary flow of transferring a substrate from a carbonization chamber to a growth chamber according to some embodiments;
FIG. 16 is an exemplary flow diagram of crystal growth according to some embodiments;
FIG. 17 is an exemplary flow diagram of a buffering and cooling process according to some embodiments.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present disclosure, the drawings used in the description of the embodiments will be briefly described below. It is obvious that the drawings in the following description are only examples or embodiments of the present description, and that for a person skilled in the art, the present description can also be applied to other similar scenarios on the basis of these drawings without inventive effort. Unless otherwise apparent from the context, or otherwise indicated, like reference numbers in the figures refer to the same structure or operation.
It should be understood that "system", "device", "unit" and/or "module" as used herein is a method for distinguishing different components, elements, parts or assemblies at different levels. However, other words may be substituted by other expressions if they accomplish the same purpose.
As used in this specification and the appended claims, the terms "a," "an," "the," and/or "the" are not intended to be inclusive in the singular, but rather are intended to be inclusive in the plural, unless the context clearly dictates otherwise. In general, the terms "comprises" and "comprising" merely indicate that steps and elements are included which are explicitly identified, that the steps and elements do not form an exclusive list, and that a method or apparatus may include other steps or elements.
Flow charts are used in this description to illustrate operations performed by a system according to embodiments of the present description. It should be understood that the preceding or following operations are not necessarily performed in the exact order in which they are performed. Rather, the various steps may be processed in reverse order or simultaneously. Meanwhile, other operations may be added to the processes, or a certain step or several steps of operations may be removed from the processes.
FIG. 1 is a schematic diagram of exemplary hardware and/or software of a crystal preparation system according to some embodiments.
As shown in FIG. 1, crystal production system 100 may include a control module 101, a detection module 102, a heating module 103, a polishing module 104, a cleaning module 105, a vacuum module 106, an etching module 107, a carbonization module 108, a growth module 109, a drive module 110, a mechanical structure 111, a communication module 112, a power supply module 113, and an input/output module 114. The modules, units, and sub-units mentioned in the present specification may be implemented by hardware, software, or a combination of software and hardware. The hardware implementation may include a circuit or a structure formed by solid components; the implementation of software may include storing operations corresponding to the modules, units, and sub-units in a memory in the form of codes, which are executed by appropriate hardware, e.g., a microprocessor. When a module, a unit or a sub-unit mentioned in this specification performs its operation, if not specifically stated, it may mean that software code including the function is executed or that hardware having the function is used. Meanwhile, when the modules, units and sub-units mentioned in the present specification correspond to hardware, the structures of the corresponding hardware are not limited, and the hardware capable of implementing the functions of the modules, units and sub-units are within the protection scope of the present specification. For example, different modules, units and sub-units mentioned in the specification may correspond to the same hardware structure. For example, a module, a unit, or a sub-unit referred to in this specification may correspond to a plurality of independent hardware configurations.
The control module 101 may be associated with other modules. In some embodiments, the control module 101 may control the operational state of other modules (e.g., the detection module 102, the heating module 103, the drive module 110, the communication module 112, the power module 113, etc.). In some embodiments, the control module 101 may control the drive module 110 to start or stop. In some embodiments, the control module 101 may control the power supply, the power supply time period, and the like of the power supply module 113. In some embodiments, the control module 101 may manage the data acquisition or transmission process in the communication module 112.
The detection module 102 is used to detect process parameters of the system, such as temperature, pressure, gas flow rate, crystal growth thickness, and the like. In some embodiments, the detection module 102 may send the detection result of the system process parameter to the control module 101, and the control module 101 may perform a subsequent operation or instruction according to the detection result. In some embodiments, the detection module 102 may monitor the temperature in the growth chamber and send the temperature data to the control module 101, and the control module 101 determines whether to adjust the operating parameters (e.g., heating current, heating power, etc.) of the heating module 103 to control the temperature in the growth chamber according to the temperature data fed back by the detection module 102 in real time. In some embodiments, the detection module 102 may monitor the pressure in the vacuum cavity and send the pressure data to the control module 101, and the control module 101 determines whether to continue to vacuumize the vacuum cavity according to the pressure data fed back by the detection module 102 in real time, and if so, the control module 101 may control the vacuum module 106 to vacuumize the vacuum cavity; conversely, the control module 101 may control the vacuum module 106 to stop pumping vacuum to maintain the current vacuum level. In some embodiments, the detection module 102 may monitor the flow rates of the various types of gas raw materials and send the flow rate data to the control module 101, and the control module 101 determines whether to adjust the flow rates of the various types of gas raw materials according to the flow rates of the gas raw materials fed back by the detection module 102 in real time to control the component ratios of the gas raw materials or the crystal growth thickness.
The heating module 103 is used to provide the thermal energy required by the system. In some embodiments, the heating module 103 may heat the growth chamber or the in-situ etch chamber. In some embodiments, the heating module 103 may include a resistive heater, an induction coil, or like heating component. The resistive heater may include a graphite resistor or a carbon silicon rod resistor. In some embodiments, the heating module 103 may be used in combination with or mounted in or outside of one or more other modules or chambers for providing the thermal energy required by the other modules or chambers. In some embodiments, subsystems of the heating module 103 are installed in the growth chamber and the in-situ etch chamber, respectively, to control the temperature in the growth chamber and the in-situ etch chamber, respectively.
In some embodiments, the polishing module 104 controls the polishing process of the substrate. In some embodiments, prior to preparing a crystal using a substrate, the surface of the substrate needs to be pretreated to keep the surface of the substrate (particularly the crystal growth surface) clean and flat. In some embodiments, the pre-treatment may include a polishing process and a cleaning process. In some embodiments, the polishing process is performed in a polishing apparatus. The polishing apparatus may comprise a polisher. In some embodiments, the substrate is placed on a polishing apparatus by a mechanical structure 111 (e.g., a robot) and the substrate is polished. In some embodiments, the polishing module can control the polishing apparatus to polish the back side of the substrate (opposite the crystal growth side) to make the surface thereof flat; the front side of the substrate (crystal growth side) is then finely polished to remove surface-cutting scratches and defects.
In some embodiments, the cleaning module 105 controls the cleaning process of the substrate. In some embodiments, the cleaning process may be performed in a cleaning apparatus. In some embodiments, the cleaning apparatus may comprise an ultrasonic cleaner. The substrate may be placed in a cleaning apparatus by a robot 111 (e.g., a robot), and cleaned at least twice by at least one of a cleaning solution and ultrasonic waves, and after cleaning, the substrate may be removed from the cleaning solution and blown dry with a gas using the robot 111. In some embodiments, the cleaning fluid may include acetone, alcohol, or deionized water. In some embodiments, the substrate may be sequentially cleaned with acetone, alcohol, and deionized water. In some embodiments, the gas used to blow dry the substrate surface is an inert gas. In some embodiments, the gas used to blow dry the substrate surface is nitrogen with a purity of over 99%.
In some embodiments, the cleaning module 105 may control the chemical etching process and the cleaning process of the composite crystal. In some embodiments, the chemical etching process and the cleaning process may be performed in a cleaning apparatus. In some embodiments, the composite crystal can be placed in a cleaning apparatus by a mechanical structure 111 (e.g., a robot), and the substrate on the composite crystal can be dissolved and removed under the action of a certain temperature, an alkali solution and ultrasonic waves to obtain a target crystal (e.g., a silicon carbide crystal). In some embodiments, the base solution may comprise a NaOH solution or a KOH solution. The silicon carbide crystal from which the substrate is removed can be placed in a cleaning apparatus by a mechanical structure 111 (e.g., a robot) and cleaned by a cleaning solution (e.g., isopropyl alcohol or deionized water) and ultrasonic waves to obtain a silicon carbide crystal without a substrate. The quality of a silicon carbide crystal can be characterized by the basal plane dislocation density (number of defects per unit area). In some embodiments, the basal plane dislocation density of the silicon carbide crystal is 100-2200 cm-2. In some embodiments, the basal plane dislocation density of the silicon carbide crystal is 120-2000cm-2. In some embodiments, the basal plane dislocation density of the silicon carbide crystal is 200-1800 cm-2. In some embodiments, the basal plane dislocation density of the silicon carbide crystal is 500-1500 cm-2. In some embodiments, carbonThe basal plane dislocation density of the silicon carbide crystal is 700-1300 cm-2. In some embodiments, the basal plane dislocation density of the silicon carbide crystal is 900-1100 cm-2
In some embodiments, the vacuum module 106 controls the evacuation process of the system. In the vacuumizing process, each cavity (such as an in-situ etching cavity, a carbonization cavity and a growth cavity) is respectively vacuumized to a certain gas pressure by controlling vacuumizing equipment. In some embodiments, the evacuation device may comprise a vacuum pump. In some embodiments, the detection module 102 may detect the pressure in each cavity separately and send the pressure data to the control module 101, and the control module 101 performs subsequent operations or instructions according to the pressure data. In some embodiments, the detection module 102 sends the pressure data in the in-situ etching chamber or the vacuum chamber to the control module 101, and the control module 101 determines that the in-situ etching chamber or the vacuum chamber needs to be continuously vacuumized according to the pressure data, and then controls the vacuum-pumping device to continuously vacuumize the in-situ etching chamber or the vacuum chamber. In some embodiments, the evacuation device may include at least one vacuum pump, and the at least one vacuum pump may be respectively connected to the cavities requiring pressure control, so as to independently evacuate each cavity.
In some embodiments, the etch module 107 controls the in situ etch process of the substrate. In some embodiments, the in-situ etch process is performed in an in-situ etch chamber. The in-situ etching chamber comprises one or more channels, one or more gas inlets and outlets, a heating assembly and a transmission assembly. In some embodiments, the substrate is transferred from the mechanical structure 111 to an in-situ etching chamber, and an in-situ etching process is performed on the surface of the substrate under the action of a certain temperature, a certain pressure and a certain gas. In some embodiments, the vacuum module 106 may evacuate the in-situ etching chamber to a certain gas pressure, slowly raise the temperature to a certain temperature for a certain time, introduce a gas (e.g., hydrogen) to the normal pressure, and raise the temperature to a certain temperature for a certain time to perform the in-situ etching process.
During the in-situ etching process, the detection module 102 may monitor the temperature and pressure inside the in-situ etching chamber in real time and transmit the temperature and pressure data to the control module 101. In some embodiments, the control module 101 may control the heating module 103 to adjust the operating parameters of the heating assembly according to the temperature transmitted by the detection module 102, thereby adjusting the temperature of the in-situ etch chamber. The control module 101 may control the vacuum module 106 to adjust the operation parameters of the vacuum pumping device or control the mechanical structure 111 to adjust the flow rate of the gas according to the pressure data transmitted by the detection module 102, so as to adjust the pressure in the in-situ etching chamber. After the in-situ etch process is complete, the substrate may be transferred out of the in-situ etch chamber. In some embodiments, the control module 101 can control the drive module 110 to open one or more channels on the in-situ etch chamber to transfer the substrate out of the in-situ etch chamber via the mechanical structure 111 (e.g., a transmission assembly).
In some embodiments, the carbonization module 108 controls the carbonization process of the substrate. In some embodiments, the carbonization process is performed in a carbonization chamber. The carbonization cavity comprises one or more channels, one or more gas inlets and outlets, a heating assembly and a transmission assembly. In some embodiments, the substrate is transported from the mechanical structure 111 to a carbonization chamber, and the substrate is carbonized at a certain temperature, a certain pressure and a certain gas. In some embodiments, the temperature of the carbonization chamber may be raised to a certain temperature in advance, the substrate is transferred to the carbonization chamber by the transfer assembly, the carbonization chamber is cooled to another temperature, the carbonization chamber is evacuated to a certain gas pressure and then heated, gas (for example, propane or hydrogen) is introduced to the carbonization chamber to a certain gas pressure, and the carbonization treatment is performed after the temperature is raised to a certain temperature and the substrate is kept for a certain period of time.
During the carbonization process, the detection module 102 may monitor the temperature and pressure data in the carbonization chamber in real time and transmit the temperature and pressure data to the control module 101. In some embodiments, the control module 101 may control the heating module 103 to adjust the operating parameters of the heating assembly based on the temperature transmitted by the detection module 102, thereby adjusting the temperature of the carbonization chamber. The control module 101 may control the vacuum module 106 to adjust the operation parameters of the vacuum equipment or control the mechanical structure 111 to adjust the flow rate of the gas according to the pressure data transmitted by the detection module 102, so as to adjust the pressure in the carbonization chamber. After the carbonization process is completed, the substrate may be transferred to the outside of the carbonization chamber. In some embodiments, the control module 101 may control the drive module 110 to open one or more channels on the carbonization chamber to transfer the substrate out of the growth chamber through the mechanical structure 111 (e.g., a transmission assembly).
In some embodiments, the growth module 109 controls the crystal growth process. The crystal growth method may include a vapor deposition method, a liquid deposition method, a czochralski method, a hydrothermal method, a flame fusion method, and the like. In particular, vapor deposition introduces vapor or other gases necessary for the reaction, containing gaseous, liquid reactants that form the film elements, into a reaction environment, chemically reacts at the substrate surface, and deposits solid products onto the substrate surface to form a film. The vapor deposition method may include a physical vapor deposition method, a chemical vapor deposition method. In some embodiments, the chemical vapor deposition process can be a metal organic chemical vapor deposition process (MOCVD), a plasma chemical vapor deposition Process (PCVD), a laser chemical vapor deposition process (LCVD), a low pressure chemical vapor deposition process (LPCVD), an ultra-vacuum chemical vapor deposition process (UHVCVD), an ultrasonic chemical vapor deposition process (UWCVD), and the like.
In some embodiments, the crystal growth is completed in a growth chamber. The growth cavity can be a kettle-type growth cavity, a tubular growth cavity, a tower-type growth cavity, a fluidized bed or a fixed bed.
In some embodiments, the growth chamber may include one or more channels, one or more gas inlets and outlets, a heating assembly, and a rotation assembly.
In some embodiments, the substrate is transferred from the mechanical structure 111 into the growth chamber, and the crystal growth process is performed at a temperature and a pressure on the surface of the substrate. Specifically, the growth chamber may be raised to a predetermined temperature that varies with the crystal being grown, either constant throughout the growth process or adjusted during the growth process in conjunction with variations in the crystal growth method. The temperature can be monitored by the detection module 102 and controlled by the control module 101 to control the heating module 103 for precise control. And certain types of gases are introduced. During the growth process, the growth cavity can maintain a certain set pressure, the pressure is different according to the grown crystal, the pressure can be kept constant in the whole growth process, and the pressure can be adjusted in the growth process according to different pressure growth methods. The pressure can be monitored by the detection module 102 and controlled precisely by the control module 101 controlling the driving module 110. Under the condition of controlling temperature and pressure, in the growth cavity, the surface of the substrate is subjected to vapor deposition to grow crystals. The detection module 102 can monitor the thickness of the crystal growth, and the control module 101 controls the temperature and pressure of the growth chamber and the flow of various gases according to the parameters of the crystal growth, such as the speed and thickness. When the crystal reaches the predetermined thickness, the control module 101 may control the driving module 110, and further control the mechanical structure 111 to stop the growth of the crystal. Specifically, the control module 101 may control the driving module 110, and the driving module 110 controls one or more channels to be opened, and the substrate on which the crystal is grown is conveyed out of the growth chamber through the mechanical structure 111 (e.g., a transmission assembly).
In some embodiments, the crystal growth apparatus can include a buffer chamber for cooling the assembled crystal. The buffer cavity comprises one or more channels, one or more gas inlets and outlets, a heating assembly and a transmission assembly. In some embodiments, the combined crystal is transferred from the mechanical structure 111 into a buffer chamber and cooled at a temperature. The cooled combined crystal can be conveyed out of the buffer cavity. In some embodiments, the control module 101 may control the driving module 110 to open one or more channels on the buffer chamber, and the combined crystal is transferred out of the buffer chamber through the mechanical structure 111 (e.g., the transmission assembly).
In some embodiments, the crystal growth apparatus can include an end cavity for further cooling of the combined crystal. The end cavity comprises one or more channels, one or more gas inlets and outlets, a heating assembly and a transmission assembly. The combined crystal after cooling in the buffer chamber is transferred from the mechanical structure 111 to the end chamber where it is further cooled at a temperature. The cooled combined crystals can be transported out of the end cavity. In some embodiments, the control module 101 can control the drive module 110 to open one or more channels on the end chamber to deliver the composite crystal out of the end chamber through the mechanical structure 111 (e.g., a transmission assembly).
In some embodiments, the drive module 110 may include one or more drive power sources. In some embodiments, the driving force source may include a driving motor driven with electric power. In some embodiments, the driving motor may be one or a combination of dc motor, ac induction motor, permanent magnet motor, switched reluctance motor, and the like. In some embodiments, the drive module 110 may include one or more drive motors. In some embodiments, the detection module 102 detects that the crystal growth thickness has reached the process requirement, and the control module 101 may control the driving module 110 to operate to drive the mechanical structure 111 to perform the corresponding operation. In some embodiments, the control module 101 issues commands that comprise an electrical signal comprising the desired operating state and duration. The driving force source of the driving module 110 is configured according to the content of the electrical signal (e.g., the driving motor in the driving module 110 rotates at a specific speed per minute for a specific duration), and the rotation of the driving motor drives the state of the mechanical structure 111 connected to the driving motor to change (e.g., the transmission assembly advances and stops, the cavity channel is opened and closed, and the gas inlet and outlet are opened and closed), so as to transfer the combined crystal to the growth cavity. In some embodiments, when the polishing module 104 polishes the substrate, the control module 101 may send a control command to the driving module 110, and the driving module 110 drives the polishing apparatus to operate according to the control command.
The mechanical structure 111 is not limited to the above-described transmission assembly, passages, gas inlets and outlets, polishing equipment, etc., but may be other structures, and the specific structure is based on the type of structure required in the crystal preparation system 100, and is not limited herein. Any mechanical mechanism that can use the crystal production method embodied in this specification is within the scope of this specification.
In some embodiments, the communication module 112 may be used for the exchange of information or data. In some embodiments, communication module 112 may be used for communication between components within crystal preparation system 100 (e.g., control module 101, detection module 102, heating module 103, vacuum module 106, input/output module 114, and/or drive module 110). In some embodiments, the detection module 102 may send system information (e.g., temperature, pressure, gas flow, etc. data) to the communication module 112, and the communication module 112 may send this information to the control module 101 for the control module 101 to determine whether to adjust the operating parameters of other modules (e.g., heating module 103, vacuum module 106); if it is determined that the operating parameters need to be adjusted, the control module 101 sends the adjusted operating parameters to the relevant modules through the communication module 112. In some embodiments, the communication module 112 may also be used for communication between the crystal preparation system 100 and other external devices (e.g., servers, user terminals, etc.). In some embodiments, the communication module 112 may transmit status information (e.g., operating parameters, etc.) of the crystal preparation system 100 to a user terminal, which may monitor the crystal preparation system 100 based on the status information. The communication module 112 may employ wired, wireless, and hybrid wired/wireless technologies. The cabling may be based on one or more fiber optic cable combinations, such as metallic cables, hybrid cables, fiber optic cables, and the like. The wireless technologies may include Bluetooth (Bluetooth), wireless network (Wi-Fi), ZigBee (ZigBee), Near Field Communication (NFC), Radio Frequency Identification (RFID), cellular networks (including GSM, CDMA, 3G, 4G, 5G, etc.), narrowband Internet of Things over cellular (NBIoT), and so on. In some embodiments, the communication module 112 may encode the transmitted information using one or more encoding schemes, for example, the encoding schemes may include phase encoding, non-return-to-zero encoding, differential manchester encoding, and the like. In some embodiments, the communication module 112 may select different transmission and encoding modes according to the type of data or the type of network that needs to be transmitted. In some embodiments, the communication module 112 may include one or more communication interfaces for different communication means. In some embodiments, other modules (e.g., heating modules 103) in crystal production system 100 may be dispersed over multiple chambers, in which case the other individual modules may each include one or more communication modules 112 for inter-module information transfer. In some embodiments, the communication module 112 may include one receiver and one transmitter. In other embodiments, the communication module 112 may be a transceiver. In some embodiments, the communication module 112 may also have a reminder or/and alarm function. In some embodiments, the communication module 112 may send a warning message or alarm message to a field operator and/or user terminal when the crystal preparation system 100 fails (e.g., the temperature or pressure of the crystal growth is exceeded). In some embodiments, the alert means may include an audible alert, a light alert, a remote alert, etc., or any combination thereof. In some embodiments, when the alert mode is remote alert, the communication module 112 may send a reminder message or an alert message to the associated user terminal, and the communication module 112 may also establish communication (e.g., voice call, video call) between the field operator and the associated user terminal. In some embodiments, communication module 112 may also send a prompt to a field operator or/and a user terminal when crystal preparation system 100 is operating properly. In some embodiments, the communication module 112 may send a prompt to an associated user terminal that the temperature or pressure meets the process requirements.
In some embodiments, power module 113 may provide power to other modules and components in crystal preparation system 100 (e.g., detection module 102, control module 101, communication module 112, input/output module 114, drive module 110). The power supply module 113 may receive control signals from the control module 101 to control the power output of the crystal preparation system 100. In some embodiments, in the event that no operation of certain modules by the control module 101 is received within a certain period of time (e.g., 1s, 2s, 3s, or 4s), the power module 113 may only provide power to the modules that are running, causing the crystal preparation system 100 to enter a power saving mode. In some embodiments, in the event that all modules of crystal preparation system 100 do not receive any operation for a certain period of time (e.g., 1s, 2s, 3s, or 4s), power module 113 may disconnect power to other modules and the data in crystal preparation system 100 may be dumped to a hard disk. In some embodiments, the power module 113 may include at least one power source. The power supply can comprise one or a combination of a plurality of fuel oil generators, gas generators, coal generators, solar generators, wind energy generators, hydroelectric generators and the like. The oil-fired generator, the gas-fired generator, and the coal-fired generator may convert chemical energy into electric energy and store the electric energy in the power supply module 113. The solar generator may convert light energy into electrical energy and store the electrical energy in the power supply module 113. The wind power generator may convert wind energy into electric energy and store the electric energy in the power supply module 113. The hydro-generator may convert mechanical energy to electrical energy and store in the power module 113. In some embodiments, when the voltage of the power supply module 113 is not stable, the control module 101 may send a control signal to the communication module 112, which may control the communication module 112 to issue a voice alert to the user terminal and/or the field operator. The voice prompt may include information that the power module 113 is unstable in voltage. In some embodiments, the power supply module 113 may include a backup power source, and the power supply module 113 may temporarily supply power using the backup power source in case of emergency (e.g., circuit failure, power failure of the external power system).
The input/output module 114 may acquire, transmit, and send signals. Input/output module 114 may be connected to or in communication with other components in crystal preparation system 100. Other components in crystal preparation system 100 may be connected or in communication via input/output module 114. The input/output module 114 may be a wired USB interface, a serial communication interface, a parallel communication interface, or a wireless bluetooth, infrared, Radio-frequency identification (RFID), Wlan Authentication and Privacy Infrastructure (wap), General Packet Radio Service (GPRS), Code Division Multiple Access (CDMA), or the like, or any combination thereof. In some embodiments, the input/output module 114 may be connected to a network and obtain information over the network. In some embodiments, the input/output module 114 may obtain crystal growth information from the detection module 102 for output via the network or communication module 112. In some embodiments, the input/output module 114 may obtain alerts or control instructions from the control module 101 through the network or communication module 112. In some embodiments, the input/output module 114 may include VCC, GND, RS-232, RS-485 (e.g., RS485-A, RS485-B), a general network interface, and the like, or any combination thereof. In some embodiments, the input/output module 114 may encode the transmitted signal using one or more encoding schemes. The encoding may include phase encoding, non-return-to-zero code, differential manchester code, or the like, or any combination thereof.
It should be understood that the system and its modules shown in FIG. 1 may be implemented in a variety of ways. For example, in some embodiments, the system and its modules may be implemented in hardware, software, or a combination of software and hardware. Wherein the hardware portion may be implemented using dedicated logic; the software portions may be stored in a memory for execution by a suitable instruction execution system, such as a microprocessor or specially designed hardware. Those skilled in the art will appreciate that the methods and systems described above may be implemented using computer executable instructions and/or embodied in processor control code, such code being provided, for example, on a carrier medium such as a diskette, CD-or DVD-ROM, a programmable memory such as read-only memory (firmware), or a data carrier such as an optical or electronic signal carrier. The system and its modules of one or more embodiments of the present specification may be implemented not only by hardware circuits such as very large scale integrated circuits or gate arrays, semiconductors such as logic chips, transistors, or programmable hardware devices such as field programmable gate arrays, programmable logic devices, etc., but also by software executed by various types of processors, for example, or by a combination of hardware circuits and software (e.g., firmware).
It should be noted that the above description of the crystal preparation system and its modules is merely for convenience of description and does not limit one or more embodiments of the present disclosure to the scope of the illustrated embodiments. It will be appreciated by those skilled in the art that, given the teachings of the present system, any combination of the various modules, or the connection of the constituent subsystems to other modules, or the omission of one or more of the modules, may be made without departing from such teachings. In some embodiments, the detection module 102 and the control module 101 may be one module that may have the functionality to detect and control crystal growth information. Such variations are within the scope of one or more embodiments of the present description.
In some embodiments, a multi-chamber growth apparatus may be used to prepare a composite crystal comprising a substrate and a target crystal. In some embodiments, the target crystal may include a silicon carbide crystal, a silicon nitride crystal, a molybdenum disulfide crystal, a boron nitride crystal, a graphene crystal, or the like. In some embodiments, the composite crystal is a composite crystal comprising a substrate and a silicon carbide crystal. In some embodiments, at least one layer of silicon carbide crystal can be deposited on the surface of the substrate to produce a composite crystal.
FIG. 2A is an exemplary schematic structural diagram of a multi-chamber growth apparatus according to some embodiments; fig. 2B is a top view of an exemplary distribution of cavities in a multi-cavity growth apparatus according to some embodiments. For convenience of illustration, the cross section of each cavity in the multi-cavity device in fig. 2A-2B is rectangular (each corresponding cavity is a cube), and it should be noted that the cross section of each cavity may also be circular, polygonal or other shape, and each corresponding cavity is a cylinder, polygonal column or other shape.
In some embodiments, as shown in FIG. 2A, the multi-chamber growth apparatus 200 may include an in-situ etch chamber 202, a carbonization chamber 203, a growth chamber 204, a buffer chamber 205, a tray 207, a drive assembly 208, and a control assembly (not shown).
The in-situ etch chamber 202 may be configured to provide a space for an in-situ etch process, wherein a gas may be introduced into the space under certain reaction conditions to perform the in-situ etch process on the substrate. The surface of the substrate can be subjected to vapor deposition to generate a film, and the substrate can support and improve the characteristics of the film deposited on the surface. In some embodiments, the substrate is transferred into the in-situ etch chamber 202 via the transfer assembly 208 and subjected to an in-situ etch process at the substrate surface under a temperature, a gas pressure, and hydrogen gas. In some embodiments, the in-situ etch chamber 202 may be evacuated to a set pressure and the substrate may be transferred to the in-situ etch chamber 202 via the transfer assembly 208; continuing to evacuate the in-situ etch chamber 202 to a set lower pressure, slowly adjusting the temperature to a certain temperature and holding for a period of time; an etching gas (e.g., hydrogen, tetrafluoromethane, sulfur hexafluoride, nitrogen trifluoride, etc.) is introduced to normal pressure, and the substrate is subjected to in-situ etching treatment by adjusting the temperature to a certain temperature and maintaining the temperature for a long period of time. Further details regarding the in-situ etching process performed on the substrate can be found in the description of fig. 13.
The carbonization chamber 203 may be used to provide a space for a carbonization process, and a gas may be introduced thereinto under a certain reaction condition to perform the carbonization process on the substrate. In some embodiments, the substrate is transferred into the carbonization chamber 203 by the drive assembly 208 and subjected to a carbonization process at a temperature and under the influence of a carbonization gas (e.g., methane, propane, butane, etc.) and hydrogen gas at the surface of the substrate. In some embodiments, the temperature of the carbonization chamber 203 can be adjusted to a certain temperature, and then a third channel between the in-situ etching chamber 202 and the carbonization chamber 203 is controlled to be opened, the substrate is transferred into the carbonization chamber 203 through the transmission assembly 208, and the third channel is closed; cooling the carbonization cavity to a certain temperature, vacuumizing to a set pressure, then starting to heat, simultaneously introducing carbonization gas (such as methane, propane, butane and the like) and hydrogen to a set pressure, adjusting the temperature to a certain temperature, and keeping the temperature for a period of time to carry out carbonization treatment. For more on the carbonization of the substrate, reference is made to the description of fig. 14.
The growth chamber 204 may be used to provide a reaction space for vapor deposition, and the reaction materials are subjected to vapor deposition to grow a crystal on the surface of the substrate under certain reaction conditions, so as to obtain a combined crystal including the substrate and the silicon carbide crystal. In some embodiments, the substrate is transferred into the growth chamber 204 through the transfer assembly 208 and subjected to a temperature and a presence of a carbonization gas (e.g., methane, propane, butane, etc.) and hydrogen gas to effect crystal growth on the surface of the substrate. In some embodiments, the temperature of growth chamber 204 may be adjusted to a certain temperature, pressurized to a set pressure; controlling a fourth channel between the carbonization cavity 203 and the growth cavity 204 to be opened, transferring the substrate into the growth cavity 204 through the transmission assembly 208, and closing the fourth channel; then, adjusting the temperature of the growth cavity 204 to a certain temperature, introducing silane, propane and hydrogen to a set pressure, and performing crystal growth on the surface of the substrate; and when the crystal growth thickness reaches the target thickness, stopping crystal growth to obtain the combined crystal. For more on the crystal growth, reference may be made to the description of fig. 15-16.
The buffer chamber 205 may be used for cool-down cooling of the combined crystal. In some embodiments, the assembled crystal is transferred into the buffer chamber 205 through the transmission assembly 208, and cooled at a certain temperature and a certain gas pressure. In some embodiments, the buffer chamber 205 is heated to a certain temperature; controlling a fifth channel between the growth cavity 204 and the buffer cavity 205 to be opened, transferring the combined crystal into the buffer cavity 205 through the transmission assembly 208, and closing the fifth channel; the buffer chamber 205 is cooled to a certain temperature, kept for a period of time, and the combined crystal is cooled. In some embodiments, the combined crystal is transferred to the buffer chamber 205 through the transmission assembly 208, and cooled at normal temperature and pressure. For more details on cooling the combined crystal, reference may be made to the description of fig. 17.
An actuator assembly 208 may be disposed at a lower end inside each chamber (e.g., the in-situ etch chamber 202, the carbonization chamber 203, the growth chamber 204, and the buffer chamber 205) for transferring a substrate or a composite crystal between each chamber in sequence. The drive assembly 208 may also be referred to as a mechanical structure 111. For more on the drive assembly 208, reference may be made to the description of FIG. 8.
The control assembly may be used to control the rotation of the drive assembly 208 to transfer the substrate or composite crystal between the chambers (in-situ etch chamber 202, carbonization chamber 203, growth chamber 204, and buffer chamber 205) in sequence. In some embodiments, the control assembly may operate by controlling the drive motor to drive the rotation of the drive assembly 208 to sequentially transfer the substrate or composite crystal between the chambers. The control component may be the control module 101 and the drive motor may be the drive module 110.
In some embodiments, the in-situ etch chamber 202, the carbonization chamber 203, the growth chamber 204, and the buffer chamber 205 may be arranged in a substantially "in-line" configuration, with the drive assemblies 208 in each chamber connected end-to-end in series, with the substrate or composite crystal being transported in a substantially straight line between each chamber. In some embodiments, as shown in FIG. 2A, the in-situ etching chamber 202, the carbonization chamber 203, the growth chamber 204, and the buffer chamber 205 may be arranged in a "straight line" configuration, with the drive assemblies 208 in each chamber connected end-to-end in series, with the substrate or composite crystal being transported in a straight line between each chamber. In some alternative embodiments, the distribution pattern of each cavity in fig. 2A can be integrally rotated by any angle to set each cavity.
In some embodiments, as shown in fig. 2B, the in-situ etching chamber 202, the carbonization chamber 203, the growth chamber 204, and the buffer chamber 205 may be arranged in a "grid-like" shape, the in-situ etching chamber 202 is located adjacent to the carbonization chamber 203, the growth chamber 204 is located adjacent to the other side of the carbonization chamber 203, and the buffer chamber 205 is adjacent to the in-situ etching chamber 202 and the growth chamber 204; the transmission assemblies 208 in each cavity are connected end to end in sequence, and the transmission assemblies 208 can cycle between each cavity in sequence.
FIG. 3A is a schematic diagram of an exemplary configuration of a multi-chamber growth apparatus according to further embodiments; fig. 3B is a top view of an exemplary distribution of cavities in a multi-cavity growth apparatus, according to other embodiments. For convenience of illustration, the cross section of each cavity in the multi-cavity device in fig. 3A-3B is rectangular (each corresponding cavity is a cube), and it should be noted that the cross section of each cavity may also be circular, polygonal or other shape, and each corresponding cavity is a cylinder, polygonal column or other shape.
In some embodiments, the multi-chamber growth device may further comprise a vacuum chamber. In some embodiments, the multi-lumen growth device may further comprise a tip lumen. In some embodiments, as shown in fig. 3A, the multi-chamber growth apparatus 300 may include a vacuum chamber 201, an in-situ etch chamber 202, a carbonization chamber 203, a growth chamber 204, a buffer chamber 205, an end chamber 206, a tray 207, a drive assembly 208, and a control assembly (not shown), the vacuum chamber 201 being adjacent to the in-situ etch chamber 202, the end chamber 206 being adjacent to the buffer chamber 205.
The vacuum chamber 201 may be used to place the substrate in a vacuum environment. In some embodiments, the substrate is placed in a vacuum chamber 201, and the vacuum chamber 201 is evacuated such that the substrate is in a vacuum environment. In some embodiments, the first channel of the vacuum chamber may be closed, and the vacuum chamber may be evacuated to a set pressure. For more on the vacuum processing of the substrate, reference may be made to the description of fig. 12.
The tip cavity 206 may be used to cool the composite crystal to room temperature. In some embodiments, the assembled crystal is transferred from the buffer chamber 205 to the end chamber 206 via the transmission assembly 208, and the assembled crystal is cooled at normal temperature and pressure. In some embodiments, a sixth passage between the buffer chamber 205 and the end chamber 206 is controlled to open, the combined crystal is transferred into the end chamber 206 through the transmission assembly 208, and the sixth passage is closed; and cooling the combined crystal. For more details on cooling the combined crystal, reference may be made to the description of fig. 17.
In some embodiments, the individual chambers of the multi-chamber growth apparatus may be arranged in a straight line or in a non-straight line. In some embodiments, as shown in fig. 3A, the chambers (vacuum chamber 201, in-situ etching chamber 202, carbonization chamber 203, growth chamber 204, buffer chamber 205, and end chamber 206) may be arranged in a straight line in sequence, the driving components 208 in the chambers are connected in sequence end to end, and the transmission route between the chambers is a straight line. In alternative embodiments, the vacuum chamber 201, in-situ etching chamber 202, carbonization chamber 203, growth chamber 204, buffer chamber 205, and end chamber 206 may also be arranged in a substantially "in-line" configuration, with the drive assemblies 208 in each chamber connected end-to-end in series, with the substrate or composite crystal being transported in a substantially straight line between each chamber. In some alternative embodiments, the cavity may be arranged by rotating the distribution pattern of the cavities in fig. 3A and the above examples by any angle.
In some embodiments, as shown in fig. 3B, the vacuum chamber 201, the in-situ etching chamber 202, the carbonization chamber 203, the growth chamber 204, the buffer chamber 205, and the end chamber 206 may be stacked in sequence, the vacuum chamber 201 is located adjacent to the in-situ etching chamber 202, the carbonization chamber 203 is located adjacent to the in-situ etching chamber 202, the growth chamber 204 is adjacent to the buffer chamber 205 and the carbonization chamber, and the end chamber 206 is located adjacent to the buffer chamber 205; the transmission assemblies 208 in each cavity are connected end to end in sequence, and the transmission assemblies 208 can cycle between each cavity in sequence. In some alternative embodiments, the cavity may be arranged by rotating the distribution pattern of the cavities in fig. 3B and the above examples by any angle as a whole.
It is noted that the vacuum chamber 201, in-situ etching chamber 202, carbonization chamber 203, growth chamber 204, buffer chamber 205, and end chamber 206 may be arranged in sequence in any configuration that enables the substrate or composite crystal to be sequentially transferred between the chambers, and are within the scope of the present disclosure. The vacuum chamber 201, the in-situ etching chamber 202, the carbonization chamber 203, the growth chamber 204, the buffer chamber 205, and the end chamber 206 may be the same or different in size, and are not limited thereto.
The various types of cavities referred to in some embodiments of the present description include, but are not limited to, a first type of cavity, a second type of cavity, a third type of cavity, and the like. In some embodiments, the first type of chamber may provide a location for the substrate or the composite crystal to be at a set pressure or temperature. In some embodiments, the second type of chamber can provide a location for processing the substrate, or a location for subjecting the composite crystal to a certain temperature. In some embodiments, the third type of cavity may provide a site for crystal growth on the surface of the substrate.
Fig. 4 is an exemplary structural schematic of a first type of cavity, according to some embodiments.
As shown in fig. 4, the first chamber 400 is provided with an inlet channel 401 and an outlet channel 402 on the side wall, and a driving assembly 404 is installed inside the first chamber 400, and the driving assembly 404 is communicated with the inlet channel 401 and the outlet channel 402 to transfer the substrate or the combined crystal between the inlet channel 501 and the outlet channel 502. In some embodiments, the inlet channel 401 and the outlet channel 402 may be disposed on two opposite sidewalls of the first-type chamber 400 such that the inlet channel 401, the transmission assembly 404, and the outlet channel 402 form a straight line. In some embodiments, the inlet channel 401 and the outlet channel 402 may be disposed on two adjacent sidewalls of the first-type chamber 400, and the inlet channel 401, the transmission assembly 404 and the outlet channel 402 form an L-shaped broken line. In some embodiments, the inlet channel 401 and the outlet channel 402 may be disposed on the same side wall of the first chamber 400, and the inlet channel 401, the transmission assembly 404 and the outlet channel 402 form a U-shaped broken line. In some embodiments, the inlet channels 401 and the outlet channels 402 are disposed at the top, middle, and bottom ends of the sidewalls of the first-type chamber 400. For example only, as shown in fig. 4, the inlet channel 401 and the outlet channel 402 are respectively disposed at the bottom ends of two opposite sidewalls of the first-type chamber 400, and the driving assembly 404 is disposed at the bottom of the first-type chamber 400. Further details regarding the drive assembly 404 can be found in the description of FIG. 8.
In some embodiments, the shape of the inlet channel 401 and the outlet channel 402 includes, but is not limited to, rectangular, circular, oval, and any other regular or irregular shape. In some embodiments, the number of the inlet channels 401 and the outlet channels 402 may be one, or two or more. In some embodiments, the number of inlet channels 401 and outlet channels 402 may be the same or different. In some embodiments, the inlet channels 401 and outlet channels 402 are the same number and are arranged in pairs. In some embodiments, two or more sets of inlet channels 401 and outlet channels 402 may be provided, with a drive assembly 404 disposed between each set of inlet channels 401 and outlet channels 402, respectively, to simultaneously transport substrates or composite crystals from different routes. In some embodiments, the number of inlet channels 401 and outlet channels 402 is different. In some embodiments, two or more inlet channels 401 may be provided, one outlet channel 402 may be provided, and a substrate or a composite crystal may be transferred from the plurality of inlet channels 401 into the first-type chamber body 400 and from the one outlet channel 402 out of the first-type chamber body 400.
In some embodiments, automatic control valves are installed at both the inlet channel 401 and the outlet channel 402 to control the opening and closing of the inlet channel 401 and the outlet channel 402 by the control module 101. In some embodiments, the inlet channel 401 and the outlet channel 402 may be used interchangeably.
As shown in fig. 4, the first chamber 400 is provided with at least one gas pipe 403 for exhausting gas from the first chamber 400 or introducing gas into the first chamber 400 to reach a desired pressure in the first chamber 400.
In some embodiments, the gas conduit 403 may be in communication with a vacuum apparatus, and the speed and time of the vacuum may be adjusted by controlling the operating parameters (e.g., power, rotational speed, operating time, etc.) of the vacuum apparatus to control the pressure variations within the first-type chamber 400. In some embodiments, the evacuation device may comprise a vacuum pump. In some embodiments, the number of gas conduits 403 may be one or more. In some embodiments, the number of vacuum pumps may be one vacuum pump or more than two. In some embodiments, the gas pipes 403 may be disposed at the top, side wall, bottom of the first-type chamber 400. For example, as shown in fig. 4, a gas pipe 403 is disposed at the bottom of the first-type chamber 400. In some embodiments, the gas pipes 403 are disposed on either side wall or the top of the first-type chamber 400. In some embodiments, the gas pipe 403 may be in communication with a gas storage tank through a pipe, and a flow regulating valve may be disposed on the pipe to control the flow rate and flow rate of the introduced gas.
In some embodiments, the first-type chamber 400 may be the vacuum chamber 201, and may also be the tip chamber 206.
The vacuum chamber 201 may be the first chamber of a multi-chamber crystal growth apparatus. The vacuum chamber may be evacuated through gas line 403.
The tip chamber 206 may be the last chamber of a multi-chamber crystal growth apparatus. In some embodiments, the tip cavity 206 may not use the gas conduit 403, i.e., the gas conduit 403 is in a closed state. In some embodiments, where the gas lines 403 include two or more, the temperature in the tip cavity 206 can be increased by introducing gas (e.g., displacing gas) into the tip cavity 206 through one or more of the gas lines 403 and removing gas from the tip cavity 206 through another one or more of the gas lines 403.
In some embodiments, the shape of the first-type cavity 400 may include, but is not limited to, a regular or irregular shape of a cylinder, a prism, a cube, a rectangular cylinder, and the like. The size of the first chamber 400 can be set according to actual production needs. In some embodiments, the height of the top wall of the first-type cavity 400 from the combined crystal growth plane may be 20-500 mm. In some embodiments, the height of the top wall of the first-type cavity 400 from the growth surface of the composite crystal may be 50-400 mm. In some embodiments, the height of the top wall of the first-type cavity 400 from the growth surface of the composite crystal assembly may be 100-300 mm. In some embodiments, the height of the top wall of the first-type cavity 400 from the composite crystal growth plane may be 150-250 mm.
In some embodiments, the material of the first chamber 400 may include high-strength stainless steel or high-strength aluminum alloy. Wherein, the strength of the high-strength stainless steel or the high-strength aluminum alloy can ensure safe production, and the first-class cavity 400 does not deform or break in the production process.
Fig. 5 is an exemplary schematic structure diagram of a second type of cavity according to some embodiments.
As shown in FIG. 5, the side wall of the second type chamber 500 is provided with an inlet channel 501 and an outlet channel 502, and a driving assembly 506 is arranged inside the second type chamber 500, and the driving assembly 506 is communicated with the inlet channel 501 and the outlet channel 502 to transfer the substrate or the combined crystal between the inlet channel 501 and the outlet channel 502. In some embodiments, the inlet channel 501 and the outlet channel 502 may be disposed on two opposite sidewalls of the second type chamber 500, such that the inlet channel 501, the transmission assembly 506, and the outlet channel 502 form a straight line. In some embodiments, the inlet channel 501 and the outlet channel 502 may be disposed on two adjacent sidewalls of the second type chamber 500, and the inlet channel 501, the transmission assembly 506 and the outlet channel 502 form an L-shaped broken line. In some embodiments, the inlet channel 501 and the outlet channel 502 may be disposed on the same side wall of the second type chamber 500, and the inlet channel 501, the transmission assembly 506 and the outlet channel 502 form a U-shaped broken line. In some embodiments, the inlet channel 501 and the outlet channel 502 are disposed at the top, middle, and bottom ends of the sidewalls of the second-type chamber 500. For example only, as shown in fig. 5, the inlet channel 501 and the outlet channel 502 are respectively disposed at the bottom ends of two opposite sidewalls of the second type chamber 500, and the transmission assembly 506 is disposed at the bottom of the second type chamber 500. For more on the drive assembly 506, reference may be made to the description of FIG. 8.
In some embodiments, the shapes of the inlet channel 501 and the outlet channel 502 include, but are not limited to, rectangular, circular, oval, and any other regular or irregular shape. In some embodiments, the number of the inlet channels 501 and the outlet channels 502 may be one, or two or more. In some embodiments, the number of inlet channels 501 and outlet channels 502 may be the same or different. In some embodiments, the inlet channels 501 and outlet channels 502 are the same number and are arranged in pairs. In some embodiments, two or more sets of inlet 501 and outlet 502 channels may be provided, with a drive assembly 506 disposed between each set of inlet 501 and outlet 502 channels, respectively, to simultaneously transport substrates or composite crystals from different routes. In some embodiments, the number of inlet channels 501 and outlet channels 502 is different. In some embodiments, two or more inlet channels 501 may be provided, and one outlet channel 502 may be provided, and a substrate or a composite crystal may be transferred from the plurality of inlet channels 501 into the second type of chamber 500 and transferred from the one outlet channel 502 out of the second type of chamber 500.
In some embodiments, automatic control valves are installed at both the inlet channel 501 and the outlet channel 502 to control the opening and closing of the inlet channel 501 and the outlet channel 502 by the control module 101. In some embodiments, the inlet channel 501 and the outlet channel 502 may be used interchangeably.
As shown in fig. 5, the second-type chamber 500 includes at least one evacuation line 503 for evacuating the second-type chamber 500 to a desired pressure within the second-type chamber 500. In some embodiments, the pumping duct 503 may be disposed at the bottom, the top, or the side wall of the second-type chamber 500. For example, as shown in FIG. 5, the pumping duct 503 is disposed at the bottom of the second type chamber 500. In some embodiments, the pumping duct 503 is disposed on any sidewall or top of the second type chamber 500. In some embodiments, the evacuation line 503 may be in communication with an evacuation device, and the speed and time of evacuation may be adjusted by controlling the operating parameters (e.g., power, rotational speed, operating time, etc.) of the evacuation device to control the pressure changes within the second type of chamber 500. In some embodiments, the evacuation device may comprise a vacuum pump. In some embodiments, the number of the pumping duct 503 may be one or more. In some embodiments, the number of vacuum pumps may be one or more than two.
In some embodiments, the second type chamber 500 includes at least one gas inlet conduit 504 for introducing gas into the second type chamber 500. In some embodiments, the inlet duct 504 may be disposed at the bottom, top, or side wall of the second type cavity 500. For example, as shown in FIG. 5, an air inlet duct 504 is disposed at the top of the second type of cavity 500. In some embodiments, the number of intake conduits 504 may be one or more. In some embodiments, one inlet conduit 504 may be provided, and all gases may be passed from the same inlet conduit 504 into the second type of chamber 500. In some embodiments, two or more gas inlet conduits 504 may be provided, with different gases passing from different gas inlet conduits 504 to the second type of chamber 500. In some embodiments, a flow regulating valve may be disposed on each inlet conduit 504 to control the flow rate of each gas, and thus the ratio (e.g., mass ratio or molar ratio) of each gas.
As shown in fig. 5, the second-type cavity 500 is further provided with a heating body 505 for adjusting the temperature of the second-type cavity 500 to control the temperature of the second-type cavity 500 to reach a desired temperature. In some embodiments, the temperature in the second type of cavity 500 can be adjusted by controlling the heating power and heating time of the heating body 505. In some embodiments, the heating body 505 may be disposed on the outer top wall, the outer side wall, the inner top wall, the inner side wall, or any combination thereof of the second-type cavity 500. For example, as shown in fig. 5, the heating body 505 is disposed on the inner sidewall of the second-type cavity 500.
In some embodiments, heater 505 may include, but is not limited to, a resistive heating assembly, an electromagnetic induction heating assembly, and/or the like. In some embodiments, the resistive heating component may comprise a graphite resistor or a carbon silicon rod resistor. After the graphite resistor or the carbon silicon rod resistor is electrified, the temperature of the second cavity 500 can be adjusted by using heat energy generated by joule effect of current flowing through the resistor. In some embodiments, the electromagnetic induction heating assembly may comprise an inductive coil. The induction coil can produce the vortex on second class cavity 500 under the alternating current effect of different frequencies, and under the vortex effect, the electric energy that produces on second class cavity 500 can change into heat energy to carry out temperature regulation to second class cavity 500.
In some embodiments, heating body 505 may include one or more heating elements.
In some embodiments, the heater 505 may include one or more resistive heating elements, and each resistive heating element may be uniformly or non-uniformly disposed on the sidewall of the second-type cavity 500. In some embodiments, the heating body 505 may include 5 graphite resistors, the second-type cavity 500 may be cylindrical, and the 5 graphite resistors are circumferentially disposed at equal intervals on the sidewall of the second-type cavity 500, i.e., each graphite resistor is located at one fifth of the sidewall of the second-type cavity 500. In some embodiments, the heater 505 may include 4 graphite resistors, the second-type cavity 500 may have a rectangular column shape, 4 graphite resistors may be respectively disposed on four sidewalls of the second-type cavity 500, or 4 graphite resistors may be respectively disposed at four corners of the second-type cavity 500.
In some embodiments, the heating body 505 may include one or more induction heating elements, and each induction heating element may be uniformly or non-uniformly disposed on the outer sidewall of the second-type cavity 500. In some embodiments, heater 505 may include multiple turns of induction coils, which may be helically wound around the outside wall of second-type cavity 500. Further, the induction coil may be wound around the entire outer sidewall of the second-type cavity 500, or may be wound around the outer sidewall of the second-type cavity 500 corresponding to the position of the tray.
In some embodiments, the second type of chamber 500 may be an in-situ etch chamber 202, a carbonization chamber 203, or a buffer chamber 205.
An in-situ etch chamber 202 may be disposed adjacent to the vacuum chamber 201. In some embodiments, the in-situ etch chamber 202 and the vacuum chamber 201 may share the same channel, i.e., the outlet channel 402 of the vacuum chamber 201 and the inlet channel 501 of the in-situ etch chamber 202 are the same channel. In some embodiments, the in-situ etch chamber 202 and the vacuum chamber 201 may not share the same channel, and the outlet channel 402 of the vacuum chamber 201 and the inlet channel 501 of the in-situ etch chamber 202 are two channels and are disposed adjacent to each other. In some embodiments, the in-situ etching chamber 202 may be temperature-regulated by the heater 505, the in-situ etching chamber 202 may be evacuated by the evacuation line 503, and the substrate may be etched in situ by introducing hydrogen into the in-situ etching chamber 202 through the gas inlet line 504.
The carbonization chamber 203 can be disposed adjacent to the in-situ etch chamber 202. In some embodiments, the carbonization chamber 203 and the in-situ etch chamber 202 may share the same channel, i.e., the outlet channel of the in-situ etch chamber 202 and the inlet channel of the carbonization chamber 203 are the same channel. In some embodiments, the carbonization chamber 203 and the in-situ etching chamber 202 may not share the same channel, and the outlet channel of the in-situ etching chamber 202 and the inlet channel of the carbonization chamber 203 are two channels and are disposed adjacent to each other. In some embodiments, the temperature of the carbonization chamber 203 can be adjusted by the heating body 505, the carbonization chamber 203 can be vacuumized by the evacuation pipe 503, and the carbonization gas (e.g., methane, propane, butane, etc.) and hydrogen can be introduced into the carbonization chamber 203 through the gas inlet pipe 504 to perform carbonization treatment on the substrate.
The buffer cavity 205 may be disposed adjacent to the tip cavity 206. In some embodiments, the buffer cavity 205 and the tip cavity 206 may share the same channel, i.e., the outlet channel 502 of the buffer cavity 205 and the inlet channel 401 of the tip cavity 206 are the same channel. In some embodiments, the buffer chamber 205 and the end chamber 206 may not share the same channel, and the outlet channel 502 of the buffer chamber 205 and the inlet channel 401 of the end chamber 206 are two channels and are disposed adjacent to each other. In some embodiments, buffer cavity 205 may be temperature regulated by heater 505. In some embodiments, the buffer chamber 205 may not use the suction duct 503 and the inlet duct 504, i.e. the suction duct 503 and the inlet duct 504 are in a closed state. In some embodiments, the gas may be introduced into the buffer chamber 205 through the gas inlet pipe 504, and the gas in the buffer chamber 205 may be exhausted through the gas exhaust pipe 503 to accelerate the cooling rate in the buffer chamber 205.
In some embodiments, the shape of the second-type cavity 500 includes, but is not limited to, a regular or irregular shape of a cylinder, a prism, a cube, a rectangular cylinder, and the like. The size of the second chamber 500 can be set according to actual production needs. In some embodiments, the height of the top wall of the second-type cavity 500 from the combined crystal growth plane may be 20-300 mm. In some embodiments, the height of the top wall of the second-type cavity 500 from the combined crystal growth plane may be 50-200 mm. In some embodiments, the height of the top wall of the second-type cavity 500 from the combined crystal growth plane may be 70-180 mm. In some embodiments, the height of the top wall of the second-type cavity 500 from the combined crystal growth plane may be 100-150 mm.
In some embodiments, the cavity wall of the second-type cavity 500 may be made of a double-layer hollow high-strength stainless steel or aluminum alloy, and cooling water is introduced into the hollow cavity to cool the cavity wall, thereby performing heat insulation and heat dissipation functions. In some embodiments, one or more layers of thermal insulation material are disposed inside the walls of the second type of cavity 500. In some embodiments, the insulating material may include graphite felt, zirconia felt.
Fig. 6 is an exemplary structural schematic diagram of a third type of cavity according to some embodiments.
In some embodiments, the third type of cavities 600 may be growth cavities 204. As shown in FIG. 6, the third type of chamber 600 (or referred to as the growth chamber 204) has an inlet channel 601 and an outlet channel 602 on its side wall, and a driving assembly 608 is installed inside the third type of chamber 600, and the driving assembly 608 is connected to the inlet channel 601 and the outlet channel 602 to transfer the substrate or the composite crystal between the inlet channel 601 and the outlet channel 602. In some embodiments, the inlet channel 601 and the outlet channel 602 may be disposed on two opposite sidewalls of the third type chamber 600, such that the inlet channel 601, the transmission assembly 608, and the outlet channel 602 form a straight line. In some embodiments, the inlet channel 601 and the outlet channel 602 may be disposed on two adjacent sidewalls of the third type chamber 600, and the inlet channel 601, the transmission assembly 608 and the outlet channel 602 form an L-shaped broken line. In some embodiments, the inlet channel 601 and the outlet channel 602 may be disposed on the same side wall of the third type chamber 600, and the inlet channel 601, the transmission assembly 608 and the outlet channel 602 form a U-shaped broken line. In some embodiments, the inlet channel 601 and the outlet channel 602 are disposed at the top, middle, and bottom ends of the sidewalls of the third type chamber 600. For example only, as shown in fig. 6, the inlet channel 601 and the outlet channel 602 are respectively disposed at the bottom ends of two opposite sidewalls of the third type chamber 600, and the transmission assembly 608 is disposed at the bottom of the third type chamber 600. For more on the drive assembly 608, reference may be made to the description of FIG. 8.
In some embodiments, the shape of the inlet channel 601 and the outlet channel 602 includes, but is not limited to, rectangular, circular, oval, and any other regular or irregular shape. In some embodiments, the number of the inlet channel 601 and the outlet channel 602 may be one, or two or more. In some embodiments, the number of inlet channels 601 and outlet channels 602 may be the same or different. In some embodiments, the inlet channels 601 and outlet channels 602 are the same number and are arranged in pairs. In some embodiments, two or more sets of inlet channels 601 and outlet channels 602 may be provided, with a drive assembly 608 disposed between each set of inlet channels 601 and outlet channels 602, respectively, to simultaneously transport substrates or composite crystals from different routes. In some embodiments, the number of inlet channels 601 and outlet channels 602 is different. In some embodiments, two or more inlet channels 601 may be provided, and one outlet channel 602 may be provided, and a substrate or a composite crystal may be transferred from the plurality of inlet channels 601 into the third type of chamber 600 and from the one outlet channel 602 out of the third type of chamber 600.
In some embodiments, automatic control valves are installed at both the inlet channel 601 and the outlet channel 602 to control the opening and closing of the inlet channel 601 and the outlet channel 602 by the control module 101. In some embodiments, the inlet channel 601 and the outlet channel 602 may be used interchangeably.
In some embodiments, the third type of chamber 600 comprises at least one evacuation conduit 603 for evacuating the third type of chamber 600 to bring the pressure in the third type of chamber 600 to a desired pressure. In some embodiments, the pumping duct 603 may be disposed at the bottom, top, or side wall of the third type of cavity 600. In some embodiments, as shown in FIG. 6, the pumping duct 603 is disposed at the bottom of the third type of cavity 600. In some embodiments, the pumping duct 603 is disposed on either side wall or the top of the third type of cavity 600. In some embodiments, the evacuation conduit 603 may be in communication with a vacuum evacuation device, and the speed and time of evacuation may be adjusted by controlling the operating parameters (e.g., power, rotational speed, operating time, etc.) of the vacuum evacuation device to control pressure variations within the third type of chamber 600. In some embodiments, the evacuation device may comprise a vacuum pump. In some embodiments, the number of evacuation ducts 603 may be one or more. In some embodiments, the number of vacuum pumps may be one or more than two.
In some embodiments, the third type chamber 600 includes at least one gas inlet pipe 604 for introducing a reaction gas. For example, silane and propane. In some embodiments, the inlet duct 604 may be disposed at the top, bottom, or side wall of the third type chamber 600. In some embodiments, as shown in FIG. 6, an air inlet duct 604 is disposed at the top of the third type of cavity 600. In some embodiments, the number of intake conduits 604 may be one or more. In some embodiments, one inlet duct 604 may be provided, and all gases may be passed from the same inlet duct 604 into the third type of chamber 600. In some embodiments, two or more gas inlet conduits 604 may be provided, and different gases may be introduced into the third type chamber 600 from different gas inlet conduits 604. In some embodiments, a flow regulating valve may be disposed on each of the gas inlet conduits 604 to control the flow rate of each gas, thereby controlling the ratio (e.g., mass ratio or molar ratio) of each gas.
In some embodiments, the third type of cavity 600 (or referred to as the growth cavity 204) is provided with a heating body 605 for adjusting the temperature of the growth cavity 204 to control the temperature in the growth cavity 204 to reach a desired temperature. In some embodiments, the temperature within the growth chamber 204 may be adjusted by controlling the heating power and heating time of the heater 605. In some embodiments, the heating body 605 may be disposed on the outer top wall, the outer side wall, the inner top wall, the inner side wall, or any combination thereof of the growth cavity 204. In some embodiments, as shown in fig. 6, the heating body 605 is disposed on the inner sidewall of the growth cavity 204.
In some embodiments, heating body 605 may include, but is not limited to, a resistive heating assembly, an electromagnetic induction heating assembly, and/or the like. In some embodiments, the resistive heating component may comprise a graphite resistor or a carbon silicon rod resistor. In some embodiments, the electromagnetic induction heating assembly may comprise an inductive coil. For more on heating body 605, reference is made to the description of heating body 505.
In some embodiments, the growth chamber 204 further comprises a rotating shaft 606 (which may also be referred to as rotating shaft 207), the rotating shaft 606 being disposed at the bottom of the growth chamber 204 for jacking the tray 607 to the middle of the growth chamber 204. For more on the tray, reference may be made to the description of fig. 7. In some embodiments, the height of the rotational axis 606 may comprise 10-200 mm. In some embodiments, the height of the rotational axis 606 may comprise 20-180 mm. In some embodiments, the height of the rotational axis 606 may comprise 30-150 mm. In some embodiments, the height of the rotational axis 606 may comprise 40-130 mm. In some embodiments, the height of the rotational axis 606 may comprise 50-100 mm. In some embodimentsThe height of the rotation axis 606 may comprise 60-80 mm. In some embodiments, the height of the rotation axis 606 may be the height of the growth chamber 204
Figure BDA0003006628400000301
In some embodiments, the height of the rotation axis 606 may be the height of the growth chamber 204
Figure BDA0003006628400000302
In some embodiments, the height of the rotation axis 606 may be the height of the growth chamber 204
Figure BDA0003006628400000303
In some embodiments, the height of the rotation axis 606 may be the height of the growth chamber 204
Figure BDA0003006628400000304
In some embodiments, the height of the rotation axis 606 may be the height of the growth chamber 204
Figure BDA0003006628400000305
In some embodiments, a positioner (not shown) is mounted on the rotating shaft 606 for detecting the position of the tray 607. In some embodiments, the positioner may be a displacement sensor. In some embodiments, a positioner may be provided at the top of the rotating shaft 606, which may detect the position of the tray 607 in real time and lift the tray 607 to the middle of the growth chamber 204 via the rotating shaft 606. In some embodiments, the positioner detects the position of the tray 607 in real time and sends the position information of the tray 607 to the control module 101, and when the positioner detects that the tray 607 is transferred to the position right above the rotating shaft 606 by the transmission assembly 608, the control module 101 may control the transmission assembly 608 to stop rotating through the driving module 110, and control the rotating shaft 606 to smoothly jack up the tray 607 to the middle of the growth chamber 204 through the driving module 110. In some embodiments, the rotation axis 606 may be continuously rotated during the growth process to make the substrate reaction uniform at various locations. In some embodiments, the locator may also be a GPS locator. In some embodiments, a GPS locator may be mounted on the tray 607 for transmitting the location information of the tray 607 to the control module 101 in real time.
Fig. 7 is a schematic diagram of an exemplary structure of a tray according to some embodiments.
In some embodiments, the multi-chamber growth apparatus includes a tray 207. In some embodiments, as shown in FIG. 7, the tray 207 is provided with at least one recess 207-1, and each recess 207-1 can receive a substrate. In some embodiments, the shape of the tray 207 includes, but is not limited to, a circle, an oval, a triangle, a rectangle, a polygon, or any other regular or irregular shape. In some embodiments, one or more than two grooves 207-1 may be provided on the upper surface of each tray 207. In some embodiments, the number of grooves 207-1 may be 1, 2, 4, 7, 11, etc. In some embodiments, the grooves 207-1 may be arranged uniformly or non-uniformly. In some embodiments, as shown in FIG. 7, the tray 207 is circular and the 6 grooves 207-1 are evenly circumferentially arranged on the upper surface of the tray 207.
In some embodiments, the tray 207 is further centrally provided with a jacking structure engaged with the rotating shaft 606, and when the tray 207 is transferred right above the rotating shaft 606, the rotating shaft 606 is engaged with the jacking structure, so that the tray 207 is smoothly jacked up to a desired height. In some embodiments, the jacking structure may be snap-fit to the rotating shaft 606. In some embodiments, the lifting structure may be a positioning hole 207-2 at the center of the tray 207, the top end of the rotating shaft 606 is a shaft with a sectional area smaller than the middle or the bottom end, and the top end of the rotating shaft 606 may be inserted into the positioning hole 207-2, so that the rotating shaft 606 can lift the tray 207 stably.
FIG. 8 is an exemplary schematic diagram of a transmission assembly according to some embodiments.
As shown in fig. 8, the transmission assembly 208 includes at least two cylindrical rollers 208-1 arranged in parallel and two transmission frames 208-2 arranged in parallel at the upper and lower ends of the cylindrical rollers 208-1, and the two transmission frames 208-2 are fixedly arranged below the cavities (not shown in fig. 8), so that the cylindrical rollers 208-1 are axially confined between the two transmission frames 208-2 and can rotate around their own axes. In some embodiments, the upper and lower ends of the cylindrical roller 208-1 are cylinders, and the sectional area of the upper and lower ends is smaller than that of the middle portion, and the transmission frame 208-2 is provided with a plurality of holes having a sectional area larger than that of the upper and lower ends of the cylindrical roller 208-1, so that the upper and lower ends of the cylindrical roller 208-1 can be inserted between the two transmission frames 208-2 and can rotate around its own axis. As shown in fig. 8, the tray 207 may be placed on the cylindrical roller 208-1, and as the cylindrical roller 208-1 rotates, the tray 207 is transferred forward by static friction between the bottom of the tray 207 and the cylindrical roller 208-1.
In some embodiments, the number of cylindrical rollers 208-1 may be determined based on the length of the transmission frame 208-2 and the diameters of the upper and lower ends of the cylindrical rollers 208-1. In some embodiments, the product of the diameter of the upper and lower ends of the cylindrical roller 208-1 and the number of cylindrical rollers 208-1 is less than or equal to the length of the drive frame 208-2. In some embodiments, the number of cylindrical rollers 208-1 may be 7, 8, 9, or 10. In some embodiments, the distance between the cylindrical rollers 208-1 can be set according to actual production requirements, so as to ensure that the tray 207 can be conveyed forward as the cylindrical rollers 208-1 rotate.
In some embodiments, the carrier 208-2 may be provided with a straight line or may be provided with an angled corner. In some embodiments, two drive frames 208-2 are each arranged as a 90L-frame and are arranged in parallel between the cylindrical rollers 208-1. It should be noted that the arrangement form of the transmission frame 208-2 is not limited, and the transmission assembly 208 can be ensured to communicate with the inlet channel and the outlet channel of each cavity, so that the tray 207 can be transmitted into and out of each cavity.
The vacuum chamber 201, the in-situ etching chamber 202, the carbonization chamber 203, the growth chamber 204, the buffer chamber 205 and the end chamber 206 are all provided with an inlet channel, an outlet channel and a transmission assembly 208, the transmission assembly 208 is communicated with the inlet channel and the outlet channel of each chamber, the tray 207 is placed on the transmission assembly 208, and the tray 207 can be conveyed among the chambers through the transmission assembly 208. In some embodiments, the inlet and outlet ports are positioned with automatic control valves that can open and close the inlet and outlet ports to control the movement of the tray 207 into and out of the corresponding chambers. In some embodiments, the number of the trays 207 may be one or more, and if a plurality of trays 207 on which the substrates are placed on the driving assembly 208, a pipelined batch transfer of the trays 207 between the chambers and growth of a composite crystal comprising the substrates and the silicon carbide crystal can be achieved.
FIG. 9 is a schematic flow chart of an exemplary method for preparing a silicon carbide crystal according to some embodiments.
In some embodiments, the silicon carbide crystal production process 900 can be performed by a control apparatus (e.g., control module 101). For example, the process 900 may be stored in a storage device in the form of a program or instructions that, when executed by the control module 101, may implement the process 900. In some embodiments, process 900 may utilize one or more additional operations not described below, and/or be accomplished without one or more of the operations discussed below. Additionally, the order of the operations shown in FIG. 9 is not limiting.
In some embodiments, the silicon carbide crystal production process may be performed in a multi-chamber growth apparatus (e.g., multi-chamber growth apparatus 200, multi-chamber growth apparatus 300) comprising a plurality of chambers arranged in series, as can be seen in FIGS. 2A-2B, 3A-3B. In some embodiments, the silicon carbide crystal production process may be performed in a single chamber or a single reaction chamber having all the functions associated with a multi-chamber growth apparatus (e.g., evacuation, heating, purging of displaced gas, etc.), i.e., the various steps in the silicon carbide crystal production process (e.g., vacuum treatment process, in-situ etching treatment process, carbonization treatment process, crystal growth process, cooling process, etc.) may be performed in the same reaction chamber. Silicon carbide crystal preparation process 900 includes:
at step 910, the substrate is sequentially transferred and processed between the plurality of chambers. In some embodiments, this step 910 may be performed by the control module 101.
The substrate is provided withSingle crystal wafers having crystal planes and appropriate electrical, optical, and mechanical properties can be used to grow epitaxial layers (e.g., target crystals) that serve to support and improve the target crystal properties. The following conditions can be taken into account in the selection of the substrate: structural characteristics (a target crystal and a substrate have the same or similar lattice structures, small lattice constant mismatch degree and good crystallization performance), interface characteristics (growth of the target crystal is facilitated, adhesion is strong), chemical stability (the target crystal is not easy to decompose and corrode in the temperature and atmosphere for growth), thermal properties (good thermal conductivity and small thermal mismatch degree), good electrical conductivity, good optical properties (little absorption of light), good mechanical properties (easy processing such as polishing and cutting) and size (the diameter is not less than 2 inches). In some embodiments, the material of the substrate may comprise sapphire (Al)2O3) Silicon (Si), silicon carbide (SiC), gallium arsenide (GaAs), aluminum nitride (AIN), zinc oxide (ZnO).
In some embodiments, the substrate may comprise monocrystalline silicon. The monocrystalline silicon is photovoltaic monocrystalline silicon. In some embodiments, the single crystal silicon purity is greater than 99.9999%. In some embodiments, the single crystal silicon purity is greater than 99.99999%. In some embodiments, the single crystal silicon purity is greater than 99.999999%. In some embodiments, the single crystal silicon purity is greater than 99.9999999%. In some embodiments, the dimension of the substrate in one direction (referred to as the X-direction) may be smaller than the dimension of a cross-section in another direction perpendicular to the X-direction. In some embodiments, the cross-sectional shape of the substrate perpendicular to the X-direction may be circular, elliptical, polygonal, regular, or irregular. In some embodiments, the cross-sectional shape of the substrate perpendicular to the X-direction is circular, and the size of the cross-section of the substrate perpendicular to the X-direction can be set according to actual production needs. The dimension of the cross-section of the substrate perpendicular to the X-direction may be the linear distance of the two points on the edge of the substrate that are furthest apart. In some embodiments, the substrate has a circular cross-sectional shape perpendicular to the X-direction, the diameter of the circle comprising 1-10 inches. In some embodiments, the diameter of the circle comprises 1.5-8 inches. In some embodiments, the diameter of the circle comprises 2-6 inches. In some embodiments, the diameter of the circle comprises 3-5 inches. In some embodiments, the diameter of the circle comprises 3-4 inches. The size of the cross section of the substrate perpendicular to the X direction can be selected according to the size of the target crystal to be actually produced, for example, if it is desired to produce a target crystal having a larger size of the cross section perpendicular to the X direction, a larger size of the cross section perpendicular to the X direction can be selected. The dimension in the X direction may be referred to as the thickness of the substrate. In some embodiments, the thickness of the substrate is the same in different regions. The same thickness may be such that the difference in thickness between the areas of maximum thickness and minimum thickness on the substrate is less than a thickness threshold (e.g., 10um or 15 um). The flat substrates with the same thickness can ensure that the stress is uniform in the crystal growth process, and crystals with consistent crystal forms are formed. In some embodiments, the substrate has a thickness of 100um-400 um. In some embodiments, the substrate has a thickness of 160um-300 um. In some embodiments, the thickness of the substrate may be 180um-280 um. In some embodiments, the substrate may have a thickness of 200um-260 um. In some embodiments, the substrate may be 220um-240um thick. The thickness of the substrate is similar to that of a mass-produced photovoltaic single crystal wafer, the substrate is easy to obtain, and the substrate is thin and low in cost.
In some embodiments, the multi-chamber growth apparatus comprises at least an in-situ etching chamber, a carbonization chamber, a growth chamber, a buffer chamber, and a transmission assembly, wherein the in-situ etching chamber, the carbonization chamber, the growth chamber, and the buffer chamber are arranged in sequence. In some embodiments, a multi-chamber growth apparatus may include a vacuum chamber, an in-situ etch chamber, a carbonization chamber, a growth chamber, a buffer chamber, a tip chamber, and a drive assembly, the in-situ etch chamber, the carbonization chamber, the growth chamber, the buffer chamber, and the tip chamber being arranged in sequence. In some embodiments, each chamber defines an inlet channel and an outlet channel, and the substrate can be transferred between the chambers by a transfer assembly (e.g., transfer assembly 208). For more on the multi-chamber device, reference may be made to the contents of fig. 2A-2B, 3A-3B.
In some embodiments, the substrate may be sequentially transferred and processed between the plurality of chambers to perform different processes on the substrate or the composite crystal, respectively. For example, the substrate or the composite crystal is subjected to in-situ etching, carbonization, crystal growth, buffer treatment, cooling, and the like. Further details regarding the transfer and processing of substrates between multiple chambers in sequence can be found in the description of fig. 11.
In some embodiments, multiple substrates (or referred to as a group or batch of substrates) may be transported simultaneously in a multi-chamber apparatus for crystal growth to enable mass production of a combined crystal. In some embodiments, multiple groups or batches of substrates may be transported in sequence in a multi-chamber apparatus for crystal growth to enable continuous flow-line production of a composite crystal. In some embodiments, before at least one group or batch of substrates is transferred and processed between the plurality of chambers in sequence, another batch of at least one substrate is started to be transferred and processed between the plurality of chambers, and the two batches of at least one substrate are simultaneously transferred and processed in different chambers respectively.
And 920, growing a target crystal on the surface of the substrate in one of the cavities through vapor deposition to obtain a combined crystal containing the substrate and the target crystal. In some embodiments, this step 920 may be performed by the control module 101.
In some embodiments, one of the cavities in the multi-cavity growth apparatus may be a growth cavity. In some embodiments, a target crystal growth process is performed by vapor deposition on a surface of a substrate in a growth chamber to produce a composite crystal comprising the substrate and the target crystal. Vapor deposition introduces vapor or other gases required for reaction, containing gaseous, liquid reactants that form the film elements, into a reaction environment, chemically reacts at the substrate surface, and deposits the solid product onto the substrate surface to form a film.
In some embodiments, the target crystal may include a silicon carbide crystal, a silicon nitride crystal, a molybdenum disulfide crystal, a boron nitride crystal, a graphene crystal, or the like. The process of producing a composite crystal will be described below mainly by taking a silicon carbide crystal as an example, and it should be noted that the target crystal in this specification is not limited to a silicon carbide crystal, and may be any composite crystal that can be produced by a vapor deposition method.
In some embodiments, the reactants to prepare the composite crystal may include a silicon source and a carbon source. In some embodiments, the silicon source may include Silane (SiH)4) Chlorosilane, trimethylchlorosilane. In some embodiments, the carbon source may include propane (C)3H8) Butane, ethane, acetylene. In some embodiments, silane and propane may be passed into the growth chamber to perform a crystal growth process on the substrate surface. In some embodiments, a carrier gas may be used to carry the reactant gas into the growth chamber. The carrier gas does not participate in the reaction and only functions as a gas carrying the reactant, and therefore, an inert gas or a gas having high chemical stability can be selected. In some embodiments, the carrier gas may be H2、N2Ar or He. In some embodiments, the carrier gas may be H, taking into account cost and chemical stability considerations2、N2
In some embodiments, the substrate on the combined crystal can be removed by chemically etching the combined crystal to yield a silicon carbide crystal. Since the silicon carbide crystal has higher acid resistance or alkali resistance due to the difference in hardness between the silicon carbide crystal and the substrate, the substrate can be removed by dissolution with an acid solution or an alkali solution, while the silicon carbide crystal remains.
In some embodiments, the combined crystal can be ultrasonically cleaned with an etching solution for a first length of time at a first temperature interval to dissolve and remove the substrate to obtain a silicon carbide crystal. In some embodiments, the first temperature interval may be 50 ℃ to 100 ℃. In some embodiments, the first temperature interval may be 65 ℃ to 80 ℃. In some embodiments, the first temperature range may be 67-78 ℃. In some embodiments, the first temperature range may be 70 to 76 ℃. In some embodiments, the first temperature range may be 72-74 ℃. The etching speed can be accelerated by setting the first temperature interval to be 50-100 ℃.
In some embodiments, the etching solution may be an alkaline solution or an acidic solution. In some embodiments, the alkali solution may include a NaOH solution, a KOH solution, or NH4And (4) OH solution. In some embodimentsIn the method, the alkali solution can be 5 to 30 percent of NaOH solution. In some embodiments, the alkali solution may be a 10% to 25% NaOH solution. In some embodiments, the alkali solution may be a 15% to 20% NaOH solution. In some embodiments, the alkali solution may be a 10% to 25% NaOH solution. In some embodiments, the alkali solution may be a 12% to 23% NaOH solution. In some embodiments, the alkali solution may be a 14% to 21% NaOH solution. In some embodiments, the alkali solution may be a 16% to 18% NaOH solution. In some embodiments, the acid solution may include a hydrochloric acid solution, a dilute sulfuric acid solution, a nitric acid solution, hydrofluoric acid, or a hypochlorous acid solution. In some embodiments, the purity of the above-described alkali or acid solution may not be limited. For example, the alkali solution and the acid solution may be recovered from other processes (e.g., photovoltaic or semiconductor device production processes), and may be recycled, cost-effective, and environmentally friendly.
In some embodiments, the first length of time is directly related to the thickness of the substrate, the thicker the substrate, the longer the first length of time required to etch away the substrate. In some embodiments, the first time period may be at least 40 minutes. In some embodiments, the first duration may be 40 to 90 minutes. In some embodiments, the first duration may be 50 to 80 minutes. In some embodiments, the first duration may be 55 to 75 minutes. In some embodiments, the first duration may be 60 to 70 minutes. In some embodiments, the first duration may be 63-68 minutes. And by setting the ultrasonic cleaning time to be 40-90 minutes, the substrate on the combined crystal can be fully etched and removed, and the silicon carbide crystal without the substrate is obtained. In some embodiments, whether the substrate is etched is determined by human eye observation or composition detection. The quality of a silicon carbide crystal can be characterized by the basal plane dislocation density (number of defects per unit area). The contents regarding the basal plane dislocation density can be referred to the description of fig. 1.
In some embodiments, the silicon carbide crystal from which the substrate was removed may be cleaned. In some embodiments, the substrate-free silicon carbide crystal can be cleaned using a cleaning fluid (e.g., isopropyl alcohol or deionized water) at 50 ℃ to 80 ℃ and ultrasonically for a period of time (e.g., 3 to 10 minutes). The silicon carbide crystal with a clean surface can be obtained by cleaning the silicon carbide crystal.
FIG. 10 is an exemplary flow diagram of a substrate surface treatment process according to some embodiments. In some embodiments, the surface of the substrate may also be cleaned and planarized before the substrate is sequentially transferred and processed between the plurality of chambers, so that the surface of the substrate, particularly the surface on which the crystal grows, remains clean and flat.
In some embodiments, the substrate surface treatment process 1000 may be performed by a control device (e.g., the control module 101). For example, the process 1000 may be stored in a storage device in the form of a program or instructions that, when executed by the control module 101, may implement the process 1000. In some embodiments, process 1000 may utilize one or more additional operations not described below, and/or be accomplished without one or more of the operations discussed below. Additionally, the order of the operations shown in FIG. 10 is not limiting.
Step 1010, polishing the surface of the substrate. In some embodiments, this step 1010 may be performed by the polishing module 104.
In some embodiments, the substrate is placed on a polishing apparatus (e.g., polisher) for polishing. In some embodiments, the back side of the substrate (opposite the crystal growth side) may be polished first, followed by a fine polishing of the front side of the substrate (the crystal growth side). In some embodiments, the front side of the substrate (the crystal growth surface) may be finely polished. In some embodiments, the backside of the substrate (opposite the crystal growth face) may be polished. By polishing the back surface of the substrate, cutting scratches and defects on the back surface of the substrate are removed, so that the substrate can be flat, and the levelness of the crystal growth surface can be maintained in the substrate conveying process. The front surface (crystal growth surface) of the substrate is finely polished to make the surface smooth, so that reaction products can be uniformly crystallized on the crystal growth surface when the crystal grows.
In some embodiments, the polished substrate may be dried. For example, the respective surfaces of the substrate are blow-dried with nitrogen or helium.
At step 1020, a cleaning process is performed on the surface of the substrate. In some embodiments, this step 1010 may be performed by the cleaning module 105.
In some embodiments, a cleaning device (e.g., an ultrasonic cleaning apparatus) may be used to perform a cleaning process on the surface of the substrate to remove residues generated during the polishing process. In some embodiments, the surface of the substrate may be cleaned at least once with at least one cleaning fluid. In some embodiments, the surface of the substrate may be ultrasonically cleaned once with acetone, alcohol, and deionized water, respectively, in sequence. In some embodiments, the one-time washing time period may be at least 5 minutes. In some embodiments, the one-time washing time period may be 5 to 30 minutes. In some embodiments, the one-time washing time period may be 10-20 minutes. In some embodiments, the one-time washing time period may be 15-18 minutes. In some embodiments, the cleaned substrate may be dried. For example, after the substrate cleaning is completed, the respective surfaces of the substrate are blow-dried with nitrogen or helium.
In some embodiments, after the substrate surface is polished and cleaned, the substrate may be further cleaned. In some embodiments, the substrate after the polishing process and the cleaning process may be immersed in a strong acid solution for a certain period of time, and then subjected to a further cleaning process. In some embodiments, the strong acid solution may include hydrochloric acid, sulfuric acid, a nitric acid solution, hydrofluoric acid, or a hypochlorous acid solution. In some embodiments, the strong acid solution may comprise a 30% -40% hydrofluoric acid (HF) solution. In some embodiments, the substrate may be immersed in the diluted acid solution after the strong acid solution is diluted, so as to prevent the substrate from being damaged due to the excessive concentration of the acid solution. In some embodiments, the 30% -40% HF solution may be diluted to 1% HF solution, and the substrate may be soaked in the 1% -3% HF solution for a certain period of time, and then further cleaned with an ultrasonic cleaning device. In some embodiments, the single crystal silicon substrate may be soaked in a 1% -3% HF solution for 5-8 minutes and then further ultrasonically cleaned with deionized water for 5-10 minutes. In some embodiments, the substrate after the further cleaning process may be dried. For example, the substrate after further cleaning is blow dried on its respective surface with nitrogen or helium.
FIG. 11 is a schematic flow diagram illustrating the transfer and processing of substrates between chambers according to some embodiments.
In some embodiments, the transfer and processing process 1100 may be performed by a control device (e.g., control module 101) between chambers. For example, the process 1100 may be stored in a storage device in the form of a program or instructions that, when executed by the control module 101, may implement the process 1100. In some embodiments, process 1100 may utilize one or more additional operations not described below, and/or be accomplished without one or more of the operations discussed below. In addition, the order of the operations shown in fig. 11 is not limiting.
For more on the multi-chamber growing apparatus, reference may be made to the contents of FIGS. 2A-2B, 3A-3B and 9. The process 1100 of transferring and processing substrates between chambers includes:
step 1110, perform an in-situ etch process on the substrate in the in-situ etch chamber.
In some embodiments, at least one substrate may be subjected to an in situ etch process. For example, one or more substrates may be placed on a tray and transferred to an in-situ etch chamber for an in-situ etch process. In some embodiments, the substrate may be subjected to an in situ etch process under reactive conditions of a gas pressure, a temperature, and a process gas. In some embodiments, the pressure of the in-situ etch chamber may be maintained at a second pressure interval and the temperature at a second temperature interval for a second time period; and then introducing hydrogen to the in-situ etching cavity to be at normal pressure, and keeping the temperature of the in-situ etching cavity within a third time range to carry out in-situ etching treatment on the substrate within a third temperature interval. For more on-site processing of the substrate, reference may be made to the description of FIG. 13.
The defects of the crystal growth surface of the substrate can be removed by carrying out in-situ etching treatment on the substrate, so that the silicon carbide crystals with consistent crystal forms and high quality can be conveniently grown on the surface of the substrate.
At step 1120, the substrate is transferred from the in situ etch chamber to the carbonization chamber via the transfer assembly for carbonization.
The substrate after the in-situ etching treatment can be further carbonized. In some embodiments, the substrate may be transferred from the in situ etch chamber to the carbonization chamber via a transfer assembly (e.g., transfer assembly 208) for carbonization. In some embodiments, the substrate may be carbonized under reaction conditions of a certain gas pressure, a certain temperature, and a process gas. In some embodiments, the pressure of the carbonization chamber may be maintained in the third pressure interval for the fourth time period, and the temperatures of the temperature in-situ etching chamber are equal or similar (the temperature difference is less than or equal to 5 ℃); then, a third channel between the in-situ etching cavity and the carbonization cavity is controlled to be opened, the substrate is conveyed into the carbonization cavity through the transmission assembly 208, and the third channel is closed; and then, cooling the carbonization cavity to a fifth temperature interval, vacuumizing to a fourth pressure interval, gradually heating the carbonization cavity to the fourth temperature interval, and introducing carbonization gas (such as methane, propane, butane and the like) and hydrogen to a third pressure for carbonization treatment. For more on the carbonization of the substrate, reference is made to the description of fig. 14.
By carbonizing the substrate, the carbonized buffer layer can be prepared on the crystal growth surface of the substrate, which is beneficial to the crystallization of the silicon carbide crystal on the surface of the substrate.
At step 1130, the substrate is transferred from the carbonization chamber to the growth chamber via the drive assembly for vapor deposition, resulting in a composite crystal.
And growing the silicon carbide crystal on the crystal growth surface of the substrate after the carbonization treatment. In some embodiments, the substrate may be transferred from the carbonization chamber into the growth chamber by a drive assembly (e.g., drive assembly 208). In some embodiments, the growth chamber may be warmed to a fourth temperature interval and pressurized to a third pressure interval; a fourth passage between the carbonization chamber and the growth chamber is then controlled to open, and the substrate is transferred into the growth chamber via the transfer assembly 208, closing the fourth passage. Further reference may be made to the description of fig. 15 with respect to the transfer of the substrate from the carbonization chamber into the growth chamber.
In some embodiments, crystal growth is performed by vapor deposition on a crystal growth face of a substrate in a growth chamber to produce a composite crystal comprising the substrate and the silicon carbide crystal. In some embodiments, the growth chamber is heated to a sixth temperature interval, and silane, propane and hydrogen are introduced to a fifth pressure interval for crystal growth; and stopping the crystal growth when the target crystal growth thickness reaches the target thickness. Further details regarding crystal growth in the growth chamber can be found in the description of fig. 16.
And step 1140, transferring the combined crystal from the growth cavity to a buffer cavity through a transmission assembly, and cooling.
The grown composite crystal can be further cooled. In some embodiments, the composite crystal may be transferred from the growth chamber to a buffer chamber via the drive assembly 208, where it is cooled. In some embodiments, the buffer cavity is heated to a sixth temperature interval, a fifth channel between the growth cavity and the buffer cavity is controlled to be opened, the combined crystal is conveyed into the buffer cavity through the transmission assembly 208, and the fifth channel is closed; and then gradually cooling the buffer cavity to a seventh temperature interval, and keeping for a fifth time. For more cooling in the buffer chamber, reference may be made to the description of fig. 17.
FIG. 12 is an exemplary flow diagram of a vacuum process according to some embodiments. In some embodiments, the substrate may be vacuum processed prior to the in situ etch process.
In some embodiments, the vacuum process 1200 may be performed by a control device (e.g., the control module 101). For example, the process 1200 may be stored in a storage device in the form of a program or instructions that, when executed by the control module 101, may implement the process 1200. In some embodiments, process 1200 may utilize one or more additional operations not described below, and/or be accomplished without one or more of the operations discussed below. In addition, the order of the operations shown in fig. 12 is not limiting.
In some embodiments, the substrate may be vacuum processed in a vacuum chamber. For more on the vacuum chamber, reference may be made to the contents of fig. 3A-3B. The process 1200 of vacuum processing a substrate includes:
at step 1210, a substrate is placed in a vacuum chamber.
In some embodiments, the substrate after the polishing process and the cleaning process may be subjected to a vacuum process. In some embodiments, the substrate may be manually placed in the vacuum chamber, or the substrate may be manually placed on the drive assembly 208 and transferred into the vacuum chamber by the drive assembly 208. In other embodiments, the substrate may be placed in the vacuum chamber by a robot 111 (e.g., a robot), or the substrate may be placed on the transfer assembly 208 by the robot 111 and transferred into the vacuum chamber by the transfer assembly 208. In some embodiments, one or more substrates may be placed in a vacuum chamber. In some embodiments, multiple sets of substrates may be placed in a vacuum chamber in succession.
Step 1220, close the first channel of the vacuum chamber, and adjust the pressure of the vacuum chamber and the in-situ etching chamber to a first pressure range.
In some embodiments, the first channel is an inlet channel (e.g., inlet channel 401) of the vacuum chamber. In some embodiments, the substrate may be transferred to the in-situ etch chamber after adjusting the pressure of the in-situ etch chamber to be equal to or similar to the vacuum chamber (by a difference of no more than 5 Pa). In some embodiments, after the substrate is placed in the vacuum chamber, the first channel of the vacuum chamber is closed, and the vacuum chamber and the in-situ etching chamber are respectively evacuated to a first pressure interval. In some embodiments, the first pressure interval may be 3 to 15 Pa. In some embodiments, the first pressure interval may be 5 to 10 Pa. In some embodiments, the first pressure interval may be 6 to 9 Pa. In some embodiments, the first pressure interval may be 7 to 8 Pa. The pressure of the vacuum cavity and the pressure of the in-situ etching cavity are adjusted to be the first pressure interval, so that the pressure difference between the vacuum cavity and the in-situ etching cavity can be reduced, and the substrate is in a relatively stable environment.
In some embodiments, the vacuum chamber and the in-situ etch chamber may be evacuated simultaneously. In some embodiments, the evacuation lines (e.g., evacuation line 403 and evacuation line 503) of the vacuum chamber and the in-situ etching chamber are connected and then communicated to an evacuation device, and the operation speed and time of the evacuation device are controlled to perform evacuation. In some embodiments, the vacuum chamber and the in-situ etch chamber may be separately evacuated and the pressure monitored in real time. In some embodiments, the pumping pipelines of the vacuum chamber and the in-situ etching chamber are respectively communicated to a plurality of vacuum pumping devices, the running speed and time of the vacuum pumping devices are controlled, the vacuum chamber and the in-situ etching chamber are respectively pumped vacuum, and the pressure is monitored in real time. In some embodiments, the evacuation may be performed using a combination of mechanical and molecular pumps. In some embodiments, the vacuum chamber and/or the in-situ etching chamber may be pumped to a certain vacuum degree by the mechanical pump, and then continuously pumped to the first pressure range by the molecular pump.
At step 1230, the transfer assembly transfers the substrate to the in-situ etch chamber through a second passage between the vacuum chamber and the in-situ etch chamber.
In some embodiments, the substrate may be transferred into the in-situ etch chamber when the pressures within the vacuum chamber and the in-situ etch chamber are equal or similar and a first pressure interval is reached. In some embodiments, the control module 101 can control the second passage between the vacuum chamber and the in-situ etch chamber to open, activate the transfer assembly 208 to transfer the substrate to a particular location in the in-situ etch chamber, close the second passage, and deactivate the transfer assembly 208. The second channel is a channel adjacent to the vacuum chamber and the in-situ etch chamber, and may be, for example, an inlet channel 501 of the in-situ etch chamber or an outlet channel 402 of the vacuum chamber. In some embodiments, the inlet channel 501 of the in-situ etch chamber and the outlet channel 402 of the vacuum chamber are the same channel. In some embodiments, the particular location in the in-situ etch chamber may be a bottom central region of the in-situ etch chamber. In some embodiments, the position of the substrate may be detected by the detection module 102 (e.g., a sensor). In some embodiments, when the detection module 102 detects that the substrate is in the bottom center region of the in-situ etch chamber, the position information of the substrate can be sent to the control module 101, and the control module 101 can control the mechanical structure 111 (e.g., the transmission assembly 208) to stop operating.
FIG. 13 is an exemplary flow diagram of an in-situ etch process according to some embodiments.
In some embodiments, the in-situ etch process 1300 may be performed by a control device (e.g., control module 101). For example, the process 1300 may be stored in a storage device in the form of a program or instructions that, when executed by the control module 101, may implement the process 1300. In some embodiments, process 1300 may utilize one or more additional operations not described below, and/or be accomplished without one or more of the operations discussed below. In addition, the order of the operations shown in fig. 13 is not limiting.
In some embodiments, the substrate may be subjected to an in-situ etch process in an in-situ etch chamber. For more details regarding the in-situ etch chamber, reference may be made to the contents of FIGS. 2A-2B and 3A-3B. The process 1300 of performing an in-situ etch process on a substrate includes:
step 1310, the pressure of the in-situ etch chamber is maintained at a second pressure interval and the temperature is maintained at a second temperature interval for a second duration.
In some embodiments, the substrate may be subjected to an in situ etch process by passing hydrogen gas under the first condition. In some embodiments, the first condition may include maintaining the pressure at a second pressure interval and the temperature at a second temperature interval over a second time period. In some embodiments, the second pressure interval is a pressure of less than 5 x 10-3Pa, in the range of Pa. In some embodiments, the second pressure interval is a pressure of less than 1 × 10-3Pa, in the range of Pa. In some embodiments, the second pressure interval may be a pressure of less than 0.8 x 10-3Pa, in the range of Pa. In some embodiments, the second pressureThe interval may be a pressure of less than 0.5X 10-3Pa, in the range of Pa. In some embodiments, the second pressure interval may be a pressure of less than 1 x 10-4Pa, in the range of Pa. In some embodiments, the second pressure interval is a pressure of less than 1 × 10-5Pa, in the range of Pa. By setting the pressure of the in-situ etching chamber to be less than 5 x 10-3And in the range of Pa, the desorption of the gas generated in the in-situ etching treatment process from the surface of the substrate is facilitated, and the desorption effect is better.
In order to remove the gas in the in-situ etching chamber as much as possible without damaging the substrate, the second temperature should be selected to be within a proper temperature range. For example, nitrogen or oxygen is adsorbed on the surface of the substrate, and the desorption of the gas is not favored when the temperature is too low, and the substrate is easily nitrided or oxidized when the temperature is too high. In some embodiments, the second temperature interval may comprise 400-900 ℃. In some embodiments, the second temperature interval may comprise 500 to 800 ℃. In some embodiments, the second temperature interval may comprise 550 to 750 ℃. In some embodiments, the second temperature interval may comprise 600 to 700 ℃. In some embodiments, the second temperature interval may comprise 630 to 680 ℃. In some embodiments, the in-situ etch chamber can be temperature regulated by heater 505. For more on heating body 505, reference may be made to the description of fig. 5.
In some embodiments, the second period of time may be at least 10 minutes. In some embodiments, the second period of time may be 10-90 minutes. In some embodiments, the second period of time may be 20 to 80 minutes. In some embodiments, the second period of time may be 25 to 75 minutes. In some embodiments, the second period of time may be 30-70 minutes. In some embodiments, the second period of time may be 40-60 minutes. By keeping the second temperature interval for 10-90 minutes, the temperature in the in-situ etching cavity can be kept stable, and the substrate can be uniformly and effectively etched in the follow-up process.
In some embodiments, after transferring the substrate to the in-situ etching chamber, the control module 101 may control the vacuum pumping device to pump vacuum into the in-situ etching chamber so that the pressure in the in-situ etching chamber reaches a second pressure interval, and slowly raise the temperature to a second temperature interval for a second duration to sufficiently exhaust the gas in the in-situ etching chamber.
And 1320, introducing hydrogen to normal pressure, and keeping the temperature of the in-situ etching cavity within the third time range to perform in-situ etching treatment within the third temperature interval.
In some embodiments, the third temperature interval may comprise 900 to 1300 ℃. In some embodiments, the third temperature interval may comprise 1000 to 1200 ℃. In some embodiments, the third temperature interval may include 1050-1150 ℃. In some embodiments, the third temperature interval may comprise 1080-1130 ℃. By setting the temperature of the in-situ etching cavity to be in the third temperature interval, the hydrogen can react with the oxide attached to the surface of the substrate, and the oxide is reduced to complete the in-situ etching treatment.
In some embodiments, the third period of time may be at least 0.5 minutes. In some embodiments, the third period of time may be 0.5 to 5 minutes. In some embodiments, the third period of time may be 1-3 minutes. In some embodiments, the third period of time may be 1.5 to 2.8 minutes. In some embodiments, the third period of time may be 1.8 to 2.5 minutes. In some embodiments, the third duration may be 2 minutes. The substrate can be fully etched by etching at the third temperature interval for the third time period at the normal pressure.
In some embodiments, after exhausting the gas in the in-situ etching chamber, the control module 101 may control the introduction of hydrogen gas into the in-situ etching chamber for the in-situ etching process. In some embodiments, the control module 101 may control a valve on the gas inlet pipe 504 to open and introduce hydrogen into the in-situ etching chamber to normal pressure, and then control the heating body 505 to heat, so that the temperature in the in-situ etching chamber rises to a third temperature interval and is maintained for a third time period, and perform in-situ etching on the crystal growth surface of the substrate to remove defects of the crystal growth surface.
Fig. 14 is an exemplary flow diagram of a carbonization process according to some embodiments. In some embodiments, the in-situ etched substrate may be transferred to a carbonization chamber and the crystal growth surface of the substrate may be carbonized to form a carbonized buffer layer at the crystal growth surface.
In some embodiments, the carbonization process 1400 may be performed by a control device (e.g., the control module 101). For example, the process 1400 may be stored in a storage device in the form of a program or instructions that, when executed by the control module 101, may implement the process 1400. In some embodiments, process 1400 may utilize one or more additional operations not described below, and/or be accomplished without one or more of the operations discussed below. In addition, the order of the operations shown in fig. 14 is not limiting. The carbonization process 1400 may include:
step 1410, adjusting the temperature of the carbonization chamber to a third temperature interval.
In some embodiments, the carbonization chamber may be warmed to a third temperature interval by a heating body within the carbonization chamber. For further details of the heating body and the third temperature interval, reference may be made to the description elsewhere. In some embodiments, the control module 101 may control the heating module 103 (e.g., a heater) to warm the carbonization chamber to a third temperature interval.
When the temperature of the carbonization cavity is increased to be equal to or close to the temperature of the in-situ etching cavity (the temperature difference is less than or equal to 5 ℃), the substrate is conveyed into the carbonization cavity, and the deformation or denaturation of the substrate caused by temperature shock is avoided.
At step 1420, the substrate is transferred into the carbonization chamber by the drive assembly.
In some embodiments, the substrate may be transferred into the carbonization chamber while the temperatures of both the in-situ etch chamber and the carbonization chamber are maintained within the third temperature interval. In some embodiments, the control module 101 can control a third channel between the in-situ etch chamber and the carbonization chamber to open, activate a drive assembly (e.g., drive assembly 208) to transport the substrate to a particular location in the carbonization chamber, close the third channel, and stop the drive assembly from operating. The third channel refers to a channel adjacent to the in-situ etch chamber and the carbonization chamber, for example, the third channel may be the outlet channel 502 of the in-situ etch chamber or the inlet channel 501 of the carbonization chamber. In some embodiments, the outlet channel 502 of the in-situ etch chamber and the inlet channel 501 of the carbonization chamber are the same channel. In some embodiments, the particular location in the carbonization cavity may be a bottom central region of the carbonization cavity. In some embodiments, the position of the substrate may be detected by the detection module 102 (e.g., a sensor). In some embodiments, when the sensor detects that the substrate is in the bottom center region of the in-situ etch chamber, the position information of the substrate can be sent to the control module 101, and the control module 101 can control the mechanical structure 111 (e.g., the drive assembly 208) to stop operating.
And 1430, adjusting the temperature of the carbonization cavity to a fifth temperature interval and the pressure to a fourth pressure interval, simultaneously introducing propane and hydrogen to a third pressure interval, keeping the pressure of the carbonization cavity as the third pressure interval in a fourth time period, and performing carbonization treatment at the temperature in the fourth temperature interval.
The temperature of the substrate is high (900-1300 ℃) after the substrate is subjected to in-situ etching treatment in the in-situ etching cavity, if the substrate is directly conveyed to the carbonization cavity, the substrate can directly react with carbonization treatment gas, and the pressure and gas components can be unstable, so that the temperature in the carbonization cavity can be reduced firstly, and the temperature is increased to the temperature required by carbonization treatment after the pressure and the gas components are stable. In some embodiments, the substrate may be carbonized by passing propane and hydrogen under the second condition. In some embodiments, the second condition may include the pressure being in a fourth pressure interval and the temperature being in a fifth temperature interval.
In some embodiments, the fifth temperature interval may be 700 to 1100 ℃. In some embodiments, the fifth temperature range may be 800 to 1000 ℃. In some embodiments, the fifth temperature interval may be 850-980 ℃. In some embodiments, the fifth temperature range may be 900 to 950 ℃. In some embodiments, the fourth pressure interval may be less than 5 x 10- 5Pa. In some embodiments, the fourth pressure interval may be less than 1 x 10-5Pa. In some embodiments, the fourth pressure interval may be less than 0.5 x 10-5Pa. In some embodiments, the fourth pressure interval may be less than 10-6Pa. After the substrate is transferred to the carbonization chamber, carbon is introducedThe temperature of the carbonization cavity is reduced to a fifth temperature range, and the carbonization cavity is vacuumized to a fourth pressure range, so that gas in the carbonization cavity can be further discharged.
In some embodiments, the third pressure interval may be 1 × 103~1×105Pa. In some embodiments, the third pressure interval may be 1 × 103-6×104Pa. In some embodiments, the third pressure interval may be 2 x 103-6×103Pa. In some embodiments, the fourth temperature range may be 1000 to 1500 ℃. In some embodiments, the fourth temperature interval may be 1100 to 1400 ℃. In some embodiments, the fourth temperature interval may be 1200-1350 ℃. In some embodiments, the fourth temperature interval may be 1250 to 1300 ℃. In some embodiments, the fourth duration may be at least 0.5 minutes. In some embodiments, the fourth time period may be 0.5 to 5 minutes. In some embodiments, the fourth time period may be 1-3 minutes. In some embodiments, the fourth time period may be 1.5 to 2.5 minutes. In some embodiments, the fourth time period may be 2 minutes. In some embodiments, propane (C)3H8) The flow rate of (C) is 3-25 sccm. In some embodiments, propane (C)3H8) The flow rate of (C) is 5-20 sccm. In some embodiments, propane (C)3H8) The flow rate of (C) is 7 to 18 sccm. In some embodiments, propane (C)3H8) The flow rate of (C) is 10-15 sccm. In some embodiments, the flow rate of hydrogen comprises 0.5 to 25L/min. In some embodiments, the flow rate of hydrogen comprises 1 to 20L/min. In some embodiments, the flow rate of hydrogen comprises 5 to 15L/min. In some embodiments, the flow rate of hydrogen comprises 7 to 12L/min.
In some embodiments, the control module 101 controls the carbonization chamber to cool to a fifth temperature interval, vacuumizes to a fourth pressure interval, and starts to heat, and simultaneously, the propane and the hydrogen are introduced until the pressure reaches a third pressure interval, and heats to the fourth temperature interval, and the carbonization process is performed at a constant temperature and a constant pressure for a fourth time.
Fig. 15 is a schematic flow diagram illustrating transfer of a substrate from a carbonization chamber to a growth chamber according to some embodiments. In some embodiments, the in-situ etched substrate may be transferred to a growth chamber to grow a silicon carbide crystal on a crystal growth surface of the substrate.
In some embodiments, the process 1500 of transferring the substrate from the carbonization chamber to the growth chamber can be performed by a control apparatus (e.g., control module 101). For example, the process 1500 may be stored in a storage device in the form of a program or instructions that, when executed by the control module 101, may implement the process 1500. In some embodiments, process 1500 may utilize one or more additional operations not described below, and/or be accomplished without one or more of the operations discussed below. In addition, the order of the operations shown in fig. 15 is not limiting. The process 1500 of transferring a substrate from a carbonization chamber to a growth chamber can include:
step 1510, adjusting the temperature of the growth chamber to a fourth temperature interval and the pressure to a third pressure interval.
In some embodiments, the growth chamber may be warmed to a fourth temperature interval by a heating body within the growth chamber. For further details of the heating body and the fourth temperature interval, reference may be made to the description elsewhere. In some embodiments, the control module 101 may control the heating module 103 (e.g., a heater) to warm the growth chamber to a fourth temperature interval. In some embodiments, the control module 101 may control the evacuation device to evacuate the growth chamber such that the pressure within the growth chamber is adjusted to a third pressure interval. For more on the third pressure interval, reference may be made to the description of fig. 14.
And when the temperature of the growth cavity is increased to be equal to or similar to that of the carbonization cavity (the temperature difference is less than or equal to 5 ℃) and the vacuum is pumped to be equal to or similar to the pressure (the pressure difference is not more than 10Pa), the substrate is conveyed into the growth cavity, so that the deformation or denaturation of the substrate caused by sudden temperature or pressure change is avoided.
At step 1520, a fourth channel between the carbonization chamber and the growth chamber is controlled to open, and the substrate is transferred into the growth chamber through the transfer assembly.
In some embodiments, the substrate may be transferred into the growth chamber when the growth chamber and the carbonization chamber both have a fourth temperature interval and a third pressure interval. In some embodiments, after the temperature of the growth chamber reaches the fourth temperature interval and the pressure reaches the third pressure interval, the control module 101 may control the fourth channel between the growth chamber and the carbonization chamber to open, activate the transfer assembly (e.g., the transfer assembly 208) to transfer the substrate to a specific location in the growth chamber, close the fourth channel, and stop the transfer assembly. The fourth channel refers to the channel where the growth chamber and the carbonization chamber are adjacent, for example, the fourth channel may be the outlet channel 502 of the carbonization chamber or the inlet channel 601 of the growth chamber. In some embodiments, the outlet channel 502 of the carbonization chamber and the inlet channel 601 of the growth chamber are the same channel. In some embodiments, the particular location in the growth chamber may be directly above the axis of rotation 606 at the bottom of the growth chamber.
In some embodiments, the position of the substrate may be detected by the detection module 102 (e.g., a positioner). The position information of the substrate may be sent to the control module 101 and the control module 101 may control the mechanical structure 111 (e.g., the drive assembly 208) to stop operating.
In some embodiments, when the positioner determines that the substrate is located at the preset position of the growth chamber, the position information of the substrate may be sent to the control module 101, and the control module 101 may control the mechanical structure 111 (e.g., the driving assembly 208) to stop driving. In some embodiments, the predetermined position of the growth chamber may be directly above the rotation axis 606. In some embodiments, the positioner may be disposed on the axis of rotation. In some embodiments, control module 101 can control rotation axis 606 to be raised to lift the substrate to the middle of the growth chamber. In some embodiments, the axis of rotation may rotate the substrate clockwise or counterclockwise. In some embodiments, the rotational speed of the rotating shaft may be adjustable.
FIG. 16 is an exemplary flow diagram of crystal growth according to some embodiments.
In some embodiments, vapor deposition may be performed at the crystal growth face of the substrate in a growth chamber to produce a composite crystal comprising the substrate and the silicon carbide crystal. For more on the growth chamber, see the contents of fig. 2A-2B, 3A-3B and 6.
In some embodiments, the crystal growth process 1600 may be performed by a control device (e.g., the control module 101). For example, the process 1600 may be stored in a storage device in the form of a program or instructions that, when executed by the control module 101, may implement the process 1600. In some embodiments, process 1600 may utilize one or more additional operations not described below, and/or be accomplished without one or more of the operations discussed below. In addition, the order of the operations shown in fig. 16 is not limiting. The crystal growth process 1600 may include:
step 1610, the growth cavity is heated to a sixth temperature interval, and the pressure is adjusted to a fourth pressure interval.
In some embodiments, the target crystal (e.g., a silicon carbide crystal) can be grown on the substrate by vapor deposition by passing silane, propane, and hydrogen gas under the third condition. In some embodiments, the third condition may include a pressure in a fourth pressure interval and a temperature in a sixth temperature interval. The sixth temperature zone differs depending on the type of crystal to be grown. In some embodiments, the sixth temperature interval may be 1300-1750 ℃. In some embodiments, the sixth temperature range may be 1400-1700 ℃. In some embodiments, the sixth temperature interval may be 1450 to 1650 ℃. In some embodiments, the sixth temperature range may be 1500-1600 ℃. In some embodiments, the sixth temperature range may be 1520 to 1570 ℃. In some embodiments, the sixth temperature interval may be constant throughout the growth process, or may be adjusted according to different stages of the crystal growth process.
In some embodiments, the control module 101 may control the heating module 103 (e.g., a heater in the growth chamber) to warm the growth chamber to a sixth temperature interval. For more on the heating body, reference may be made to the description elsewhere.
In some embodiments, the growth chamber may be evacuated to a fourth pressure interval by a vacuum device (e.g., a vacuum pump). More about the fourth pressure interval can be described in fig. 14.
Step 1620, introducing silane, propane and hydrogen to a fifth pressure interval for crystal growth.
The fifth pressure interval is different according to the type of the crystal to be grown, and for a specific crystal (such as silicon carbide crystal), the fifth pressure interval is too small, so that the crystal growth rate is low; and the fifth pressure is too high, and defects are easily formed during crystal growth. In some embodiments, the fifth pressure interval may be 20 to 100 Pa. In some embodiments, the fifth pressure interval may be 30 to 90 Pa. In some embodiments, the fifth pressure interval may be 40 to 80 Pa. In some embodiments, the fifth pressure interval may be 50 to 70 Pa. In some embodiments, the fifth pressure interval may be 55 to 65 Pa. In some embodiments, the fifth pressure interval may be constant throughout the growth process or may be adjusted for different stages of the crystal growth process.
In some embodiments, Silane (SiH) is introduced4) The flow rate of the gas comprises 300-800 sccm. In some embodiments, Silane (SiH) is introduced4) The flow rate of (2) comprises 400-600 sccm. In some embodiments, Silane (SiH) is introduced4) The flow rate of (A) is 450-550 sccm. In some embodiments, Silane (SiH) is introduced4) The flow rate of (2) comprises 480-520 sccm. In some embodiments, propane (C) is passed in3H8) The flow rate of (C) is 100 to 250 sccm. In some embodiments, propane (C) is passed in3H8) The flow rate of (2) includes 133-200 sccm. In some embodiments, propane (C) is passed in3H8) The flow rate of (C) is 150-180 sccm. In some embodiments, propane (C) is passed in3H8) The flow rate of (2) comprises 160-170 sccm. In some embodiments, hydrogen (H) is introduced2) The flow rate of (A) is 10-90L/min. In some embodiments, hydrogen (H) is introduced2) The flow rate of (A) is 20-80L/min. In some embodiments, hydrogen (H) is introduced2) The flow rate of (A) is 30-70L/min. In some embodiments, hydrogen (H) is introduced2) The flow rate of (A) is 40-60L/min.
In some embodiments, the control module 101 may control the flow rates of the silane, the propane, and the hydrogen gas into the growth chamber to make the pressure of the growth chamber be a fifth pressure interval. In the growth cavity, the substrate is subjected to crystal growth under the conditions of a sixth temperature interval, a fifth pressure interval and reactants (silane, propane and hydrogen).
Step 1630, stopping the crystal growth when the target crystal thickness reaches the target thickness.
In some embodiments, the target thickness may be 200-600 μm in some embodiments, the target thickness may be 300-500 μm. In some embodiments, the target thickness may be 320-480 μm. In some embodiments, the target thickness may be 350-450 μm. In some embodiments, the target thickness may be 380-420 μm. In some embodiments, the target thickness may be 390 to 410 μm. By setting the target thickness to be 200-600 mu m, the wafer with the specified thickness can be obtained directly by polishing without subsequent treatment such as cutting and the like, so that the production efficiency is improved, the processing cost is saved, and the industrial application is facilitated.
In some embodiments, the thickness of the crystal growth can be monitored during the crystal growth process, and the temperature, pressure and flow ratio of silane, propane and hydrogen of the growth chamber can be controlled according to the parameters of the speed, thickness and the like of the crystal growth. In some embodiments, the crystal growth thickness may be monitored using a reflective high-energy electron diffraction device (RHEED). In some embodiments, the temperature of the growth cavity can be adjusted by regulating the heating power of the heating body. In some embodiments, the silicon source and carbon source ratios in the reactants can be adjusted by adjusting the flow rates of silane and propane, respectively. In some embodiments, the pressure of the growth chamber can be adjusted by adjusting the flow rates of the silane, propane, and hydrogen gas.
In some embodiments, the control module 101 may control stopping crystal growth when the crystal grows to the target thickness. In some embodiments, the control module 101 may control to stop the feeding of silane, propane and hydrogen, and control to stop the heating body to heat the growth chamber.
FIG. 17 is an exemplary flow diagram of a buffering and cooling process according to some embodiments.
In some embodiments, a buffer chamber and a terminal chamber are provided adjacent to the growth chamber for subsequent operations after crystal growth is complete, such as cooling the resulting composite crystal. The combined crystal is transferred from the growth cavity to the buffer cavity through the transmission assembly, and is cooled to a certain temperature (for example, a seventh temperature interval); the combined crystal is then transferred into the end cavity to cool to room temperature. The combined crystal is cooled to a seventh temperature range (500-1200 ℃) in the buffer cavity by arranging the buffer cavity, and then the combined crystal is conveyed to the tail end cavity to be cooled to room temperature, so that the condition that the combined crystal is cracked due to sudden drop of environmental temperature (the combined crystal is directly conveyed from the growth cavity to the tail end cavity) is avoided.
In some embodiments, the buffering and cooling process 1700 may be performed by a control device (e.g., the control module 101). For example, the process 1700 may be stored in a storage device in the form of a program or instructions that, when executed by the control module 101, may implement the process 1700. In some embodiments, process 1700 may utilize one or more additional operations not described below, and/or be accomplished without one or more of the operations discussed below. In addition, the order of the operations shown in fig. 17 is not limiting.
Step 1710, adjusting the temperature of the buffer cavity to a sixth temperature interval.
In some embodiments, the buffer cavity may be heated to a sixth temperature interval by a heating body within the buffer cavity. In some embodiments, the control module 101 may control the heating module 103 (e.g., a heating body) to heat the buffer cavity to the sixth temperature interval. For more on the heating body and the sixth temperature interval, reference may be made to the description elsewhere.
When the buffer cavity is heated to be equal to or close to the temperature of the growth cavity (the temperature difference is less than or equal to 5 ℃), the temperature shock caused by overlarge temperature difference between the buffer cavity and the growth cavity is avoided, and thus the combined crystal is deformed or denatured.
At 1720, the assembled crystal is transferred to a buffer chamber via a transfer assembly.
In some embodiments, when the temperature of the buffer chamber reaches the sixth temperature interval, a fifth channel between the growth chamber and the buffer chamber may be opened, a drive assembly (e.g., drive assembly 208) may be activated to transport the composite crystal to a particular location in the buffer chamber, the fifth channel may be closed, and the drive assembly may be stopped. The fifth channel refers to a channel where the growth chamber and the buffer chamber are adjacent, for example, the fifth channel may be the outlet channel 602 of the growth chamber or the inlet channel 501 of the buffer chamber. In some embodiments, the outlet channel 602 of the growth chamber and the inlet channel 501 of the buffer chamber are the same channel. In some embodiments, the particular location in the buffer cavity may be a bottom central region of the buffer cavity. In some embodiments, the position of the substrate may be detected by the detection module 102 (e.g., a sensor). In some embodiments, when the sensor detects that the substrate is in the bottom center region of the buffer chamber, the position information of the substrate may be sent to the control module 101, and the control module 101 may control the mechanical structure 111 (e.g., the transmission assembly 208) to stop operating.
And step 1730, adjusting the temperature of the buffer cavity to a seventh temperature interval, and keeping the fifth time period for cooling.
In some embodiments, the seventh temperature range may be 500 to 1200 ℃. In some embodiments, the seventh temperature interval may be 550 to 1000 ℃. In some embodiments, the seventh temperature range may be 600 to 800 ℃. In some embodiments, the seventh temperature interval may be 650 to 750 ℃. In some embodiments, the seventh temperature range may be 680-720 ℃. In some embodiments, the fifth duration may be at least 1 h. In some embodiments, the fifth duration may be 1-7 h. In some embodiments, the fifth duration may be 2-6 h. In some embodiments, the fifth time period may be 2.5-5.5 hours. In some embodiments, the fifth duration may be 3-5 h. In some embodiments, the fifth time period may be 3.5-4.5 hours.
In some embodiments, the control module 101 may control the buffer cavity to gradually cool down to a seventh temperature interval. In some embodiments, the control module 101 may control the valve on the inlet pipe 504 to open and introduce a replacement gas (e.g., hydrogen, nitrogen, argon, or helium) into the buffer cavity through the inlet pipe 504; meanwhile, the vacuumizing equipment can be controlled to exhaust the buffer cavity so as to keep the pressure in the buffer cavity close to the normal pressure. In some embodiments, when the temperature of the buffer cavity is in the seventh temperature interval, the control module 101 may control the seventh temperature interval of the buffer cavity to be kept for a fifth time period, so that the temperature of the component or the combined crystal in the buffer cavity is stabilized in the seventh temperature interval.
The composite crystal is transferred into the end cavity by the drive assembly, step 1740.
In some embodiments, the combined crystal may be transferred into the end cavity for further cooling. In some embodiments, the temperature of the tip cavity may be room temperature. In some embodiments, the control module 101 can control the sixth channel between the buffer chamber and the end chamber to open, activate the drive assembly (e.g., drive assembly 208) to transport the composite crystal to a particular location in the end chamber, close the sixth channel, and stop the drive assembly from running. The sixth channel refers to a channel where the buffer cavity and the end cavity are adjacent, for example, the sixth channel may be the outlet channel 502 of the buffer cavity or the inlet channel 401 of the end cavity. In some embodiments, the outlet channel 502 of the buffer cavity and the inlet channel 401 of the tip cavity are the same channel. In some embodiments, the particular location in the buffer cavity may be a bottom center region or other designated region of the buffer cavity. In some embodiments, the position of the combined crystal may be detected by a detection module 102 (e.g., a sensor). In some embodiments, when the sensor detects that the composite crystal is in the bottom center region or other designated region of the end chamber, the position information of the composite crystal can be sent to the control module 101, and the control module 101 can control the mechanical structure 111 (e.g., the transmission assembly 208) to stop operating.
At step 1750, the combined crystals are cooled to room temperature.
The combined crystals may continue to cool to room temperature within the tip cavity. In some embodiments, the combined crystal can be cooled to room temperature after 8-12 hours of natural cooling in the end cavity. In some embodiments, a displacement gas may be introduced into the tip cavity to cool the composite crystal. In some embodiments, the end chamber is provided with an inlet pipe and an outlet pipe, and the control module 101 may control a valve on the inlet pipe to open and introduce a replacement gas (e.g., hydrogen, nitrogen, argon, or helium) into the end chamber through the inlet pipe; meanwhile, the vacuum pumping equipment can be controlled to pump air to the tail end cavity so as to keep the pressure in the tail end cavity close to the normal pressure.
In some embodiments, after the composite crystal has cooled to room temperature, the control module 101 can control the outlet channel 402 of the end chamber to open and deliver the composite crystal to the vicinity of the outlet channel 402 of the end chamber via the transmission assembly 208, either manually or by a robotic arm to remove the composite crystal. And after the combined crystal is taken out, the substrate on the combined crystal can be removed by chemical etching on the combined crystal, so that the silicon carbide crystal is obtained. Further details regarding chemical etching can be found in the description of fig. 9.
In some embodiments, the process 1700 may not include steps 1740 and 1750, i.e., without an end cavity, and the combined crystals are cooled down in the natural environment directly after being taken out of the buffer cavity.
The following is a specific embodiment of the present invention. The process for preparing a silicon carbide crystal by a multi-cavity growth apparatus may comprise the steps of:
(1) polishing treatment and cleaning treatment: polishing a round monocrystalline silicon wafer with a crystal growth surface of (111), a thickness of 100-400 mu m and a diameter of 1-10 inches on a polishing machine, and polishing the (11-1) surface to make the surface flat; then, the (111) surface is finely polished to remove surface cutting scratches and defects. The polished single crystal silicon wafer is ultrasonically cleaned for 10-20 minutes by cleaning solution (such as acetone, alcohol, deionized water), and then dried by high-purity nitrogen or helium. And then placing the monocrystalline silicon piece into 1% -3% HF solution to be soaked for 5-8 minutes, and then ultrasonically cleaning the monocrystalline silicon piece for 5-10 minutes by using deionized water. And drying the monocrystalline silicon wafer by using nitrogen or helium after cleaning.
(2) And (3) vacuum treatment: at least one single crystal silicon wafer is placed in a recessed position on a tray and fixed with the (111) side of the single crystal silicon wafer facing upward. Putting the tray into a vacuum cavity, and vacuumizing the vacuum cavity to 3-15 Pa. During this time, the in-situ etch chamber is evacuated to a pressure equal to or similar to the pressure in the vacuum chamber (the difference is no more than 5 Pa).
(3) In-situ etching treatment: and conveying the tray with the at least one monocrystalline silicon wafer into the in-situ etching chamber. Continuously vacuumizing the in-situ etching cavity to 5 multiplied by 10-3Heating to 900 ℃ below Pa slowly, keeping the temperature for 10-90min, and degassing at high temperature; and then introducing hydrogen into the in-situ etching cavity to normal pressure, heating to 1000-1200 ℃, keeping the normal pressure and preserving the heat for 1-3 minutes, and carrying out in-situ etching treatment to remove the defects of the crystal growth surface.
(4) Carbonizing treatment: and conveying the tray with at least one monocrystalline silicon wafer into a carbonization cavity, and carbonizing the crystal growth surface to prepare a carbonized buffer layer. Firstly, cooling the carbonization cavity to 800-; when the vacuum pressure is less than 1 x 10-5After Pa, the temperature is raised, and propane (C) of 5-20sccm is introduced into the carbonization cavity3H8) And 1-20L/min hydrogen to maintain the pressure in the carbonization chamber at 1X 103~6×104Pa. The temperature of the carbonization cavity is increased to 1100-. During this period, the temperature of the growth chamber was controlled to 1100-1400 ℃.
(5) Crystal growth: and conveying the tray with at least one monocrystalline silicon wafer into the growth cavity, and regulating the temperature of the growth cavity to 1400-1700 ℃. Introducing SiH of 400-600sccm into the growth cavity4133 + 200sccm C3H820-80L/min H2And keeping the pressure of the growth chamber at 30-90Pa, and performing crystal growth in the growth chamber. During this period, the temperature of the buffer chamber was controlled to 1400-1700 ℃. After growing for 10-12h in the growth cavity, the tray is transferred to the buffer cavity.
(6) Cooling: after the tray is conveyed to the buffer cavity, the buffer cavity is cooled to 500-1200 ℃ after 2-6 h. The tray was then transferred to the end chamber and cooled to room temperature over 8-12 h. The combined crystals were removed.
(7) Chemical etching treatment: and taking out the combined crystal, and performing ultrasonic cleaning by using 10-25% NaOH solution at 65-80 ℃ for rapid etching for 50-80 minutes to obtain the chemically etched silicon carbide crystal.
(8) Cleaning treatment: and putting the silicon carbide crystal into a cleaning solution (such as isopropanol), and ultrasonically cleaning for 3-10 minutes at the temperature of 50-80 ℃. And then ultrasonically cleaning the silicon carbide crystal by using deionized water for 3-10 minutes to obtain the silicon carbide crystal.
(9) And (3) testing: through tests, the thickness of the prepared silicon carbide crystal is 300-500 mu m, the wafer has no obvious warpage, and the surface is smooth.
It should be noted that the above description of the method for preparing silicon carbide crystals is merely for convenience of description and should not be construed as limiting the scope of the present disclosure to the examples. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the principles of the present disclosure. However, such changes and modifications do not depart from the scope of the present specification.
The beneficial effects that may be brought by the embodiments of the present description include, but are not limited to: (1) a multi-cavity growth device is adopted for crystal preparation, at least one substrate or combined crystal is conveyed among the cavities, and different technological treatment processes are independently carried out in each cavity, so that the mass production of the crystals in a production line is realized; (2) in the growth process, the thickness of the target crystal can be monitored, the target crystal with the target thickness is prepared, a single target wafer finished product can be obtained after chemical etching, cutting is not needed, the crystal preparation period is short, the processing cost is low, and the efficiency is high; (3) the monocrystalline silicon wafer is used as a substrate, the target crystal is prepared on the substrate by adopting a vapor deposition method to obtain the combined crystal, and the substrate can be removed by chemically etching the combined crystal by using acid liquor or alkali liquor used in other processes (such as a photovoltaic or semiconductor device production process), so that the production cost is saved, the resource recycling is realized, and the production mode is more environment-friendly.
It is to be noted that different embodiments may produce different advantages, and in different embodiments, any one or combination of the above advantages may be produced, or any other advantages may be obtained.
The foregoing describes the present specification and/or some other examples. Various modifications may be made in the present disclosure in light of the above teachings. The subject matter disclosed herein is capable of being implemented in various forms and examples, and of being applied to a wide variety of applications. All applications, modifications and variations that may be claimed in the following claims are within the scope of the present description.
Also, the description uses specific words to describe embodiments of the description. Reference throughout this specification to "one embodiment," "an embodiment," and/or "some embodiments" means that a particular feature, structure, or characteristic described in connection with at least one embodiment of the specification is included. Therefore, it is emphasized and should be appreciated that two or more references to "an embodiment," or "one embodiment," or "an alternative embodiment," or "another embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, some features, structures, or characteristics of one or more embodiments of the specification may be combined as appropriate.
Those skilled in the art will appreciate that various modifications and improvements may be made to the disclosure herein. For example, the different system components described above are implemented by hardware devices, but may also be implemented by software solutions only. For example: the system is installed on an existing server. Further, the location information disclosed herein may be provided via a firmware, firmware/software combination, firmware/hardware combination, or hardware/firmware/software combination.
All or a portion of the software may sometimes communicate over a network, such as the internet or other communication network. Such communication enables loading of software from one computer device or processor to another. For example: from a management server or host computer of the radiation therapy system to a hardware platform of a computer environment, or other computer environment implementing the system, or similar functionality associated with providing information needed to determine wheelchair target structural parameters. Thus, another medium capable of transferring software elements may also be used as a physical connection between local devices, such as optical, electrical, electromagnetic waves, etc., propagating through cables, optical cables, or the air. The physical medium used for the carrier wave, such as an electric, wireless or optical cable or the like, may also be considered as the medium carrying the software. As used herein, unless limited to a tangible "storage" medium, other terms referring to a computer or machine "readable medium" refer to media that participate in the execution of any instructions by a processor.
Computer program code required for the operation of various portions of this specification may be written in any one or more programming languages, including an object oriented programming language such as Java, Scala, Smalltalk, Eiffel, JADE, Emerald, C + +, C #, VB.NET, Python, and the like, a conventional programming language such as C, Visual Basic, Fortran 2003, Perl, COBOL 2002, PHP, ABAP, a dynamic programming language such as Python, Ruby, and Groovy, or other programming languages. The program code may execute entirely on the user's computer, partly on the user's computer, as a stand-alone software package, partly on the user's computer and partly on a remote computer or entirely on the remote computer or server. In the latter scenario, the remote computer may be connected to the user's computer through any network, such as a Local Area Network (LAN) or a Wide Area Network (WAN), or the connection may be made to an external computer (for example, through the Internet), or in a cloud computing environment, or as a service using, for example, software as a service (SaaS).
Additionally, the order in which the elements and sequences of the process are recited in the specification, the use of alphanumeric characters, or other designations, is not intended to limit the order in which the processes and methods of the specification occur, unless otherwise specified in the claims. While various presently contemplated embodiments of the invention have been discussed in the foregoing disclosure by way of example, it is to be understood that such detail is solely for that purpose and that the appended claims are not limited to the disclosed embodiments, but, on the contrary, are intended to cover all modifications and equivalent arrangements that are within the spirit and scope of the embodiments herein. For example, although the system components described above may be implemented by hardware devices, they may also be implemented by software-only solutions, such as installing the described system on an existing server or mobile device.
Similarly, it should be noted that in the preceding description of embodiments of the present specification, various features are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure aiding in the understanding of one or more of the embodiments. This method of disclosure, however, is not intended to imply that more features than are expressly recited in a claim. Indeed, the embodiments may be characterized as having less than all of the features of a single embodiment disclosed above.
Numbers describing attributes, quantities, etc. are used in some embodiments, it being understood that such numbers used in the description of the embodiments are modified in some instances by the use of the modifier "about", "approximately" or "substantially". Unless otherwise indicated, "about", "approximately" or "substantially" indicates that the number allows a variation of ± 20%. Accordingly, in some embodiments, the numerical parameters used in the specification and claims are approximations that may vary depending upon the desired properties of the individual embodiments. In some embodiments, the numerical parameter should take into account the specified significant digits and employ a general digit preserving approach. Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the range are approximations, in the specific examples, such numerical values are set forth as precisely as possible within the scope of the application.
For each patent, patent application publication, and other material, such as articles, books, specifications, publications, documents, articles, and the like, cited in this specification, the entire contents of each patent, patent application publication, and other material is specifically incorporated by reference into this specification. Except where the application history document does not conform to or conflict with the contents of the present specification, it is to be understood that the application history document, as used herein in the present specification or appended claims, is intended to define the broadest scope of the present specification (whether presently or later in the specification) rather than the broadest scope of the present specification. It is to be understood that the descriptions, definitions and/or uses of terms in the accompanying materials of this specification shall control if they are inconsistent or contrary to the descriptions and/or uses of terms in this specification.
Finally, it should be understood that the embodiments described herein are merely illustrative of the principles of the embodiments of the present disclosure. Other variations are also possible within the scope of the present description. Thus, by way of example, and not limitation, alternative configurations of the embodiments of the specification can be considered consistent with the teachings of the specification. Accordingly, the embodiments of the present description are not limited to the embodiments explicitly described and depicted herein.

Claims (21)

1. A method for preparing silicon carbide crystals is characterized in that the preparation method is carried out in a multi-cavity growing device, and the multi-cavity growing device comprises a plurality of cavities and a transmission assembly; the method comprises the following steps:
sequentially transferring and processing at least one substrate among a plurality of cavities, wherein the transmission assemblies in the cavities are sequentially connected end to end;
growing a silicon carbide crystal by vapor deposition in one of the plurality of cavities to obtain at least one combined crystal comprising the substrate and the silicon carbide crystal;
etching the combined crystal by using an etching solution in a first temperature range to obtain a basal plane dislocation density of 120-2000cm-2The silicon carbide crystal of (1), wherein different process treatments are independently performed in each chamber.
2. The method of claim 1, wherein the etching the composite crystal with an etching solution comprises:
using the etching solution toThe combined crystal is subjected to ultrasonic cleaning for a first time to obtain the basal plane dislocation density of 120-2000cm-2The silicon carbide crystal of (1).
3. The method of claim 1, wherein the plurality of cavities comprises at least: the in-situ etching chamber, the carbonization chamber, the growth chamber and the buffer chamber; and the transmission assembly sequentially processes at least one substrate through the in-situ etching cavity, the carbonization cavity, the growth cavity and the buffer cavity.
4. The method of claim 3, wherein the method further comprises:
before the at least one substrate is sequentially transferred and processed among the plurality of cavities, at least one substrate of another batch is started to be transferred and processed among the plurality of cavities, and at least one substrate of the two batches is simultaneously and respectively transferred and processed in different cavities.
5. The method of claim 3, wherein the plurality of cavities further comprises a vacuum cavity; the method comprises the following steps:
placing the at least one substrate in the vacuum chamber prior to processing the at least one substrate in the in-situ etch chamber;
adjusting the pressure of the vacuum cavity and the in-situ etching cavity to a first pressure interval;
the drive assembly conveys the at least one substrate to the in-situ etch chamber.
6. The method of claim 3, wherein processing the at least one substrate in the in-situ etch chamber comprises:
keeping the pressure of the in-situ etching cavity in a second pressure interval and the temperature in a second temperature interval within a second time length range;
and introducing hydrogen to the in-situ etching cavity to normal pressure, and keeping the temperature of the in-situ etching cavity within a third time range at a third temperature interval for in-situ etching treatment.
7. The method of claim 6, wherein processing the at least one substrate in the carbonization chamber comprises:
and keeping the pressure of the carbonization cavity in a third pressure interval within a fourth time period, and carrying out carbonization treatment at the fourth temperature interval.
8. The method of claim 7, wherein the carbonizing treatment comprises:
adjusting the temperature of the carbonization cavity to the third temperature interval;
transferring the at least one substrate into the carbonization chamber via the drive assembly,
adjusting the temperature of the carbonization cavity to a fifth temperature interval and the pressure to a fourth pressure interval, simultaneously introducing propane and hydrogen to a third pressure interval, keeping the pressure of the carbonization cavity as the third pressure interval within a fourth time period, and carrying out carbonization treatment at the temperature within the fourth temperature interval.
9. The method of claim 8, wherein processing the substrate in the growth chamber comprises:
keeping the temperature of the growth cavity in a sixth temperature interval and the pressure in a fourth pressure interval, introducing reaction raw materials, and adjusting the pressure in a fifth pressure interval to perform a crystal growth process.
10. The method of claim 9, wherein the crystal growth process comprises:
adjusting the temperature of the growth cavity to the fourth temperature interval and the pressure to the third pressure interval;
transferring the at least one substrate into the growth chamber by the transfer assembly,
adjusting the temperature of the growth cavity to a sixth temperature interval, wherein the pressure is the fourth pressure interval, and introducing silane, propane and hydrogen to a fifth pressure interval to perform crystal growth;
and stopping the crystal growth when the thickness of the silicon carbide crystal reaches the target thickness.
11. The method of claim 9, wherein the processing in the buffer cavity comprises:
and cooling within a seventh temperature interval of keeping the temperature of the buffer cavity within the fifth time.
12. The method of claim 11, wherein the plurality of cavities further comprises a tip cavity; the method further comprises the following steps:
maintaining the temperature of the end cavity at room temperature;
transferring the composite crystal into the end cavity through the transmission assembly;
the combined crystals were cooled to room temperature.
13. A multi-chamber growth apparatus for use in a crystal preparation process, the multi-chamber growth apparatus comprising:
etching the cavity in situ;
carbonizing the cavity;
a growth chamber for growing a silicon carbide crystal by vapor deposition, resulting in at least one composite crystal comprising a substrate and a silicon carbide crystal;
a buffer cavity;
a transmission assembly; the transmission assembly sequentially processes the at least one substrate through the in-situ etching cavity, the carbonization cavity, the growth cavity and the buffer cavity, wherein the transmission assemblies in the cavities are sequentially connected end to end, and different process treatment processes are independently performed in each cavity.
14. The multi-chamber growth apparatus of claim 13, wherein the multi-chamber growth apparatus further comprises a vacuum chamber.
15. The multi-lumen growth device of claim 13, further comprising a tip lumen.
16. A multi-chamber growth apparatus according to claim 13, wherein the drive assembly comprises at least two rotatable cylindrical rollers arranged in parallel, the rotatable cylindrical rollers being located side by side below each chamber.
17. The multi-chamber growth apparatus of claim 13, wherein the multi-chamber growth apparatus comprises a tray; the tray is provided with at least one groove, and the at least one groove is used for placing at least one substrate.
18. A multi-chamber growth apparatus according to claim 17, wherein the growth chamber comprises a rotating shaft.
19. The multi-chamber growth apparatus of claim 13, wherein the in-situ etch chamber, the carbonization chamber, and the growth chamber each comprise at least one gas inlet conduit therein.
20. The multi-chamber growth apparatus of claim 14, wherein the vacuum chamber, the in-situ etch chamber, the carbonization chamber, and the growth chamber each comprise at least one evacuation line therein.
21. The multi-chamber growth apparatus of claim 13, wherein heating bodies are disposed in the in-situ etching chamber, the carbonization chamber, the growth chamber, and the buffer chamber, respectively.
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