CN111663119A - TM022 mode microwave plasma reactor suitable for MPCVD - Google Patents

TM022 mode microwave plasma reactor suitable for MPCVD Download PDF

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Publication number
CN111663119A
CN111663119A CN202010616434.XA CN202010616434A CN111663119A CN 111663119 A CN111663119 A CN 111663119A CN 202010616434 A CN202010616434 A CN 202010616434A CN 111663119 A CN111663119 A CN 111663119A
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China
Prior art keywords
molybdenum
tray
mpcvd
molybdenum tray
microwave plasma
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Pending
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CN202010616434.XA
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Chinese (zh)
Inventor
袁博
刘虎
陈实
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Sichuan Sanzero Semiconductor Co ltd
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Sichuan Sanzero Semiconductor Co ltd
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Priority to CN202010616434.XA priority Critical patent/CN111663119A/en
Publication of CN111663119A publication Critical patent/CN111663119A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/511—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using microwave discharges
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
    • C23C16/274—Diamond only using microwave discharges
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/458—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
    • C23C16/4582—Rigid and flat substrates, e.g. plates or discs
    • C23C16/4583—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally
    • C23C16/4586—Elements in the interior of the support, e.g. electrodes, heating or cooling devices
    • 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
    • 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
    • C30B29/02—Elements
    • C30B29/04—Diamond

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

Abstract

The invention relates to the technical field of microwave plasma reactors, in particular to a TM022 mode microwave plasma reactor suitable for MPCVD (Multi-phase plasma deposition), which is used for solving the problem that flat plasma cannot be generated on a molybdenum tray in the reactor in the prior art, so that the growth efficiency of diamond crystals or a coating film is reduced. The reaction chamber comprises a reaction chamber body and a coaxial feed-in, wherein a molybdenum tray is arranged in the reaction chamber body, a water cooling table is arranged on the top surface of a quartz sealing window, the molybdenum tray is arranged on the top surface of the water cooling table, a channel communicated with the coaxial feed-in is arranged in the water cooling table, a pit communicated with the channel and positioned on the bottom surface of the molybdenum tray is further formed in the top surface of the water cooling table, and a through hole communicated with the pit is further formed in the edge of the molybdenum tray. Under the combined action of the microwave high-intensity field and the temperature field, a high folded electric field area which is distributed flatly is obtained in the reactor, so that a flat plasma is obtained, and the growth efficiency of the diamond crystal is improved.

Description

TM022 mode microwave plasma reactor suitable for MPCVD
Technical Field
The invention relates to the technical field of microwave plasma reactors, in particular to a TM022 mode microwave plasma reactor suitable for MPCVD.
Background
The unique properties of CVD diamond make it an ideal choice for high power electronics, and in order to achieve industrial application of CVD diamond, excellent control of film purity, very low defect content and sufficiently fast growth rate must be achieved simultaneously. Currently, microwave plasma-assisted chemical vapor deposition (MPCVD) processes that utilize only a resonant cavity system can provide sufficient atomic hydrogen to meet these requirements, and in order to increase the diamond growth rate, plasmas with sufficiently high microwave power density must be provided to provide atomic hydrogen, while plasmas also need to be more uniformly distributed over as large an area as possible to increase the area of a single CVD diamond growth, thereby increasing the growth number of diamonds.
In the prior art, the generation of plasmas needs to generate a quite high electric field on a flat area in a reactor, the reactor comprises a reaction cavity, a molybdenum tray is arranged in the reaction cavity and coaxially fed and extended into the reaction cavity, the growth of diamond crystals is distributed on the plane of the molybdenum tray, if the plasma discharge is spherical or cylindrical, the area intersected with the crystal tray is smaller, the number of atomic hydrogen at the edge of the tray is insufficient, the surface temperature of the tray is uneven, and then diamond can be grown only in a small area in the center. If the plasma is flat, the intersecting area of the plasma and the surface of the tray is as large as possible when the microwave power, the power density and the plasma discharge volume are the same, so that the growth efficiency of diamond crystals on the molybdenum tray can be improved.
The spatial distribution of the plasma discharge fireball is related to the spatial distribution of the folded electric field, and in order to make the plasma discharge fireball as flat as possible at a certain microwave power and microwave power density, a flatter folded electric field spatial distribution should be generated by the microwave plasma reactor. According to the folded electric field E/n ═ E ═ R ═ T)/P, the folded electric field is a constant value of P and a constant of R, the folded electric field at a certain point in the space is positively correlated with the temperature and the electric field intensity at the point, so that a relatively flat high electric field intensity area and a flat high temperature area are generated in the space, and the flat folded electric field spatial distribution can be obtained.
In the reactor in the prior art, the area of the process gas flowing through the surface of the molybdenum tray is small, so that the edge of the molybdenum tray cannot be heated, and therefore, a flat high-temperature area cannot be generated on the molybdenum tray, a flat folded electric field cannot be obtained, a flat plasma cannot be obtained, the number of single diamond crystal growth is finally caused, and the growth efficiency of diamond crystals is influenced. Therefore, there is a strong need for an MPCVD reactor that allows for a greater area of process gas flow over the surface of the molybdenum trays, and that produces a flat high temperature zone, thereby allowing for the growth of more diamond crystals at one time.
Disclosure of Invention
Based on the above problems, the present invention aims to: the TM022 mode microwave plasma reactor suitable for MPCVD is provided for solving the problems that the area of the surface of a molybdenum tray, which is flowed by process gas in the reactor in the prior art, is small, the edge of the molybdenum tray can not be heated, and a flat high-temperature area can not be generated on the molybdenum tray, so that flat plasma can not be generated, and further the growth efficiency of diamond crystals or a coating film is reduced.
The invention specifically adopts the following technical scheme for realizing the purpose:
the utility model provides a TM022 mode microwave plasma reactor suitable for MPCVD, includes reaction cavity and coaxial feed-in, install the molybdenum tray in the reaction cavity, still install quartz seal window in the reaction cavity, the water-cooling platform is installed to the top surface of quartz seal window, the top surface at the water-cooling platform is installed to the molybdenum tray, it has the passageway with coaxial feed-in intercommunication to open in the water-cooling platform, the top surface of water-cooling platform still opens the pit that just is located molybdenum tray bottom surface with the passageway intercommunication, the edge of molybdenum tray still opens the through-hole that has and pit intercommunication.
Preferably, the through holes are round holes, waist holes or arc-shaped array holes.
Preferably, the inner surface of the pit is uniformly provided with a plurality of heat conducting fins.
As a preferable mode, the edge of the pit is further provided with a step, and the molybdenum tray is mounted on the step.
As a preferable mode, an observation window is arranged on the reaction cavity.
Preferably, the upper portion of the coaxial feed is tapered and gradually increases in diameter.
As a preferred mode, TM022 mode resonance occurs within the reaction chamber.
The invention has the following beneficial effects:
(1) the microwave enters the pit through the channel from the coaxial feed-in, the pit is positioned at the lower part of the molybdenum tray, and the microwave in the pit enters the reaction cavity through the through hole at the edge of the molybdenum tray, so that the temperature of the surface of the molybdenum tray is basically uniform, and the edge of the molybdenum tray can be heated, so that a large-area high-temperature boundary can be formed below the plasma discharge fireball, a flat distribution high-folding electric field area can be obtained on the molybdenum tray, flat plasma can be obtained on the molybdenum tray, and finally the growth quantity of diamond crystals in one time can be improved.
(2) According to the invention, through reasonably designing the shape of the molybdenum tray, the molybdenum tray can reach thermal balance near 1000 ℃, namely, the heat flux transmitted into the molybdenum tray by the plasma is equal to the heat flux transmitted into the water cooling table by the molybdenum tray, so that a good thermal environment can be formed on the molybdenum tray, and the growth efficiency of diamond crystals is improved.
(3) According to the invention, the plurality of heat conduction fins are uniformly arranged on the inner surface of the pit, the heat conduction fins can form a good heat conduction environment in the pit, and a heat source for continuously heating the molybdenum tray is formed in the pit, so that the temperature on the surface of the molybdenum tray is basically constant.
(4) The upper part of the coaxial feed-in part is conical, and the diameter of the coaxial feed-in part is gradually increased, so that the microwave reaching the bottom surface of the molybdenum tray from the coaxial feed-in part is more uniform, and a uniformly distributed high folding electric field is formed on the molybdenum tray.
(5) The gas passage formed by the through holes can effectively discharge the process gas from the edge of the molybdenum tray, and improves the flow field distribution in the reactor, thereby improving the growth efficiency of the diamond film and the single crystal diamond.
(6) In the invention, TM022 mode resonance occurs in the reaction cavity, a flat microwave high field intensity region can be generated above the molybdenum tray by the TM022 mode microwave reactor, and a flat distributed high folding electric field region is obtained in the reactor under the combined action of the microwave high field intensity region and the temperature field, so that flat plasma is obtained, and finally, the growth quantity of single diamond crystals is improved, thereby improving the growth efficiency of the diamond crystals.
(7) The TM022 resonant mode reaction cavity has larger volume, the plasma discharge area is far away from the wall of the reactor, the heating condition of high-temperature plasma on the wall of the container is improved, and the pollution problem of the wall of the container to process gas is also improved.
(8) In the invention, the microwave is fed in from the bottom of the reactor through coaxial feeding, and finally, a high-field-intensity area is concentrated on a water-cooling platform in the center of the reactor. Therefore, the plasma can be far away from the observation window, the atmosphere pollution and overheating of the observation window caused by the observation window are avoided, and the power capacity of the reactor is further improved.
Drawings
FIG. 1 is a schematic front sectional view of the present invention;
FIG. 2 is a schematic diagram of the front sectional view of the coaxial feed-in and water-cooling table and molybdenum tray installation of the present invention;
FIG. 3 is a schematic top view of the copper tray and molybdenum tray of the present invention when they are mounted together;
FIG. 4 is a schematic perspective view of a molybdenum pallet of the present invention;
FIG. 5 is a schematic three-dimensional structure of the red copper tray of the present invention;
FIG. 6 is a schematic sectional front view of a water cooling table according to the present invention;
reference numerals: the device comprises a coaxial feed-in device 1, a quartz sealing window 2, a reaction cavity 3, a water cooling table 4, a step 41, a pit 42, a channel 43, a molybdenum tray 5, a through hole 51, an observation window 6 and a heat conduction fin 7.
Detailed Description
For a better understanding of the present invention by those skilled in the art, the present invention will be described in further detail below with reference to the accompanying drawings and the following examples.
Example (b):
as shown in fig. 1-6, a TM022 mode microwave plasma reactor suitable for MPCVD comprises a reaction chamber 3 and a coaxial feed-in 1, a molybdenum tray 5 is installed in the reaction chamber 3, a quartz sealing window 2 is also installed in the reaction chamber 3, a water cooling table 4 is installed on the top surface of the quartz sealing window 2, the molybdenum tray 5 is installed on the top surface of the water cooling table 4, a channel 43 communicated with the coaxial feed-in 1 is opened in the water cooling table 4, a pit 42 communicated with the channel 43 and located on the bottom surface of the molybdenum tray 5 is also opened on the top surface of the water cooling table 4, and a through hole 51 communicated with the pit 42 is also opened on the edge of the molybdenum tray 5.
The working principle is as follows: the microwave enters the pit 42 from the coaxial feed-in 1 through the channel 43, the pit 42 is positioned at the lower part of the molybdenum tray 5, the microwave in the pit 42 enters the reaction cavity 3 through the through hole 51 at the edge of the molybdenum tray 5, the molybdenum tray 5 has enough thickness to improve the heat capacity, the quartz sealing window 2 is used for sealing and isolating, so that the upper part of the reactor is kept in vacuum, the temperature of the surface of the molybdenum tray 5 is basically uniform, the edge of the molybdenum tray 5 can also be heated, the high-temperature area of the surface of the molybdenum tray 5 is larger, the temperature is more uniform, a large-area high-temperature boundary can be formed below a plasma discharge fireball, a flat distribution high-folding electric field area can be obtained on the molybdenum tray 5, flat plasma can be obtained on the molybdenum tray 5, and finally the growth quantity of diamond crystals in one time can be improved.
Preferably, the through holes 51 are circular hole type or waist hole type or arc array holes, and the through holes 51 with various shapes can be arranged in a staggered manner, so that the heat flux of the molybdenum pallet 5 can be further improved, the temperature field on the surface of the molybdenum pallet 5 is more uniform, and flat plasma is favorably generated.
Preferably, a plurality of heat conducting fins 7 are uniformly arranged on the inner surface of the pit 42, a step 41 is further arranged on the edge of the pit 42, the molybdenum tray 5 is mounted on the step 41, the heat conducting fins 7 can form a good heat conducting environment in the pit 42, and a heat source for continuously heating the molybdenum tray 5 is formed in the pit 42, so that the temperature of the surface of the molybdenum tray 5 can be substantially constant.
Preferably, the reaction chamber 3 is provided with an observation window 6, and the growth of diamond crystals on the molybdenum tray 5 can be observed through the observation window 6. The upper part of the coaxial feed-in 1 is tapered and gradually increases in diameter, so that the microwaves arriving from the coaxial feed-in 1 to the bottom surface of the molybdenum pallet 5 are more uniform, thereby facilitating the formation of a uniformly distributed high folded electric field on the molybdenum pallet 5.
TM022 mode resonance occurs within the reaction chamber 3, and TM022 mode resonance is selected for the following reasons: since the size of the microwave high-field intensity region of the TM01 × equal resonance mode is small, but the high-field intensity region of the resonant cavity is limited by the wavelength of the microwave and cannot be amplified infinitely, the TM03x resonance mode causes the resonant cavity of the reactor to be oversized and difficult to process, so the TM02x mode is selected as the main resonance mode of the reactor.
Further, since the MPCVD apparatus is operated normally, the gas filled in the reactor is mostly hydrogen, the gas thermal conductivity is high, in order to avoid microwave energy loss caused by excessive heating of the reactor wall, it is necessary to make the plasma zone far from the reactor wall, but not to make the reactor volume too large, so in TM02x, TM022 mode is selected to design the microwave reactor. The TM022 mode microwave reactor can generate a relatively flat microwave high field intensity region above the molybdenum tray 5, and a high folded electric field area which is distributed flatly is obtained in the reactor under the combined action of the microwave high field and the temperature field, so that flat plasma is obtained, the number of single diamond crystal growth is finally increased, and the growth efficiency of the diamond crystal is further improved.
The above is an embodiment of the present invention. The embodiments and specific parameters in the embodiments are only for the purpose of clearly illustrating the verification process of the invention and are not intended to limit the scope of the invention, which is defined by the claims, and all equivalent structural changes made by using the contents of the specification and the drawings of the present invention should be covered by the scope of the present invention.

Claims (7)

1. A TM022 mode microwave plasma reactor suitable for MPCVD, comprising a reaction chamber (3) and a coaxial feed-through (1), a molybdenum tray (5) being installed inside the reaction chamber (3), characterized in that: still install quartzy sealed window (2) in reaction cavity (3), water-cooling platform (4) are installed to the top surface of quartzy sealed window (2), the top surface at water-cooling platform (4) is installed in molybdenum tray (5), it has passageway (43) with coaxial feed-in (1) intercommunication to open in water-cooling platform (4), the pit (42) that just are located molybdenum tray (5) bottom surface with passageway (43) intercommunication are still opened to the top surface of water-cooling platform (4), the edge of molybdenum tray (5) still opens through-hole (51) with pit (42) intercommunication.
2. A TM022 mode microwave plasma reactor suitable for MPCVD according to claim 1, characterized in that: the through holes (51) are round hole type or waist hole type or arc array holes.
3. A TM022 mode microwave plasma reactor suitable for MPCVD according to claim 1, characterized in that: the inner surface of the concave pit (42) is uniformly provided with a plurality of heat conduction fins (7).
4. A TM022 mode microwave plasma reactor suitable for MPCVD according to claim 1, characterized in that: the edge of the pit (42) is also provided with a step (41), and the molybdenum tray (5) is arranged on the step (41).
5. A TM022 mode microwave plasma reactor suitable for MPCVD according to claim 1, characterized in that: an observation window (6) is arranged on the reaction cavity (3).
6. A TM022 mode microwave plasma reactor suitable for MPCVD according to claim 1, characterized in that: the upper part of the coaxial feed-in (1) is conical and gradually increases in diameter.
7. A TM022 mode microwave plasma reactor suitable for MPCVD according to any of claims 1-6, wherein: TM022 mode resonance occurs in the reaction cavity (3).
CN202010616434.XA 2020-06-30 2020-06-30 TM022 mode microwave plasma reactor suitable for MPCVD Pending CN111663119A (en)

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CN202010616434.XA CN111663119A (en) 2020-06-30 2020-06-30 TM022 mode microwave plasma reactor suitable for MPCVD

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112647126A (en) * 2020-12-02 2021-04-13 哈尔滨工业大学 Embedded water cooling table for large-particle MPCVD single crystal diamond temperature-control continuous growth and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112647126A (en) * 2020-12-02 2021-04-13 哈尔滨工业大学 Embedded water cooling table for large-particle MPCVD single crystal diamond temperature-control continuous growth and application thereof

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Application publication date: 20200915