CN111826718B - 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

Info

Publication number
CN111826718B
CN111826718B CN202010678954.3A CN202010678954A CN111826718B CN 111826718 B CN111826718 B CN 111826718B CN 202010678954 A CN202010678954 A CN 202010678954A CN 111826718 B CN111826718 B CN 111826718B
Authority
CN
China
Prior art keywords
barrel
tube
reaction tube
growth
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010678954.3A
Other languages
Chinese (zh)
Other versions
CN111826718A (en
Inventor
方文卿
蒲勇
程海英
陈炳安
赵鹏
杨超普
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanchang University
Original Assignee
Nanchang University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanchang University filed Critical Nanchang University
Priority to CN202010678954.3A priority Critical patent/CN111826718B/en
Publication of CN111826718A publication Critical patent/CN111826718A/en
Application granted granted Critical
Publication of CN111826718B publication Critical patent/CN111826718B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/08—Reaction chambers; Selection of materials therefor
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/10—Heating of the reaction chamber or the substrate
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/16—Controlling or regulating
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Landscapes

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

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 growth equipment, wherein the barrel-shaped structure can greatly improve the yield of silicon carbide epitaxial wafers, and the temperature uniformity performance of a substrate is naturally ensured; with the increase of the size of the substrate, the diameter of the barrel can be increased, the heating coil can be made into a plurality of fan-shaped parts, and the graphite barrel can be formed by splicing a plurality of fan-shaped parts; the main body of the reaction tube is replaced every furnace, so that the initial state of epitaxial growth is constant, and the current common repeatability problem is overcome; the manipulator is used for operation, so that the machine time is not wasted; the use cost is reduced by adopting a pipe sleeve structure; the device is provided with a laser online film thickness monitoring and dual-wavelength online temperature measuring device; the design of symmetry of air flow and water flow is focused on to ensure natural and uniform growth parameters; the invention belongs to a near coupling system, and the uniformity of 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 silicon carbide epitaxial wafer growth equipment, in particular to a barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure.
Background
SiC is a new generation of wide bandgap semiconductor material, and its power semiconductor devices are currently very hot. However, the current yield of the whole industry chain is also extremely low, which includes the growth yield of SiC single crystal material and the controllability of SiC epitaxial growth. In particular to epitaxial growth, the existing epitaxial growth equipment used at home and abroad generally has the problems of poor repeatability and incapability of accurately controlling process parameters. Therefore, it is necessary to develop an epitaxial growth apparatus that can be stably mass-produced in combination with the practical situation of growth of SiC single crystal materials, the core of which is the reaction tube technology.
There are mainly three SiC epitaxial equipment suppliers internationally, which are Aixtron corporation, LPE corporation and TEL corporation, japan, germany, and the semiconductor technology limited of the eastern guan city and the long sand company, respectively, in developing SiC epitaxial equipment. Because the epitaxial growth temperature of SiC is about 1700 ℃, the high temperature brings about the problem of temperature uniformity, and in the heat preservation mode, a hot wall system and a hot wall system are divided at present; theoretically, a "hot wall" system is easier to achieve good temperature uniformity and a more stable airflow pattern. However, the "hot wall" may also cause a slow rise and fall of temperature so that the material growth interface is not steep. The scheme adopts a warm wall design, but the temperature of the warm wall is obviously higher.
The applicant has patented an invention of a cylindrical GaN epitaxial growth reactor in which the epitaxial substrate is placed horizontally. In this case, the SiC epitaxial substrate is vertically placed. The barrel-shaped chip loading structure has the greatest advantage of naturally guaranteeing the uniformity of temperature, but has the disadvantage of being possibly limited to 2 inches of epitaxial wafer growth. Only this happens to be appropriate for the current supply of SiC substrates, with 2 inch SiC substrates currently being used, the economics may be better. In the long term, the likelihood of using multiple 6 inch and 8 inch SiC substrates is not high in the future. This is because when the substrate is placed horizontally, the growth temperature is too high to determine the uniformity of the multi-wafer epitaxy, and the growth of SiC single crystal rods is not satisfactory at present, and the large-size yield is not satisfactory.
The existing SiC epitaxial growth reaction tube cannot be essentially manufactured with the stability of air flow and the uniformity of growth thickness. The scheme 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 cleaning, and all reaction tubes are basically not cleaned until growth cannot be performed at present because the SiC material is very stable. This aspect results in expensive reactor tube fittings being wasted, and most importantly, in the inability of furnace-to-furnace process parameters to be repeatable, resulting in extremely poor levels of profitability throughout the industry at present, greatly limiting the range of applications for SiC high power devices. The scheme makes serious consideration in this aspect, and all the good accessories in the reaction tube of each furnace are replaced. And the whole manipulator is used for quick replacement, so that the production efficiency is not affected.
The existing temperature control system of the SiC epitaxial growth equipment cannot be corrected every furnace, the sapphire infrared temperature measurement probe is used, every furnace is replaced and automatically corrected, the temperature control system is provided with gas purging protection, and then power parameters of induction heating are associated, so that accurate control of temperature measurement is ensured. The temperature among the epitaxial devices is corrected according to the unified standard, so that the process parameters of all epitaxial furnaces in a company are ensured to be consistent, and the process transplanting and the production expanding are convenient.
The existing SiC epitaxial furnace does not have an online film thickness monitoring system, and the sapphire template with the surface on which AlN is epitaxially grown is used as a accompanying piece, so that the defect that homoepitaxy cannot monitor film thickness online is overcome, and the precise structural design of a SiC device is enabled to be possible.
The scheme adopts a plurality of epitaxial furnaces to share one manipulator, and shares one feeding LoadLock and one discharging LoadLock, thereby maximally ensuring the clean growth environment and improving the production efficiency.
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 conventional SiC epitaxial furnace, and particularly solves the problem that the initial state of a reaction tube cannot be stabilized.
The object of the invention is achieved in that:
a plurality of cylindrical symmetrical silicon carbide epitaxial growth reaction tubes, wherein a substrate is vertically arranged on the surface of a graphite barrel, and a carbon source and a silicon source for growth are respectively sprayed from respective source tubes to the surface of the substrate through nozzles for growth; the heating coil heats the graphite barrel through electromagnetic induction; the graphite barrel rotates around a central symmetry axis; the waste gas after growth is pumped out through a tail gas port positioned at the lower part of the center of the graphite.
The graphite barrel comprises a slide glass barrel, an upper graphite barrel and a lower graphite barrel, and n is uniformly cut out from the surface of the slide glass barrel 1 Each plane is provided withCan place n on the plane 2 A sheet substrate, such that n can be grown at a time 1 *n 2 A piece of SiC epitaxial wafer; for example, 24 vertical planes are uniformly cut on the surface of a slide glass barrel, and 3 substrates with 2 inches 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 and the lower graphite barrel are arranged to ensure the uniformity of the axial temperature of the slide 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 the gap between the stainless steel base and 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 operation of a mechanical arm is convenient, and if a 4-inch SiC epitaxial wafer is to be grown, the diameter of the graphite barrel is required to be enlarged proportionally.
The source tube and the heat insulation tube are coaxial, and the outer walls of the heat insulation tubes are clung to each other after the thermal expansion factor is considered, so that the external heat radiation of the graphite barrel is isolated, and the inner surface of the quartz tube is protected from deposition of reactants; in order to improve the isolation effect, the heat insulation pipe is partially ground flat in the technical scheme to become a cut flat pipe; the heat insulation pipe also insulates the source pipe inside 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 are sealed through side sealing O rings; the upper half of the heat insulating pipe is processed into a half pipe form, and the nozzle is arranged on the half pipe.
The temperature measuring protective conduit is used for inflating and protecting the transparent light guide column in the temperature measuring protective conduit, and optical signals from the light guide column are subjected to optical temperature measurement to become electric signals, and finally 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 mechanical arm can hook a loading and unloading hanging card with heat insulation, so that the integral replacement of the reaction tube main body is realized; before replacement, the manipulator can also hook the upper cover hanging clamp to remove the upper cover plate and the upper heat insulation plate; the stainless steel base is movably connected with the bottom of the reaction chamber.
The loose joint comprises various gases 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 is in surface contact with the bottom of the reaction chamber, so that the indirect cooling effect is ensured; and the independent transportation of the quartz tube shielding gas, the heat insulation tube shielding gas, the reaction source and the carrier gas and the sufficient cooling of the corresponding sealing O ring are realized.
The water flow directions of the water inlet and the water outlet of the heating coil and the protective sleeve are symmetrically arranged, 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 changed into an insulating high-temperature cooling medium, such as high-temperature oil resistance, so that the temperature of the graphite barrel can be further increased; the heating coil and the protective sleeve also comprise necessary designs for changing the direction of magnetic force lines and heat preservation and energy saving designs, and also comprise necessary filling designs, such as filling heat conduction SiC fine sand between the quartz tube and the coil, so as to ensure that the quartz tube is fully and uniformly cooled by heat conduction, further ensure the service life and strength of the quartz tube, and avoid the adhesion of high-temperature sediments which are not easy to clean.
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 air flow limiting plate is used for radially separating the growth area from the non-growth area.
The standard temperature generator is formed by simulating blackbody radiation by an infrared light emitting diode and is used for automatic correction of each furnace, the battery is powered, and the standard temperature generator is loaded to a set position by a manipulator to automatically correct optical measurement before growth.
The whole process of the cylindrical symmetrical multi-piece silicon carbide epitaxial growth reaction tube comprises the following steps,
s1, carbon source (e.g. ethylene C 2 H 2 But are not limited thereto) and a silicon source (e.g., silane SiH 4 ) The carrier gas is sprayed out from a plurality of small spray holes of the carbon source tube and the silicon source tube respectively to the surface of the substrate for high-temperature growth, and the waste gas is discharged from a tail gas port;
s2, after the growth is completed, the small rail vehicle carries a manipulator to the position of the reaction tube along the sliding rail, removes the upper cover plate of the reaction tube, places the upper cover plate of the reaction tube on a support of a discharging LoadLock, and then takes out the whole reaction tube main body on the stainless steel base by the manipulator and places the whole reaction tube main body in the discharging LoadLock;
s3, then, the manipulator takes out another set of reaction tube main body from the feeding LoadLock and puts the reaction tube main body into a quartz tube for the growth of a new furnace;
s4, automatically calibrating the temperature of the optical temperature by a standard temperature generator bound on the manipulator before growth;
s5, after a new furnace starts to grow, an operator takes out an epitaxial wafer from the discharging LoadLock, and disassembles the main body of the reaction tube, wherein the main body comprises all heat insulation tubes, silicon source tubes and carbon source tubes, and the main body is mechanically cleaned piece by piece; then cleaning the nonmetallic high-temperature resistant insulating part in the whole reaction tube main body at a vacuum high temperature outside the furnace;
s6, after cleaning, reloading a new substrate, and feeding the new substrate into a feeding LoadLock for standby; 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 finish various operations.
In addition, the quartz tube is not taken out of each furnace, which involves the problems of cleaning and service life of the quartz tube, one method is to add a barrel-shaped SiC lining between the quartz tube and the heat insulation tube, and then the lining is taken out and cleaned every time; the heating coil and the heat preservation sleeve are made into two symmetrical half barrels, and when the quartz is grown, the two half barrels are folded, 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 or SiC or alumina; in order to make the tail gas flow of the reaction tube more reasonable, 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 rotating gear and the bearing are designed to be deeply submerged in the bottom of the reaction chamber with water cooling, so that better cooling and smoother rotating effects are obtained.
The invention has the beneficial effects that:
1. the barrel structure can greatly improve the yield of the silicon carbide epitaxial wafer, and the temperature uniformity performance of the substrate is naturally ensured; along with the increase of the size of the substrate, the diameter of the barrel can be increased, the heating coil can be made into a plurality of fan-shaped sections, the graphite barrel can also be formed by splicing a plurality of fan-shaped sections, and the near coupling and the low rotating speed are added, so that a giant multi-chip machine is possible, for example, 72 SiC epitaxial wafers with the size of 6 inches 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, thereby ensuring stable and controllable production and overcoming the current ubiquitous production repeatability problem;
3. the mechanical arm is used for operation, so that the production stability is further improved;
4. the tube sleeve structure which is easy to maintain and low in cost is used, and the multiple epitaxial furnaces share an automatic production mode of a set of manipulator, so that the cost of accessories and peripheral auxiliary equipment of the epitaxial equipment is saved to the greatest extent, and the occupied area is reduced;
5. the 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 the air flow and the water flow to ensure the natural and uniform growth parameters; importance is attached to the influence of the temperature of the quartz tube wall on the uniformity of the substrate temperature; the protection of the quartz tube is achieved;
drawings
FIG. 1 is a schematic diagram of a barrel type SiC epitaxial reactor tube of the present invention;
FIG. 2 is a schematic diagram of the dual thermal insulation of the tube sleeve and the separate transport of the silicon source carbon source according to 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 diagram of the sealing and air supply of a dual tube of the present invention;
FIG. 5 is a schematic view of cooling and air supply of a base of the present invention;
FIG. 6 is a schematic view of an outer SiC tube nozzle mount of the invention;
FIG. 7 is a three-view of a nozzle assembly of the present invention;
FIG. 8 is a schematic diagram of an on-line film thickness monitoring and outer sleeve sticking mode according to the present invention;
FIG. 9 is a schematic diagram of a semi-cylindrical induction coil winding method according to the present invention;
FIG. 10 is a schematic diagram of a robot operation of the present invention;
in the figure: 1-a graphite barrel; 101-a slide bucket; 102-loading a graphite barrel; 103-lower graphite barrel; 2-a substrate; 3-source tube; 301-carbon source tube; 302-a silicon source tube; 4-a heat insulating pipe; 401-half tube; 402-flattening the tube; 5-a nozzle; 6-loose joint; 601-quartz tube shielding gas; 602-insulating tube shielding gas; 603-a reaction source and a carrier gas; 604-indirect cooling; 7-a motor; 8-a tail gas port; 9-optical temperature measurement; 10-rotating a gear; 11-stainless steel base; 12-a bearing; 13-lower insulation and loading and unloading cards; 14-temperature measuring protective tube; 15-a standard temperature generator; 16-heating coils and heat preservation sleeves; 1601-water inlet; 1602-water outlet; 17-upper heat insulation plate; 18-an upper cover plate; 19-hanging a card on the upper cover; 20-quartz tube; 21 barrels support; 22-bottom of reaction chamber; 23-an air flow restriction plate; 24-laser interference film thickness on-line monitor; 25-a spray tube plug and a fixing clip; 26-a manipulator; 27-a track trolley; 28-slide rails; 29-feed LoadLock; 30-discharging LoadLock; 31-an inert gas chamber; 32-side sealing O ring; 33-sapphire template.
Detailed Description
The technical solutions 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 will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the 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 placed on the surface of the graphite barrel 1, and a carbon source and a silicon source for growth are sprayed from the source pipe 3 to the surface of the substrate 2 through the nozzle 5 for growth; the heating coil and the heat preservation 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, wherein 24 planes are uniformly cut out of the surface of the slide glass barrel 101, and 3 substrates with the thickness of 2 inches can be placed on each plane, so that 72 SiC epitaxial wafers with the thickness of 2 inches can be grown at one time in the embodiment; the upper graphite barrel 102 and the lower graphite barrel 103 are arranged to ensure the temperature uniformity of the slide barrel 101; the whole graphite barrel 1 is placed on the barrel support 21 and is driven by the motor 7 and the rotary gear 10 to rotate around the central shaft; 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 clung to each other after the thermal expansion factor is considered, so that the graphite barrel 1 is isolated from external heat radiation and the inner surface of the quartz tube 20 is protected from deposition of reactants; to improve the insulation effect, the insulating tube 4 is partly ground flat in this embodiment, as shown by the cut flat tube 402; the heat insulation pipe 4 also insulates the source pipe 3 inside, and the source pipe 3 comprises a carbon source pipe 301 and a silicon source pipe 302; the source pipes 3 and the heat insulation pipes 4 are inserted into the stainless steel base 11 and are 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 installed on the half pipe 11.
The temperature measuring protective conduit 14 is used for inflating and protecting the transparent light guide column in the interior of the temperature measuring protective conduit, and optical signals from the light guide column are changed into electric signals through the optical temperature measurement 9 and finally used for measuring and controlling temperature.
The stainless steel base 11 is loaded with all the 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, so that the replacement of the reaction tube main body is realized; before replacement, the manipulator 20 can also hook the upper cover hanging clamp 19 to remove the upper cover plate 18 and the upper heat insulation plate 17; the stainless steel base 11 and the bottom 22 of the reaction chamber are connected through a loose joint 6.
The loose joint 6 comprises various 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; the quartz tube protective gas 601, the heat insulation tube protective gas 602, the reaction source and the carrier gas 603 are respectively and hermetically transported and correspondingly cooled by the sealing O ring.
The water flow directions of the heating coil and the protective sleeve 16, the water inlet 1601 and the water outlet 1602 of the cooling water are symmetrically arranged, 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 changed into 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 also comprise necessary designs for changing the direction of magnetic lines of force and heat-preserving and energy-saving designs, and also comprise necessary filling designs, such as filling heat-conducting SiC fine sand between the quartz tube 20 and the coil, so as to ensure that the quartz tube 20 is sufficiently and uniformly cooled by heat conduction, thereby ensuring the service life and strength of the quartz tube 20 and avoiding high-temperature deposition which is not easy to clean.
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, thereby deducing the growth condition of the epitaxial layer on the silicon carbide substrate, and the air flow limiting plate 23 is used for separating a growth area from a non-growth area.
The standard temperature generator 15 is formed by simulating blackbody radiation by an infrared light emitting diode and is used for automatic correction of each furnace, battery power supply and automatic correction of the optical measurement 9 before growth by means of the manipulator 26 brought to a set position.
The invention also provides a process for preparing the cylindrical symmetrical multi-piece silicon carbide epitaxial growth reaction tube, which comprises the following steps:
s1, carbon source (e.g. ethylene C 2 H 2 ) A silicon source (e.g. silane SiH 4 ) The carrier gas is sprayed from a plurality of small spray holes of the carbon source tube 301 and the silicon source tube 302 respectively to the surface of the substrate 2 for high-temperature growth, and the waste gas is discharged from the tail gas port 8;
s2, after the growth is completed, the track trolley 27 carries the manipulator 26 to the position of the reaction tube along the sliding rail 28, removes the upper cover plate 18 of the reaction tube, and places the reaction tube on a support of the discharging LoadLock30, and then the manipulator 26 takes out the whole reaction tube main body on the stainless steel base 11 and places the whole reaction tube main body into the discharging LoadLock30;
s3, then, the manipulator 26 takes out another set of reaction tube main bodies from the feeding LoadLock29 and puts the reaction tube main bodies into the quartz tube 20 for the growth of a new furnace;
s4, automatically calibrating the optical temperature measurement 9 by a standard temperature generator bound on the manipulator 26 before growth;
s5, after a new furnace starts to grow, an operator takes out the epitaxial wafer from the discharging LoadLock30, and disassembles the main body of the reaction tube to mechanically clean the reaction tube piece by piece;
s6, cleaning the nonmetallic high-temperature resistant insulating part in the whole reaction tube main body at a vacuum high temperature outside the furnace; after cleaning, reloading a new substrate, and feeding the new substrate into a feeding LoadLock30 for standby; obviously, a set of manipulators 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 jar 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 for every furnace, which involved the problems of cleaning and life of the quartz tube 20, and one method was to add a cylindrical SiC liner between the quartz tube 20 and the insulating tube 4, and then remove the liner each time; the heating coil and the heat preservation sleeve 16 are made into two symmetrical half barrels, and when the two half barrels are grown, the two half barrels are folded, and before the two half barrels are assembled and disassembled, 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 flow of the reaction tube more reasonable, 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 positioned at the same height; in this embodiment, the rotating gear 10 and bearing 12 are submerged in the water-cooled reaction chamber bottom 22, resulting in better cooling and smoother rotation.
The flow-through gas types of the insulating tube protecting gas 602, the reaction source, and the carrier gas 603, which flow through the silicon source and the carrier gas, the carbon source, and the carrier gas, respectively, are adjusted in this embodiment.
Obviously, if the vacuum tightness of the inert gas chamber 31 is good enough, the air tightness of the quartz tube 20 may not be required, and even the quartz tube 20 may be eliminated; the fence is directly formed by a plurality of heating coils and a thermal insulation sleeve 16; the low speed rotation and near coupling of the present invention provides the possibility of growth without the quartz tube 20. Other similar embodiments 1 will not be described in detail.
The foregoing embodiments are merely examples, and are not intended to limit the scope of the present invention, so that all equivalent changes made in the present specification and the accompanying drawings or direct or indirect application in the relevant technical fields are included in the scope of the present invention.

Claims (7)

1. A cylindrical symmetrical multichip silicon carbide epitaxial growth reaction tube, comprising:
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 from respective source pipes to the surface of the substrate through a nozzle for growth; the distance between the spray hole of the source tube and the surface of the substrate is less than 30mm; 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 a central symmetry axis; a heating coil and a heat preservation sleeve outside the quartz tube heat the graphite barrel through electromagnetic induction; the waste gas after growth is pumped away through a tail gas port at the bottom of the graphite barrel; the graphite barrel is externally provided with a quartz tube, an upper cover plate is arranged on the upper part of the quartz tube and fixedly connected with the upper heat insulation plate through an upper cover hanging clamp, and the stainless steel base is provided with a lower heat insulation and loading and unloading clamp, so that the manipulator is convenient to operate;
the source pipe and the heat insulation pipes are coaxially arranged, and each heat insulation pipe is internally inserted with one source pipe; the heat insulating pipes are tightly attached to each other, so that heat radiation of the graphite barrel to the outside is isolated, and the inner surface of the quartz pipe is protected from deposition of 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 a stainless steel base, and the stainless steel base is contacted with the bottom of the reaction chamber;
the process for preparing the cylindrical symmetrical multi-piece silicon carbide epitaxial growth reaction tube comprises the following steps:
s1, a carbon source and a silicon source are sprayed out from a plurality of small spray holes of a carbon source tube and a silicon source tube respectively by carrier gas to the surface of a substrate for high-temperature growth, and waste gas is discharged from a tail gas port;
s2, after the growth is completed, the small rail vehicle carries a manipulator to the position of the reaction tube along the sliding rail, the upper cover plate of the reaction tube is removed, the upper cover plate is placed on a support of a discharging LoadLock, and then the manipulator takes out the whole reaction tube main body on the stainless steel base and also places the whole reaction tube main body in the discharging LoadLock;
s3, then, the manipulator takes out another set of reaction tube main body from the feeding LoadLock and puts the reaction tube main body into a quartz tube for the growth of a new furnace;
s4, automatically calibrating the temperature of the optical temperature by a standard temperature generator bound on the manipulator before growth;
s5, after a new furnace starts to grow, an operator takes out an epitaxial wafer from the discharging LoadLock, and disassembles the main body of the reaction tube, wherein the main body comprises all heat insulation tubes, silicon source tubes and carbon source tubes, and the main body is mechanically cleaned piece by piece; then cleaning the nonmetallic high-temperature resistant insulating part in the whole reaction tube main body at a vacuum high temperature outside the furnace;
s6, after cleaning, reloading a new substrate, and feeding the new substrate into a feeding LoadLock for standby; the manipulator moves in the stainless steel inert gas chamber to automatically finish various operations.
2. A cylindrical symmetrical multichip silicon carbide epitaxial growth reaction tube according to claim 1, wherein: the graphite barrel consists of a slide glass barrel, an upper graphite barrel and a lower graphite barrel, and n is uniformly cut out from the surface of the slide glass barrel 1 A plurality of planes, each plane can be provided with n 2 A sheet substrate, such that n can be grown at a time 1 *n 2 And (3) a SiC epitaxial wafer.
3. A cylindrical symmetrical multichip silicon carbide epitaxial growth reaction tube according to claim 1, wherein: the outer surface parts of the heat insulating pipes are ground or embedded with each other to enhance the heat insulating effect and reduce the deposition on the inner surface of the quartz pipe.
4. A cylindrical symmetrical multichip silicon carbide epitaxial growth reaction tube according to claim 1, wherein: the temperature measuring and protecting tube is used for inflating and protecting the transparent light guide column in the temperature measuring and protecting tube, and the optical signals from the light guide column are subjected to optical temperature measurement and become electrical signals, and finally are used for temperature measurement and temperature control; when measuring temperature, in order to eliminate the influence of optical surface deposition on measurement, dual-wavelength temperature measurement is used; the standard temperature generator bound on the manipulator is formed by simulating blackbody radiation by an infrared light-emitting diode, is used for automatically correcting the temperature of each furnace, adopts self battery power supply, and is carried to a set position by means of the manipulator to automatically correct the optical measurement before growth.
5. A cylindrical symmetrical multichip silicon carbide epitaxial growth reaction tube according to claim 1, wherein: a barrel-shaped heat insulation lining is additionally arranged between the heat insulation pipe and the quartz pipe and is used for reducing the deposition of reactants on the quartz pipe.
6. A cylindrical symmetrical multichip silicon carbide epitaxial growth reaction tube according to claim 1, wherein: the device also comprises a laser interference film thickness on-line monitor, which monitors the growth condition of the SiC film on the sapphire template on line through the quartz tube, thereby monitoring the growth condition of the epitaxial layer on the silicon carbide substrate.
7. A cylindrical symmetrical multichip silicon carbide epitaxial growth reaction tube according to claim 1, wherein: 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 type of the flowing gas of the shielding gas, the reaction source and the carrier gas of the heat insulation pipe is adjusted.
CN202010678954.3A 2020-07-15 2020-07-15 Barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure Active CN111826718B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010678954.3A CN111826718B (en) 2020-07-15 2020-07-15 Barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010678954.3A CN111826718B (en) 2020-07-15 2020-07-15 Barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure

Publications (2)

Publication Number Publication Date
CN111826718A CN111826718A (en) 2020-10-27
CN111826718B true CN111826718B (en) 2023-06-27

Family

ID=72923264

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010678954.3A Active CN111826718B (en) 2020-07-15 2020-07-15 Barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure

Country Status (1)

Country Link
CN (1) CN111826718B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6214662B1 (en) * 2000-07-03 2001-04-10 Taiwan Semiconductor Manufacturing Company Forming self-align source line for memory array
CN101265570A (en) * 2008-04-30 2008-09-17 苏州纳晶光电有限公司 High-temperature metal organic chemical gas-phase deposition reactor
CN102094185A (en) * 2011-01-27 2011-06-15 方文卿 Barrel-shaped metal organic chemical vapor deposition reaction tube
JP2011195346A (en) * 2010-03-17 2011-10-06 Nuflare Technology Inc Film forming apparatus and film forming method
CN103540914A (en) * 2013-09-24 2014-01-29 中国科学院苏州纳米技术与纳米仿生研究所 Bucket-type CVD (chemical vapor deposition) equipment reaction chamber using radio-frequency heating

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6214662B1 (en) * 2000-07-03 2001-04-10 Taiwan Semiconductor Manufacturing Company Forming self-align source line for memory array
CN101265570A (en) * 2008-04-30 2008-09-17 苏州纳晶光电有限公司 High-temperature metal organic chemical gas-phase deposition reactor
JP2011195346A (en) * 2010-03-17 2011-10-06 Nuflare Technology Inc Film forming apparatus and film forming method
CN102094185A (en) * 2011-01-27 2011-06-15 方文卿 Barrel-shaped metal organic chemical vapor deposition reaction tube
CN103540914A (en) * 2013-09-24 2014-01-29 中国科学院苏州纳米技术与纳米仿生研究所 Bucket-type CVD (chemical vapor deposition) equipment reaction chamber using radio-frequency heating

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
MOCVD 外延生长原位光致发光谱测量方法;方文卿等;《人工晶体学报》;第第47卷卷(第第11期期);第2316-2321页 *

Also Published As

Publication number Publication date
CN111826718A (en) 2020-10-27

Similar Documents

Publication Publication Date Title
US8293014B2 (en) Substrate processing apparatus and reaction tube for processing substrate
WO2011114858A1 (en) Semiconductor thin-film manufacturing method, seminconductor thin-film manufacturing apparatus, susceptor, and susceptor holding tool
US9194056B2 (en) Film-forming apparatus and method
JP2012054528A (en) Semiconductor manufacturing apparatus
KR101458195B1 (en) Batch Type Apparatus For Forming Epitaxial Layer And Method For The Same
CN113604873B (en) Vapor phase epitaxy system and maintenance operation method thereof
JP5542560B2 (en) Semiconductor manufacturing apparatus and susceptor cleaning method
US20100282166A1 (en) Heat treatment apparatus and method of heat treatment
CN113737154A (en) Growth chamber of epitaxial equipment
JP2002158175A (en) Chemical vapor deposition system and method for growing semiconductor film
US6800136B2 (en) Axial gradient transport apparatus and process
CN111826718B (en) Barrel-shaped symmetrical multi-piece silicon carbide epitaxial growth reaction tube structure
CN212375420U (en) Novel barrel-shaped symmetrical multi-disc silicon carbide epitaxial growth reaction tube structure
CN113604874B (en) Vapor phase epitaxy system and maintenance operation method thereof
CN109075040B (en) Film forming apparatus
JPH08236463A (en) Barrel type vapor growth device
CN113604875B (en) Vapor phase epitaxy system and maintenance operation method thereof
JP2013115281A (en) Vapor phase growth apparatus
JP5535955B2 (en) Vapor growth equipment
WO2024045822A1 (en) Temperature control component and cvd reaction device
JPS60152675A (en) Vertical diffusion furnace type vapor growth device
KR102652637B1 (en) Film formation method and film formation equipment
CN114197037B (en) Vapor phase epitaxial growth device
JP2012019081A (en) Substrate treatment apparatus, semiconductor device manufacturing method and substrate manufacturing method
JPH08139028A (en) Vertical vapor growth equipment

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant