CN111826718A - Barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure - Google Patents

Barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure Download PDF

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CN111826718A
CN111826718A CN202010678954.3A CN202010678954A CN111826718A CN 111826718 A CN111826718 A CN 111826718A CN 202010678954 A CN202010678954 A CN 202010678954A CN 111826718 A CN111826718 A CN 111826718A
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barrel
tube
reaction tube
heat insulation
growth
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CN111826718B (en
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方文卿
蒲勇
程海英
陈炳安
赵鹏
杨超普
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Nanchang University
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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
    • C30B25/08Reaction chambers; Selection of materials therefor
    • 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
    • C30B25/10Heating of the reaction chamber or the substrate
    • 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
    • C30B25/16Controlling or regulating
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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Abstract

The invention relates to a barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube, which relates to the technical field of silicon carbide epitaxial wafer manufacturing growth equipment, wherein a barrel-shaped structure can greatly improve the yield of silicon carbide epitaxial wafers, and the temperature uniformity of a substrate is naturally ensured; along with the increase of the size of the substrate, the diameter of the barrel can also be increased, the heating coil can be made into a plurality of fan-shaped bodies, and the graphite barrel can also be formed by splicing a plurality of fan-shaped surfaces; the main body of the reaction tube is replaced in each furnace, so that the initial state of epitaxial growth is constant, and the problem of repeatability commonly existing at present is solved; the manipulator is used for operation, so that the machine time is not wasted; the use cost is reduced by adopting a pipe sleeve pipe structure; a laser online film thickness monitoring and dual-wavelength online temperature measuring device is arranged; the air flow and water flow symmetry design is adopted to ensure natural and uniform growth parameters; the invention belongs to a near-coupling system, and the uniformity of the film thickness is easy to be ensured; the invention is also suitable for the production of devices such as UV LEDs and the like.

Description

Barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure
Technical Field
The invention relates to the technical field of manufacturing silicon carbide epitaxial wafer growth equipment, in particular to a barrel-shaped symmetrical multi-chip silicon carbide epitaxial growth reaction tube structure.
Background
SiC is a new generation of wide bandgap semiconductor material, and the power semiconductor device thereof is very hot at present. However, the current yield of the whole industry chain is extremely low, which includes the growth yield of SiC single crystal material and the controllability of SiC epitaxial growth. Especially epitaxial growth, the problems of poor repeatability and incapability of accurately controlling process parameters commonly exist in the current epitaxial growth equipment used at home and abroad. Therefore, it is necessary to develop an epitaxial growth apparatus capable of stable mass production in combination with the actual situation of the growth of SiC single crystal material, which is the reaction tube technology at the core.
Three suppliers of SiC epitaxial equipment are mainly found internationally, i.e., Aixtron, italy LPE, and TEL, germany, and the national institute of semiconductor technology, ltd, and changsha, which are located in dongguan. Because the SiC epitaxial growth temperature is about 1700 ℃, the temperature uniformity problem is caused due to the high temperature, and in the aspect of heat preservation, the heat preservation mode is divided into a 'hot wall' system and a 'hot wall' system at present; in theory, "hot wall" systems are more likely to achieve good temperature uniformity and more stable gas flow patterns. However, the "hot wall" may also result in a slow temperature ramp rate, so that the material growth interface is not steep. The design of the warm wall is adopted in the scheme, but the temperature of the warm wall is obviously higher.
The applicant has been granted the invention of a cylindrical GaN epitaxial growth reactor in which the epitaxial substrate is horizontally disposed. In the present case, the SiC epitaxial substrate is vertically placed. The wafer mounting structure with a round barrel shape is used, the maximum benefit is that the temperature uniformity can be naturally ensured, but the defect is that the growth of the epitaxial wafer can be limited to 2 inches. While this is just well suited to the current state of supply of SiC substrates, currently with 2 inch SiC substrates, economics may be better. In the long run, the possibility of using multiple 6 inch and 8 inch SiC substrates in the future is not high. This is because when the substrate is horizontally placed, the uniformity of the multi-wafer epitaxy is not good due to the excessively high growth temperature, and the yield of large size of the SiC single crystal rod is not satisfactory at present due to the growth thereof.
The stability of airflow and the uniformity of growth thickness of the existing SiC epitaxial growth reaction tube cannot be essentially made. The device adopts a near-coupling technology to uniformly distribute the growth sources on the surface of the epitaxial wafer, thereby fundamentally ensuring the uniformity of growth.
The biggest defect of the existing SiC epitaxial growth equipment is the cleaning problem, and all reaction tubes are basically not cleaned until the SiC material is very stable until the SiC material cannot grow. On the one hand, expensive reaction pipe fittings are wasted, most importantly, process parameters between furnaces cannot be repeated, so that the profitability level of the whole industry is extremely poor at present, and the application range of SiC high-power devices is greatly limited. In this respect, the scheme is carefully considered, and all the good fittings in the reaction tube of each furnace are replaced. And the whole quick replacement of the manipulator is used, and the production efficiency is not influenced.
The temperature control system of the existing SiC epitaxial growth equipment cannot be corrected in each furnace, the sapphire infrared temperature measurement probe is used in the scheme, each furnace is replaced and automatically corrected, gas purging protection is carried out, and power parameters of induction heating are correlated to ensure that temperature measurement can be accurately controlled. The temperature among the epitaxial devices is corrected according to a unified standard, so that the process parameters of all epitaxial furnaces in a company are ensured to be consistent, and the process transplantation and the production expansion are facilitated.
The existing SiC epitaxial furnace has no on-line film thickness monitoring system, and the sapphire template with AlN epitaxially grown on the surface is used as a companion wafer in the scheme, so that the defect that the film thickness cannot be monitored on line by homoepitaxy is overcome, and the precise structure design of a SiC device becomes possible.
The present case adopts a manipulator of many epitaxial furnaces sharing, a feeding loadLock of sharing and an ejection of compact loadLock thereby furthest guarantees that the growing environment is clean, guarantees production efficiency's improvement.
Disclosure of Invention
The invention aims to solve the problems of capacity, stability, cost of ownership, precise design of an epitaxial structure, automatic operation and the like of the existing SiC epitaxial furnace, and particularly solves the problem that the initial state of a reaction tube cannot be stable.
The purpose of the invention is realized by the following steps:
a cylindrical symmetrical multi-chip silicon carbide epitaxial growth reaction tube, a substrate is vertically placed on the surface of a graphite barrel, and a carbon source and a silicon source for growth are respectively sprayed to the surface of the substrate from respective source tubes through nozzles to grow; the heating coil heats the graphite barrel through electromagnetic induction; the graphite barrel rotates around the central symmetry axis; the waste gas after growth is pumped out through a tail gas port at the lower part of the graphite center.
The graphite barrel comprises a slide glass barrel, an upper graphite barrel and a lower graphite barrel, wherein n is uniformly cut on the surface of the slide glass barrel1A plane, each plane can be placed with n2A sheet substrate so that n can be grown at a time1*n2A SiC epitaxial wafer; for example, 24 upright planes are uniformly cut on the surface of the slide bucket, and 3 pieces of 2-inch substrates can be placed on each plane, so that 72 pieces of 2-inch SiC epitaxial wafers can be grown at one time; the upper graphite barrel and the lower graphite barrel are arranged to ensure the axial temperature uniformity of the slide glass barrel; a motor is arranged in the bottom of the reaction chamber, and the upper barrel is supported to rotate around the central shaft under the drive of the motor and the rotating gear; the stainless steel base is provided with a bearing at a gap with the barrel support, the whole graphite barrel is placed on the barrel support, a quartz tube is arranged outside the graphite barrel, an upper cover plate is arranged on the upper portion of the quartz tube and fixedly connected with an upper heat insulation plate through an upper cover hanging clamp, the stainless steel base is provided with a lower heat insulation and loading and unloading clamp, the mechanical hand operation is facilitated, and if a 4-inch SiC epitaxial wafer needs to grow, the diameter of the graphite barrel needs to be enlarged in proportion.
The source tube and the heat insulation tube are coaxial, and the outer walls of the heat insulation tubes are tightly attached to each other after thermal expansion factors are considered, so that the external heat radiation of the graphite barrel is isolated, and the inner surface of the quartz tube is protected from being deposited by reactants; in order to improve the isolation effect, the heat insulation pipe is partially ground to be a flat cutting pipe in the technical scheme; the heat insulation pipe is also used for insulating heat of a source pipe in the heat insulation pipe, and the source pipe comprises a carbon source pipe and a silicon source pipe; a plurality of source pipes and heat insulation pipes are inserted into the stainless steel base and sealed by side sealing O rings; the upper half of the heat insulating pipe is processed into a half pipe form, and the nozzle is installed on the half pipe.
The temperature measurement protective guide tube is used for protecting a transparent light guide column inside the temperature measurement protective guide tube in an inflating mode, optical signals from the light guide column are subjected to optical temperature measurement to become electric signals, and finally the electric signals are used for temperature measurement and temperature control.
The stainless steel base is loaded with all reaction tube components surrounded by a quartz tube (bell jar), namely, a manipulator can hook a loading and unloading hanging card with heat insulation, so that the whole reaction tube main body is replaced; before replacement, the manipulator can hook the upper cover hanging card and move the upper cover plate together with the heat insulation plate on the upper cover plate; the stainless steel base and the bottom of the reaction chamber are connected through a loose joint.
The loose joint comprises various types of gas and cooling connection of a reaction tube and also comprises conventional double-O-ring vacuum sealing connection; after the double O rings are vacuumized, the stainless steel base toilet and the bottom of the reaction chamber realize surface contact, so that the indirect cooling effect is ensured; and the independent transportation of quartz tube shielding gas, heat insulation tube shielding gas, reaction source and carrier gas and the sufficient cooling of corresponding sealing O rings are realized.
The heating coil and the protective sleeve are symmetrically arranged in the water flow direction of the water inlet and the water outlet of the cooling water, so that the temperature of the coil is ensured to be consistent in the height direction, and the temperature uniformity of the graphite barrel is improved; the cooling water is replaced by an insulating high-temperature cooling medium such as high-temperature-resistant oil, so that the temperature of the graphite barrel can be further increased; the heating coil and the protective sleeve further comprise a necessary design for changing the direction of magnetic force lines, a heat-preservation energy-saving design and a necessary filling design, for example, heat-conducting SiC fine sand is filled between the quartz tube and the coil to ensure that the quartz tube is sufficiently and uniformly cooled in a heat conduction manner, so that the service life and the strength of the quartz tube are ensured, and the adhesion of high-temperature deposits which are difficult to clean is also avoided.
The laser interference film thickness on-line monitor can monitor the growth condition of the SiC film on the sapphire template on line through the quartz tube, so that the growth condition of the epitaxial layer on the silicon carbide substrate is deduced, and the airflow limiting plate is used for radially separating a growth area from a non-growth area.
The standard temperature generator is formed by simulating black body radiation by an infrared light emitting diode, is used for automatic correction of each furnace, is powered by a battery, is loaded to a set position by a manipulator, and performs automatic correction before growth on optical measurement.
The whole process of the barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube comprises the following steps,
s1. carbon source (e.g. ethylene C)2H2But not limited to) and a silicon source (e.g., silane SiH)4) Respectively spraying carrier gas from a plurality of small spray holes of the carbon source pipe and the silicon source pipe to the surface of the substrate for high-temperature growth, and discharging waste gas from a tail gas port;
s2, after the growth is finished, carrying a manipulator by the rail trolley to the position of the reaction tube along the slide rail, removing the upper cover plate of the reaction tube, placing the upper cover plate of the reaction tube on a support of a discharging LoadLock, and then taking out the whole reaction tube main body on the stainless steel base by the manipulator and placing the whole reaction tube main body in the discharging LoadLock;
s3, then, taking out the other set of reaction tube main body from the feeding LoadLock by the mechanical arm, and putting the reaction tube main body into a quartz tube for growing a new furnace;
s4, a standard temperature generator bound on the manipulator before growth performs automatic temperature correction on optical temperature measurement;
s5, when a new furnace starts to grow, an operator takes out an epitaxial wafer from the discharging loadLock, detaches the main body of the reaction tube, contains all the heat insulation tubes, the silicon source tube and the carbon source tube, and mechanically cleans the heat insulation tubes, the silicon source tube and the carbon source tube one by one; then, performing vacuum high-temperature cleaning outside the furnace on the non-metal high-temperature resistant insulating piece in the whole reaction tube main body;
s6, after cleaning, reloading a new substrate, and sending the substrate into a feeding LoadLock for later use; obviously, a set of mechanical arm, a set of feeding LoadLock and a set of discharging LoadLock can be shared by a plurality of epitaxial furnaces; the manipulator moves in the stainless steel inert gas chamber to automatically complete various operations.
In addition, the quartz tube cannot be taken out of every furnace, which relates to the problems of cleaning and service life of the quartz tube, and one method is to add a cylindrical SiC lining between the quartz tube and the heat insulation tube, and then take out and clean the lining every time; the other method is that the heating coil and the heat-insulating sleeve are made into two symmetrical half-barrels, when in growth, the two half-barrels are closed, and before the quartz is taken out, the two half-barrels are separated; at the moment, a quartz tube is replaced by a bell jar, and the bell jar is made of high-temperature resistant insulating ceramics such as quartz, SiC or alumina; in order to make the tail gas of the reaction tube flow more reasonably, a tail gas tube is inserted into the tail gas port, and the upper end of the tail gas tube and the upper end of the graphite barrel are at about the same height; in addition, the rotary gear and the bearing are designed to be deeply sunk at the bottom of the reaction chamber with water cooling, so that better cooling and more stable rotating effect are obtained.
The invention has the beneficial effects that:
1. the bucket structure can greatly improve the yield of the silicon carbide epitaxial wafer, and the temperature uniformity of the substrate is naturally ensured; along with the increase of the size of the substrate, the diameter of the barrel can also be increased, the heating coil can be made into a plurality of fan-shaped bodies, the graphite barrel can also be formed by splicing a plurality of fan-shaped surfaces, and near coupling and low rotating speed are added, so that a huge multi-wafer machine becomes possible, for example, 72 pieces of 6-inch SiC epitaxial wafers can be grown at one time.
2. The main body of the reaction tube is replaced in each furnace, so that the initial state of epitaxial growth is constant, the production is stable and controllable, and the problem of production repeatability commonly existing at present is solved;
3. the manipulator is used for operation, so that the production stability is further improved;
4. the automatic production mode that a pipe sleeve pipe structure which is easy to maintain and low in cost and a plurality of epitaxial furnaces share one set of manipulator is adopted, so that the cost of epitaxial equipment accessories and peripheral auxiliary equipment is saved to the maximum extent, and the occupied area is also reduced;
5. a laser online film thickness monitoring and dual-wavelength online temperature measuring device is additionally arranged, so that the controllability and the precision of epitaxial growth are greatly improved;
6. the symmetrical design is adopted by airflow and water flow to ensure that the growth parameters are natural and uniform; the influence of the temperature of the quartz tube wall on the temperature uniformity of the substrate is taken into consideration; the quartz tube is protected;
drawings
FIG. 1 is a schematic view of a barrel SiC epitaxial reactor structure according to the present invention;
FIG. 2 is a schematic view of the dual thermal insulation of the pipe in pipe casing and the separate transportation of the carbon source of silicon source in accordance with the present invention;
FIG. 3 is a schematic view of the water flow direction and nozzle of the induction coil of the present invention;
FIG. 4 is a schematic view of the sealing and gas supply of the double tube of the present invention;
FIG. 5 is a schematic view of the base cooling and gas supply of the present invention;
FIG. 6 is a schematic view of an outer SiC tube nozzle mount of the present invention;
FIG. 7 is a three-dimensional view of the nozzle assembly of the present invention;
FIG. 8 is a schematic view of an on-line film thickness monitoring and outer sleeve attaching method according to the present invention;
FIG. 9 is a schematic diagram of a half-cylinder induction coil winding method of the present invention;
FIG. 10 is a schematic view of the robot operation of the present invention;
in the figure: 1-a graphite barrel; 101-slide bucket; 102-upper graphite barrel; 103-lower graphite barrel; 2-a substrate; 3-source tube; 301-carbon source tube; 302-a silicon source tube; 4-a heat insulation pipe; 401-half tube; 402-flattening the tubes; 5-a nozzle; 6-loose joint; 601-quartz tube shielding gas; 602-insulating tube shielding gas; 603-reaction source and carrier gas; 604-indirect cooling; 7-a motor; 8-tail gas port; 9-optical temperature measurement; 10-a rotating gear; 11-stainless steel base; 12-a bearing; 13-lower heat insulation and loading and unloading card; 14-temperature measurement and catheter protection; 15-standard temperature generator; 16-heating coil and insulating sleeve; 1601-a water inlet; 1602-water outlet; 17-mounting a heat insulation plate; 18-an upper cover plate; 19-hanging the upper cover; 20-a quartz tube; 21, supporting the barrel; 22-reaction chamber bottom; 23-a gas flow restrictor plate; 24-laser interference film thickness on-line monitor; 25-nozzle plug and fixing clip; 26-a manipulator; 27-a rail trolley; 28-a slide rail; 29-LoadLock feed; 30-discharging LoadLock; 31-an inert gas chamber; 32-side seal O-rings; 33-sapphire template.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention; it is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: a barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure. See fig. 1-10.
The substrate 2 is vertically arranged on the surface of the graphite barrel 1, and a carbon source and a silicon source for growth are sprayed to the surface of the substrate 2 from a source tube 3 through a nozzle 5 for growth; the heating coil and the heat insulation sleeve 16 heat the graphite barrel 1 through electromagnetic induction; the graphite barrel 1 rotates around a central symmetry axis; the exhaust gas after growth is pumped out through the exhaust port 8.
The graphite barrel 1 consists of a slide glass barrel 101, an upper graphite barrel 102 and a lower graphite barrel 103, 24 planes are uniformly cut on the surface of the slide glass barrel 101, and 3 2-inch substrates can be placed on each plane, so that 72 SiC epitaxial wafers with 2 inches can be grown at one time; the upper graphite barrel 102 and the lower graphite barrel 103 are arranged to ensure the temperature uniformity of the slide glass barrel 101; the whole graphite barrel 1 is placed on the barrel support 21 and rotates around the central shaft under the drive of the motor 7 and the rotating gear 10; a bearing 12 is arranged at the gap between the stainless steel base 11 and the barrel support 21.
The source tube 3 and the heat insulation tube 4 are coaxial, and the outer walls of the heat insulation tube 4 are tightly attached to each other after thermal expansion factors are considered, so that the heat radiation of the graphite barrel 1 to the outside is isolated and the inner surface of the quartz tube 20 is protected from being deposited by reactants; to enhance the insulation effect, the insulating tube 4 is partially ground flat in this embodiment, as shown by the flattened tube 402; the heat insulation pipe 4 also insulates heat of the source pipe 3 in the heat insulation pipe, and the source pipe 3 comprises a carbon source pipe 301 and a silicon source pipe 302; a plurality of source pipes 3 and heat insulation pipes 4 are inserted into the stainless steel base 11 and sealed by side sealing O rings 32; the upper half of the heat insulating pipe 4 is formed in the form of a half pipe 11, and the nozzle 5 is mounted on the half pipe 11.
The temperature measurement protection conduit 14 is used for inflating and protecting the transparent light guide column inside, and the optical signals from the light guide column pass through the optical temperature measurement 9 to be converted into electric signals, and finally are used for temperature measurement and temperature control.
The stainless steel base 11 is loaded with all reaction tube components surrounded by the quartz tube 20, namely, the manipulator 20 can hook the lower heat insulation and loading and unloading card 13 to realize the replacement of the reaction tube main body; before replacement, the manipulator 20 can hook the upper cover hanging card 19 to remove the upper cover plate 18 together with the upper heat insulation plate 17; the stainless steel base 11 and the reaction chamber bottom 22 are connected by a loose joint 6.
The loose joint 6 comprises various types of gas and cooling connection of a reaction tube and also comprises conventional double-O-ring vacuum sealing connection; after the double O rings are vacuumized, the stainless steel base 11 is in surface contact with the bottom 22 of the reaction chamber, so that the effect of indirect cooling 604 is ensured; and the quartz tube shielding gas 601, the heat insulation tube shielding gas 602, the reaction source and the carrier gas 603, the respective sealing transportation and the corresponding sealing O-ring cooling are also realized.
The heating coil and the protective sleeve 16 are symmetrically arranged in the water flow direction of the cooling water inlet 1601 and the cooling water outlet 1602, so as to ensure that the temperature of the coil is consistent in the height direction, thereby increasing the temperature uniformity of the graphite barrel 1; the cooling water is replaced by an insulating high-temperature cooling medium such as high-temperature-resistant oil, so that the temperature of the graphite barrel 1 can be further increased; the heating coil and the protective sleeve 16 further comprise a necessary design for changing the direction of magnetic lines of force, a heat-insulating and energy-saving design, and a necessary filling design, for example, heat-conducting SiC fine sand is filled between the quartz tube 20 and the coil to ensure that the quartz tube 20 is sufficiently and uniformly cooled by heat conduction, so that the service life and the strength of the quartz tube 20 are ensured, and high-temperature deposition which is difficult to clean is also avoided.
The laser interference film thickness on-line monitor 24 can monitor the growth condition of the SiC film on the sapphire template 33 on line through the quartz tube 20, so that the growth condition of the epitaxial layer on the silicon carbide substrate is inferred, and the airflow limiting plate 23 is used for separating a growth area from a non-growth area.
The standard temperature generator 15 is formed by simulating black body radiation by an infrared light emitting diode, is used for automatic correction of each furnace, is powered by a battery, is brought to a set position by a manipulator 26, and performs automatic correction before growth on the optical measurement 9.
The invention also provides a process for preparing the barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube, which comprises the following steps:
s1. carbon source (e.g. ethylene C)2H2) And a silicon source (e.g., silane SiH)4) Respectively spraying carrier gas from a plurality of small spray holes of the carbon source pipe 301 and the silicon source pipe 302 to the surface of the substrate 2 for high-temperature growth, and discharging waste gas from the tail gas port 8;
s2, after the growth is finished, carrying a manipulator 26 by the rail trolley 27 to the position of the reaction tube along the slide rail 28, removing the upper cover plate 18 of the reaction tube, placing the reaction tube on a support of a discharging LoadLock30, and then taking out the whole reaction tube main body on the stainless steel base 11 by the manipulator 26 and placing the whole reaction tube main body in the discharging LoadLock 30;
s3, subsequently, the mechanical arm 26 takes out another set of reaction tube main body from the feeding LoadLock29 and puts the reaction tube main body into the quartz tube 20 for the growth of a new furnace;
s4, a standard temperature generator bound on the manipulator 26 before growth performs automatic temperature correction on the optical temperature measurement 9;
s5, after a new furnace starts to grow, an operator takes out epitaxial wafers from a discharge LoadLock30, and detaches the main body of the reaction tube to perform mechanical cleaning piece by piece;
s6, performing vacuum high-temperature cleaning outside the furnace on the non-metal high-temperature-resistant insulating piece in the whole reaction tube main body; after cleaning, new substrates are reloaded and sent to a feed LoadLock30 for standby; obviously, a set of mechanical arm 26, a set of feeding LoadLock29 and a set of discharging LoadLock30 can be shared by a plurality of epitaxial furnaces; the robot 26 moves in the stainless steel inert gas chamber 31 and operates automatically.
Example 2: the reaction tube bell cover also takes out the cleaned barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure. See fig. 1-10.
In example 1, the quartz tube 20 was not removable from the furnace, which involved the problem of cleaning and life of the quartz tube 20, by adding a cylindrical SiC liner between the quartz tube 20 and the heat insulating tube 4, and then removing the liner each time; the other method is that the heating coil and the heat-insulating sleeve 16 are made into two symmetrical half-barrels, when in growth, the two half-barrels are closed, and before loading and unloading, the two half-barrels are separated; at this time, the quartz tube 20 is replaced by a bell jar, and the bell jar is made of high-temperature resistant insulating ceramics such as quartz, SiC or alumina; in order to make the tail gas of the reaction tube flow more reasonably, a tail gas tube is inserted into the tail gas port 8, and the upper end of the tail gas tube and the upper end of the graphite barrel 1 are fixed at the same height; in this embodiment, the rotating gear 10 and the bearing 12 are recessed in the bottom 22 of the reaction chamber where water is cooled, resulting in better cooling and smoother rotation.
The types of flow gases for the insulating tube shielding gas 602, the reaction source and the carrier gas 603 are adjusted in this embodiment so that they flow through the silicon source and the carrier gas, the carbon source and the carrier gas, respectively.
Obviously, if the vacuum tightness of the inert gas chamber 31 is good enough, the airtightness of the quartz tube 20 may not be required, and even the quartz tube 20 may be eliminated; a fence is directly formed by a plurality of heating coils and a heat insulation sleeve 16; the low speed rotation and the close coupling of the present invention provide the possibility of growing the tube 20 without quartz. Other similar examples to example 1 will not be described.
The above description is only an example and is not intended to limit the scope of the present disclosure, and all equivalent modifications made by the present disclosure and the attached drawings or directly or indirectly applied to the related technical fields are also included in the scope of the present disclosure.

Claims (8)

1. The utility model provides a circular barrel shape symmetry multi-disc carborundum epitaxial growth reaction tube which characterized in that includes:
the substrate is vertically placed on the surface of the graphite barrel, and a carbon source and a silicon source for growth are separately sprayed to the surface of the substrate from respective source pipes through nozzles for growth; the distance between the spray hole of the source tube and the surface of the substrate is less than 30 mm; a motor is arranged in the bottom of the reaction chamber, and the upper barrel is supported to rotate around the central shaft under the drive of the motor and the rotating gear; a bearing is arranged at the gap between the stainless steel base and the barrel support, the whole graphite barrel is placed on the barrel support, and the graphite barrel rotates around the central symmetry axis; a heating coil and a heat-insulating sleeve outside the quartz tube heat the graphite barrel through electromagnetic induction; the grown waste gas is pumped out through a tail gas port at the bottom of the graphite barrel; a quartz tube is arranged outside the graphite barrel, an upper cover plate is arranged at the upper part of the quartz tube and fixedly connected with the upper heat insulation plate through an upper cover hanging clamp, and a lower heat insulation and assembling and disassembling clamp is arranged on the stainless steel base, so that the operation of a manipulator is facilitated;
the source pipe and the heat insulation pipes are coaxially arranged, and one source pipe is inserted into each heat insulation pipe; the heat insulation pipes are tightly attached to each other, so that the heat radiation of the graphite barrel to the outside is isolated, and the inner surface of the quartz pipe is protected from being deposited by reactants; the source tube comprises a carbon source tube and a silicon source tube, and the heat insulation tube, the carbon source tube and the silicon source tube are sequentially arranged; the source pipe and the heat insulation pipe are inserted into the stainless steel base, and the stainless steel base is contacted with the bottom of the reaction chamber.
2. The barrel-shaped symmetric multi-piece silicon carbide epitaxial growth reaction tube of claim 1, characterized in that: the graphite barrel consists of a slide glass barrel, an upper graphite barrel and a lower graphite barrel, and n is uniformly cut on the surface of the slide glass barrel1A plane, each plane can be placed with n2A sheet substrate so that n can be grown at a time1*n2And (5) carrying out SiC epitaxial wafer.
3. The barrel-shaped symmetric multi-piece silicon carbide epitaxial growth reaction tube of claim 1, characterized in that: the outer surface parts of the heat insulation pipe are ground flat or embedded with each other for enhancing the heat insulation effect and reducing the deposition on the inner surface of the quartz pipe.
4. The barrel-shaped symmetric multi-piece silicon carbide epitaxial growth reaction tube of claim 1, characterized in that: the temperature measurement and protection catheter is used for inflating and protecting the transparent light guide column inside the temperature measurement and protection catheter, optical signals from the light guide column are subjected to optical temperature measurement and converted into electric signals, and the electric signals are finally used for temperature measurement and temperature control; during temperature measurement, dual-wavelength temperature measurement is used for eliminating the influence of optical surface deposition on measurement; the standard temperature generator bound on the manipulator is formed by simulating black body radiation by an infrared light emitting diode and is used for automatically correcting the temperature of each furnace, self batteries are adopted for supplying power, the manipulator is brought into a set position, and the optical measurement is automatically corrected before growth.
5. The barrel-shaped symmetric multi-piece silicon carbide epitaxial growth reaction tube of claim 1, characterized in that: a barrel-shaped thermal liner is disposed between the thermal tube and the quartz tube to reduce deposition of reactants on the quartz tube.
6. The barrel-shaped symmetric multi-piece silicon carbide epitaxial growth reaction tube of claim 1, characterized in that: the device also comprises a laser interference film thickness on-line monitor, which can monitor the growth condition of the SiC film on the sapphire template on line through the quartz tube, and further monitor the growth condition of the epitaxial layer on the silicon carbide substrate.
7. The barrel-shaped symmetric multi-piece silicon carbide epitaxial growth reaction tube of claim 1, characterized in that: the upper half part of the heat insulation pipe is processed into a half pipe, and the nozzle is arranged on the half pipe; the types of the flowing gas of the protective gas, the reaction source and the carrier gas of the heat insulation pipe are adjusted.
8. A process for preparing a barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube is characterized by comprising the following steps:
s1, spraying carrier gas to the surface of a substrate from a plurality of small spray holes of a carbon source tube and a silicon source tube respectively to perform high-temperature growth, and discharging waste gas from a tail gas port;
s2, after the growth is finished, carrying a manipulator by the rail trolley to the position of the reaction tube along the slide rail, removing an upper cover plate of the reaction tube, placing the upper cover plate on a support of a discharging LoadLock, and then taking out the whole reaction tube main body on the stainless steel base by the manipulator and placing the whole reaction tube main body in the discharging LoadLock;
s3, then, taking out the other set of reaction tube main body from the feeding LoadLock by the mechanical arm, and putting the reaction tube main body into a quartz tube for growing a new furnace;
s4, a standard temperature generator bound on the manipulator before growth performs automatic temperature correction on optical temperature measurement;
s5, when a new furnace starts to grow, an operator takes out an epitaxial wafer from the discharging loadLock, detaches the main body of the reaction tube, contains all the heat insulation tubes, the silicon source tube and the carbon source tube, and mechanically cleans the heat insulation tubes, the silicon source tube and the carbon source tube one by one; then, performing vacuum high-temperature cleaning outside the furnace on the non-metal high-temperature resistant insulating piece in the whole reaction tube main body;
s6, after cleaning, reloading a new substrate, and sending the substrate into a feeding LoadLock for later use; the manipulator moves in the stainless steel inert gas chamber to automatically complete various operations.
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