CN115161763B - Microwave plasma chemical vapor deposition device - Google Patents
Microwave plasma chemical vapor deposition device Download PDFInfo
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- CN115161763B CN115161763B CN202210901764.2A CN202210901764A CN115161763B CN 115161763 B CN115161763 B CN 115161763B CN 202210901764 A CN202210901764 A CN 202210901764A CN 115161763 B CN115161763 B CN 115161763B
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- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 15
- 238000000151 deposition Methods 0.000 claims abstract description 63
- 230000008021 deposition Effects 0.000 claims abstract description 59
- 238000007789 sealing Methods 0.000 claims abstract description 56
- 239000004020 conductor Substances 0.000 claims abstract description 30
- 239000010453 quartz Substances 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 230000005540 biological transmission Effects 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000005530 etching Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 238000001816 cooling Methods 0.000 claims description 27
- 239000000498 cooling water Substances 0.000 claims description 27
- 230000007246 mechanism Effects 0.000 claims description 21
- 239000011229 interlayer Substances 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 4
- 239000003566 sealing material Substances 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 15
- 239000010432 diamond Substances 0.000 description 13
- 229910003460 diamond Inorganic materials 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000003028 elevating effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000009191 jumping Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical class [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/3244—Gas supply means
- H01J37/32449—Gas control, e.g. control of the gas flow
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32715—Workpiece holder
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
Abstract
The invention discloses a microwave plasma chemical vapor deposition device, which comprises a multi-medium transmission structure, wherein the multi-medium transmission structure comprises a microwave conversion assembly, an antenna terminal assembly connected with the microwave conversion assembly and a deposition furnace assembly connected with the antenna terminal assembly, and a lifting type sample platform assembly is arranged in the deposition furnace assembly; the microwave conversion assembly comprises a rectangular waveguide, a three-pin adapter arranged on the rectangular waveguide and a microwave mode converter arranged on the rectangular waveguide, wherein the microwave mode converter is used for converting TE10 modes in the rectangular waveguide into TEM modes in the coaxial waveguide; the antenna terminal assembly comprises a first connecting piece, an inner conductor, an upper cover body, a disc antenna and a lower flange plate; the two ends of the first connecting piece are respectively connected with the rectangular waveguide and the upper cover body, and the upper end of the inner conductor is connected with the microwave mode converter. The invention solves the technical problem that the quartz sealing ring window is polluted by etching in the production process in the existing device.
Description
Technical Field
The invention relates to the technical field of plasma chemical vapor deposition, in particular to a microwave plasma chemical vapor deposition device.
Background
The artificial diamond is industrially applied to cutting, grinding and drilling, can be used as a radiating plate of a semiconductor device due to high heat conductivity and good electrical insulation, has excellent light transmittance and corrosion resistance, is widely applied to optical windows and electronic industries, and meanwhile, the preparation of the diamond at the precious stone level is a research direction of being hot in recent years.
The Microwave Plasma Chemical Vapor Deposition (MPCVD) single crystal diamond growth technology is one of the most promising technologies for preparing large-size and high-quality single crystal diamond because of the advantages of no pollution of microwave energy, pure gas raw materials and the like.
Currently, microwave plasma CVD is considered to be an ideal method of depositing diamond. The principle is as follows: under the action of microwave energy, the deposition gas is excited into a plasma state, electrons in the cavity collide with each other and generate intense oscillation under the action of an electromagnetic field generated by microwaves, and the mutual collision among other atoms, groups and molecules in the resonant cavity is promoted, so that the ionization degree of the reaction gas is effectively improved, and the generation of plasma with higher density is generated. In the reaction process, the ionization degree of the raw material gas reaches more than 10 percent, so that the cavity is filled with supersaturated atomic hydrogen and carbon-containing groups, thereby effectively improving the deposition rate and improving the deposition quality of the diamond.
In the diamond produced by MPCVD, the main impurity elements present are nitrogen and silicon, wherein nitrogen impurities come from equipment leakage, raw material gas impurities, or nitrogen atoms adsorbed by the wall, etc., and silicon elements come from etching of quartz windows by plasma. However, in the existing MPCVD device, a quartz sealing ring window is polluted by etching in the production process, and the deposition efficiency is low due to microwave energy dispersion; meanwhile, the adjusting device is too redundant, plasma jumping up and down occurs when the sample table is adjusted, and the utilization rate of raw gas is not high; the problem of low diamond yield caused by uneven heat dissipation of the deposition table.
Disclosure of Invention
The invention aims to provide a microwave plasma chemical vapor deposition device which solves the technical problem that a quartz sealing ring window is polluted by etching in the production process in the existing device.
In order to solve the technical problems, the invention adopts the following technical scheme:
the microwave plasma chemical vapor deposition device comprises a multi-medium transmission structure, wherein the multi-medium transmission structure comprises a microwave conversion assembly, an antenna terminal assembly connected with the microwave conversion assembly and a deposition furnace assembly connected with the antenna terminal assembly, and a lifting sample platform assembly is arranged in the deposition furnace assembly;
the microwave conversion assembly comprises a rectangular waveguide, a three-pin adapter arranged on the rectangular waveguide and a microwave mode converter arranged on the rectangular waveguide, wherein the microwave mode converter is used for converting TE10 modes in the rectangular waveguide into TEM modes in the coaxial waveguide;
the antenna terminal assembly comprises a first connecting piece, an inner conductor, an upper cover body, a disc antenna and a lower flange plate; the two ends of the first connecting piece are respectively connected with the rectangular waveguide and the upper cover body, the upper end of the inner conductor is connected with the microwave mode converter, an air channel is formed in the inner conductor, and a microwave channel is formed between the inner conductor and the first connecting piece; the inner conductor is fixedly connected with the disc antenna, the disc antenna is connected with the upper cover body through a supporting column, an annular air gathering groove communicated with the air channel is formed in the disc antenna, a first sealing groove is formed in the disc antenna, a second sealing groove is formed in the lower flange, a quartz sealing ring window is arranged between the disc antenna and the lower flange, the upper end and the lower end of the quartz sealing ring window are respectively located in the first sealing groove and the second sealing groove, and soft sealing materials are arranged in the first sealing groove and the second sealing groove; the lower flange plate is connected with the upper cover body and then fixes the quartz sealing ring window;
the deposition furnace component is connected with the lower flange plate, and the lifting sample platform component is installed in the deposition furnace component in a sliding and sealing manner.
The microwave mode converter is a conical body made of copper or aluminum, the bottom edge of the conical body is tapped, the conical body is arranged in the rectangular waveguide, the upper end of the conical body is arranged at the opening of the upper end face of the rectangular waveguide, and the conical body is fixed through bolts; the middle part of the conical body is provided with a through hole, the upper end of the inner conductor is arranged in the through hole, a water cooling cavity is arranged in the conical body, and the cooling water inlet and the cooling water outlet are both positioned on the outer side of the upper end face of the rectangular waveguide and are communicated with the water cooling cavity.
Further preferably, the middle part of the first connecting piece is an outer conductor, and a first water cooling interlayer for cooling water to flow is arranged on the outer side of the outer conductor.
Wherein, the outer side of the upper cover body of the sample platform is provided with a second cooling interlayer for cooling water to flow.
Further optimized, the deposition furnace assembly comprises an inner cavity plate, a connecting plate and a vacuum cavity tube, wherein two ends of the inner cavity plate are respectively connected with the connecting plate and the lower flange plate, a shell is arranged on the outer side of the inner cavity plate, and a third water-cooling interlayer for cooling water to flow is formed between the shell and the inner cavity plate; the vacuum cavity pipe is connected with the connecting plate and is communicated with the area above the connecting plate, and the lower end of the vacuum cavity is connected with the vacuum flange; the lifting sample platform component is arranged on the vacuum cavity tube, the upper end of the lifting sample platform component extends into a deposition cavity formed by the inner cavity plate,
further limiting, namely a deposition cavity bottom plate of which the lifting type sample platform assembly is in an inverted conical structure, a bottom plate support column connected with the deposition cavity bottom plate, a sample platform support column arranged in the bottom plate support column in a sliding manner, and a sample platform assembly arranged on the sample platform support column, wherein a sealing ring is arranged between the bottom plate support column and the sample platform support column; the bottom plate of the deposition cavity is slidably arranged on the connecting plate through an upper guide ring, and the sample stage support column is connected with a first driving mechanism which is used for driving the sample stage support column to move in the bottom plate support column; the bottom plate support column is connected with a second driving mechanism, and the second driving mechanism is used for driving the bottom plate support column to move in the vacuum cavity tube and the deposition cavity.
The first driving mechanism comprises a corrugated pipe upper flange, a corrugated pipe lower flange, a corrugated pipe, a support, a screw rod nut and a motor, wherein the upper end of the corrugated pipe upper flange is connected with the vacuum flange, a bottom plate support column is connected with the corrugated pipe upper flange in a sliding mode through a second guide ring, the corrugated pipe upper flange is arranged on the support, the screw rod upper end is rotatably arranged on the corrugated pipe upper flange, the lower end is rotatably arranged on the support, the motor is arranged on the support and then connected with the screw rod, the screw rod nut is arranged on the screw rod, the lower end of the sample table support column is connected with the corrugated pipe lower flange through a sealing plug, the corrugated pipe lower flange is connected with the screw rod nut, and the corrugated pipe upper flange is connected with the corrugated pipe lower flange through the corrugated pipe.
Further limited, the second driving mechanism comprises a gear, a rack and a transmission shaft, wherein the rack is fixedly arranged on the bottom plate supporting column, the transmission shaft is used for being rotatably and hermetically arranged on the vacuum cavity tube, the gear is positioned in the vacuum cavity tube and meshed with the rack, and one end, far away from the gear, of the transmission shaft is connected with a driving motor.
The sample platform assembly comprises a platform column arranged above the sample platform supporting column and a sample platform upper cover arranged on the platform column; a positioning ring for placing a molybdenum support is arranged at the top of the upper cover of the sample table;
the bench post is provided with a mounting hole and a stepped through hole communicated with the mounting hole, a mounting area is formed between the mounting hole on the bench post and the upper cover of the sample bench, a waterway plate is arranged in the mounting area, a water inlet hole is arranged in the middle of the waterway plate, a plurality of first water tanks communicated with the water inlet hole are arranged at the top of the waterway plate, the lower end surface of the waterway plate is provided with a bulge corresponding to the stepped through hole, after the bulge on the waterway plate is matched with the bracket body through hole, the edge of the waterway plate and the edge of the mounting hole form a waterway, and the lower end surface of the waterway plate is provided with a plurality of second water tanks communicated with the waterway and the stepped through hole;
the lower end of the sample stage support column is provided with a plug, the water inlet hole is connected with a cooling water inlet pipe, the lower end of the cooling water inlet pipe penetrates through the plug, and the plug is provided with a cooling water outlet pipe.
Further optimized, the copper water-cooling coil is arranged on the outer side face of the bottom plate of the deposition cavity, and the water-cooling coil is arranged in a spiral rising mode.
The sealing ring is arranged in the dovetail groove.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the three-pin tuner is arranged together with the rectangular waveguide, and the microwave mode converter is arranged on the rectangular waveguide, so that an integrated structure of the three-pin tuner and the microwave mode converter is formed, the mode of the traditional mode converter matched with the sliding short-circuiting device is simplified, the microwave transmission index is ensured, the structure is simplified, the cost is saved, the redundant regulating mechanism is reduced, and the three-pin tuner is more friendly to non-professional people;
meanwhile, the air inlet structure is arranged on the inner conductor, the annular air gathering groove is arranged at the lower end of the disc antenna, so that the uniformity of air distribution on the sample growth table is improved, the waste of raw material air is reduced, and most of raw material air flows around the sample table; the quartz sealing ring window is positioned between the lower side of the disc antenna and the deposition cavity, so that the microwave strong electric field area is avoided, the problem of etching the quartz window by secondary plasma is avoided, and the quartz sealing ring window is determined by the relative position of the quartz sealing ring window and the disc antenna, so that the main flowing area of raw gas is avoided, and the problem of pollution etching is further avoided. Compared with the conventional TM01x mode, the device only has a strong electric field area above the sample stage, so that the problems of microwave energy dispersion and plasma ball up-down jumping in the sample stage adjusting process of the conventional device are solved, and the diamond deposition efficiency is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the overall structure of the present invention.
Fig. 2 is a schematic diagram of the overall structure of the microwave conversion assembly of the present invention.
Fig. 3 is a schematic view of the internal structure of fig. 2 according to the present invention.
Fig. 4 is a schematic diagram of the overall structure of the antenna terminal assembly of the present invention.
FIG. 5 is a schematic diagram of the overall structure of the deposition furnace assembly and the lift sample platform assembly of the present invention.
FIG. 6 is a schematic view of the overall structure of the elevating sample platform assembly according to the present invention.
FIG. 7 is a schematic diagram of the mating relationship of the sample stage support column and the floor support column of the present invention.
FIG. 8 is a schematic view of a waterway board according to the present invention.
FIG. 9 is a second schematic view of the waterway board of the present invention.
Fig. 10 is an enlarged schematic view of a portion of fig. 7 a in accordance with the present invention.
Reference numerals:
1-microwave conversion assembly: 101-rectangular waveguide, 102-three pin adapter, 103-microwave mode converter, 104-cone, 105-through hole, 106-first water-cooled interlayer;
2-antenna terminal assembly: 201-quartz sealing ring window, 202-first connecting piece, 203-inner conductor, 204-upper cover body, 205-disc antenna, 206-lower flange, 207-air channel, 208-microwave channel, 209-support column, 210-annular gas gathering groove, 211-first sealing groove, 212-second sealing groove, 213-second cooling interlayer;
3-deposition furnace assembly: 301-inner cavity plate, 302-connecting plate, 303-vacuum cavity tube, 304-outer shell, 305-third water-cooling interlayer, 306-deposition cavity;
4-lifting sample platform assembly: 401-deposition chamber bottom plate, 402-bottom plate support column, 403-sample stage support column, 404-sealing ring, 405-upper guide ring, 406-first driving mechanism, 407-bellows upper flange, 408-bellows lower flange, 409-bellows, 410-support, 411-lead screw, 412-lead screw nut, 413-motor, 414-second driving mechanism;
5-sample stage assembly: 501-table column, 502-sample table upper cover, 503-positioning ring, 504-mounting hole, 505-step through hole, 506-waterway plate, 507-water inlet, 508-first water tank, 509-bulge, 510-water cooling coil pipe, 511-second water tank, 512-plug, 513-cooling water inlet pipe, 514-cooling water outlet pipe, 515-cut-off observation window.
Detailed Description
Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in numerous different ways without departing from the spirit or scope of the embodiments of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive.
In the description of the embodiments of the present invention, it should be understood that the terms "length," "vertical," "horizontal," "top," "bottom," and the like indicate an orientation or a positional relationship based on that shown in the drawings, and are merely for convenience in describing the embodiments of the present invention and to simplify the description, rather than to indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the embodiments of the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the embodiments of the present invention, the meaning of "plurality" is two or more, unless explicitly defined otherwise.
In the embodiments of the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured" and the like are to be construed broadly and include, for example, either permanently connected, removably connected, or integrally formed; the device can be mechanically connected, electrically connected and communicated; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the embodiments of the present invention will be understood by those of ordinary skill in the art according to specific circumstances.
In embodiments of the invention, unless expressly stated or limited otherwise, a first feature "above" or "below" a second feature may include both the first and second features being in direct contact, or may include both the first and second features not being in direct contact but being in contact with each other through additional features therebetween. Moreover, a first feature being "above," "over" and "on" a second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is less level than the second feature.
The following disclosure provides many different implementations, or examples, for implementing different configurations of embodiments of the invention. In order to simplify the disclosure of embodiments of the present invention, components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit embodiments of the present invention. Furthermore, embodiments of the present invention may repeat reference numerals and/or letters in the various examples, which are for the purpose of brevity and clarity, and which do not themselves indicate the relationship between the various embodiments and/or arrangements discussed.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
Referring to fig. 1-10, the embodiment discloses a microwave plasma chemical vapor deposition device, which comprises a multi-medium transmission structure, wherein the multi-medium transmission structure comprises a microwave conversion assembly 1, an antenna terminal assembly 2 connected with the microwave conversion assembly 1, and a deposition furnace assembly 3 connected with the antenna terminal assembly 2, and a lifting sample platform assembly 4 is arranged in the deposition furnace assembly 3;
the microwave conversion assembly 1 comprises a rectangular waveguide 101, a three-pin adapter 102 mounted on the rectangular waveguide 101 and a microwave mode converter 103 mounted on the rectangular waveguide 101, wherein the microwave mode converter 103 is used for converting TE10 modes in the rectangular waveguide 101 into TEM modes in a coaxial waveguide;
the antenna terminal assembly 2 comprises a first connector 202, an inner conductor 203, an upper cover 204, a disc antenna 205 and a lower flange 206; the two ends of the first connecting piece 202 are respectively connected with the rectangular waveguide 101 and the upper cover 204, the upper end of the inner conductor 203 is connected with the microwave mode converter 103, an air channel 207 is arranged in the inner conductor 203, and a microwave channel 208 is formed between the inner conductor 203 and the first connecting piece 202; the inner conductor 203 is fixedly connected with the disc antenna 205, the disc antenna 205 is connected with the upper cover 204 through a supporting column 209, an annular gas collecting groove 210 communicated with the air channel 207 is arranged on the disc antenna 205, a first sealing groove 211 is arranged on the disc antenna 205, a second sealing groove 212 is arranged on the lower flange 206, a quartz sealing ring window 201 is arranged between the disc antenna 205 and the lower flange 206, the upper end and the lower end of the quartz sealing ring window 201 are respectively positioned in the first sealing groove and the second sealing groove, and soft sealing materials are arranged in the first sealing groove and the second sealing groove; the lower flange 206 is connected with the upper cover 204 to fix the quartz sealing ring window 201;
the deposition furnace assembly 3 is connected to the lower flange 206 and the elevating sample platform assembly 4 is slidably and sealingly mounted within the deposition furnace assembly 3.
The microwave mode converter 103 is a conical body 104 made of copper or aluminum, the bottom edge of the conical body 104 is tapped, the conical body 104 is installed in the rectangular waveguide 101, the upper end of the conical body is installed at an opening of the upper end face of the rectangular waveguide 101, and the conical body is fixed through bolts; the middle part of the conical body 104 is provided with a through hole 105, the upper end of the inner conductor 203 is arranged in the through hole 105, the inside of the conical body 104 is provided with a water cooling cavity, and the cooling water inlet and the cooling water outlet are both positioned outside the upper end face of the rectangular waveguide 101 and are communicated with the water cooling cavity.
The middle part of the first connecting piece 202 is an outer conductor, and a first water cooling interlayer 106 for cooling water to flow is arranged outside the outer conductor.
Further preferably, a second cooling interlayer 213 for flowing cooling water is arranged outside the upper cover 204 of the sample stage.
The deposition furnace assembly 3 comprises an inner cavity plate 301, a connecting plate 302 and a vacuum cavity tube 303, wherein two ends of the inner cavity plate 301 are respectively connected with the connecting plate 302 and the lower flange 206, a shell 304 is arranged on the outer side of the inner cavity plate 301, and a third water-cooling interlayer 305 for cooling water to flow is formed between the shell 304 and the inner cavity plate 301; the vacuum cavity tube 303 is connected with the connecting plate 302 and is communicated with the area above the connecting plate 302, and the lower end of the vacuum cavity is connected with the vacuum flange; the elevating sample platform assembly 4 is mounted on the vacuum chamber tube 303 with its upper end extending into the deposition chamber 306 formed by the inner chamber plate 301,
further optimizing, the lifting type sample platform assembly 4 is a deposition cavity bottom plate 401 with an inverted cone structure, a bottom plate support column 402 connected with the deposition cavity bottom plate 401, a sample platform support column 403 arranged in the bottom plate support column 402 in a sliding manner, a sample platform assembly 5 arranged on the sample platform support column 403, and a sealing ring 404 is arranged between the bottom plate support column 402 and the sample platform support column 403; the deposition chamber bottom plate 401 is slidably mounted on the connection plate 302 through an upper guide ring 405, and the sample stage support column 403 is connected with a first driving mechanism 406, and the first driving mechanism 406 is used for driving the sample stage support column to move in the bottom plate support column 402; the floor support columns 402 are coupled to a second drive mechanism 414, the second drive mechanism 414 being used to drive the floor support columns 402 within the vacuum chamber tube 303 and the deposition chamber 306.
The first driving mechanism 406 comprises a bellows upper flange 407, a bellows lower flange 408, a bellows 409, a support 410, a screw 411, a screw nut 412 and a motor 413, wherein the upper end of the bellows upper flange 407 is connected with the vacuum flange, the bottom plate support column 402 is in sliding connection with the bellows upper flange 407 through a second guide ring, the bellows upper flange 407 is installed on the support 410, the upper end of the screw 411 is rotatably installed on the bellows upper flange 407, the lower end of the screw 411 is rotatably installed on the support 410, the motor 413 is installed on the support 410 and then is connected with the screw 411, the screw nut 412 is installed on the screw 411, the lower end of the sample stage support column 403 is connected with the bellows lower flange 408 through a sealing plug 512, the bellows lower flange 408 is connected with the screw nut 412, and the bellows upper flange 407 is connected with the bellows lower flange 408 through the bellows 409.
The second driving mechanism 414 includes a gear, a rack, and a driving shaft, the rack is fixedly installed on the bottom plate support column 402, the driving shaft is used for rotating and sealing and installed on the vacuum chamber 303, the gear is located in the vacuum chamber 303 and meshed with the rack, and one end, far away from the gear, of the driving shaft is connected with the driving motor 413.
Further preferably, the sample stage assembly 5 comprises a stage post 501 mounted above the sample stage support post 403, and a sample stage upper cover 502 mounted on the stage post 501; a positioning ring 503 for placing a molybdenum support is arranged on the top of the upper cover 502 of the sample table;
the bench post 501 is provided with a mounting hole 504 and a stepped through hole 505 communicated with the mounting hole 504, a mounting area is formed between the mounting hole 504 on the bench post 501 and the upper cover 502 of the sample bench, a waterway plate 506 is arranged in the mounting area, a water inlet 507 is arranged in the middle of the waterway plate 506, a plurality of first water tanks 508 communicated with the water inlet 507 are arranged at the top of the waterway plate, protrusions 509 corresponding to the stepped through hole 505 are arranged on the lower end surface of the waterway plate 506, after the protrusions 509 on the waterway plate 506 are matched with the through holes 105 of the frame body, a waterway is formed between the edge of the waterway plate 506 and the edge of the mounting hole 504, and a plurality of second water tanks 511 communicated with the waterway and the stepped through holes 505 are arranged on the lower end surface of the waterway plate 506;
the lower extreme of sample platform support column 403 is provided with end cap 512, and inlet port 507 is connected with cooling water inlet tube 513, and cooling water inlet tube 513 lower extreme passes end cap 512, is provided with cooling water outlet pipe 514 on the end cap 512.
The copper water-cooling coil 510 is disposed on the outer side surface of the deposition chamber bottom plate 401, and the water-cooling coil 510 is spirally rising.
Further preferably, a dovetail groove is formed in one surface, which is contacted with the sample stage support column 403, of the bottom plate support column 402, and a sealing ring 404 is arranged in the dovetail groove.
The present invention is further described below in order to facilitate a further understanding of the present invention by those skilled in the art.
The three-pin adapter 102 and the microwave mode converter 103 are welded into a whole, and the end part of the rectangular waveguide 101 is a short-circuit surface; the microwave mode converter 103 is a complete mode converter formed by a conical hollow oxygen-free copper body and the inner conductor 203, and is used for converting TE10 modes in the rectangular waveguide 101 into TEM modes of the coaxial waveguide; the inner conductor 203 is a hollow oxygen-free copper tube with one end serving as a gas inlet for raw gas, is welded all the way down to the disc antenna 205 into a whole, is converged by the annular gas converging groove 210 and flows near the growth stage (sample stage assembly 5).
In this embodiment, the support column is composed of six small cylinders with a diameter of 10mm, the small cylinders are uniformly arranged on the annular belt with weaker microwave electric field of the disc antenna 205 at 60 ° intervals, six corresponding positioning grooves are provided at the upper end of the disc antenna 205, so that the position of the support column can be determined during assembly, an annular second sealing groove 212 is designed at the lower end of the disc antenna 205, a quartz sealing ring window 201 is assembled between the disc antenna 205 and the deposition chamber 306, and soft sealing materials are filled in the second sealing groove 212 to ensure the high vacuum property of the deposition chamber 306.
In practical use, the outside of the deposition chamber 306 is provided with four cut-off observation windows 515, the cut-off observation windows 515 are positioned at the middle height of the deposition chamber 306, and the four windows are separated by 90 degrees; the cut-off window 515 is sized so that the microwave mode is in a cut-off state, without affecting the distribution of microwave fields within the chamber, for observing and measuring the state of the wafer during production.
The outside of the bottom of the deposition lower chamber is provided with a deposition chamber bottom plate 401 with an inverted cone structure, a water cooling coil 510 made of brass is coiled on the outside of the deposition chamber bottom plate 401, water is fed into the water cooling coil 510 from the bottom of the deposition chamber bottom plate 401, and water is discharged from the top of the water cooling coil, so that no dead water area is reserved on the deposition chamber bottom plate 401;
the thin steel plate between the bottom plate 401 of the deposition cavity and the support column 403 of the sample stage is provided with a circle of vent holes with the size of 3mm, which is beneficial to converging the gas around the sample stage assembly 5, and increases the utilization rate of raw gas and the deposition efficiency; the third water-cooled interlayer 305 is provided to ensure that the wafer is not broken by thermal stress caused by high temperature during growth.
In specific implementation, the specific steps are as follows:
1. the molybdenum table is used as a sample table for growth, the molybdenum table is placed on a sample table upper cover 502, the diameter is 70mm, the height is 10mm, 21 diamond seed crystals with the size of 10mm x 10mm are ground, washed by ultrasonic waves, dried by hot air and placed on the sample table;
2. adjusting the sample stage to a proper height by the first drive mechanism 406 and the second drive mechanism 414, closing all air inlet valves, and pumping the pressure of the chamber to within 10 e-1;
3. opening a circulating water cooling system, supplying circulating cooling water to each part of the device, and checking that the water inlet and outlet joints have no drip;
4. opening an air inlet valve, introducing 250sccm of hydrogen into the cavity, and regulating the pressure in the cavity to 5KPa through a balance valve;
5. turning on a microwave power supply, setting the microwave power to be 1KW, generating spheroid plasma in the deposition cavity 306, and adjusting the three-pin tuner and the deposition cavity bottom plate 401 to enable the reflected power to be zero;
6. gradually increasing the microwave power and the hydrogen gas pressure to enable the temperature of the upper surface of the substrate table to reach 950 ℃ when the microwave power is 6 KW;
7. introducing methane gas of 5sccm, starting formally growing, and forming a diamond monocrystal with the thickness of 3mm on a substrate table after 250 hours;
8. and closing a microwave power supply, closing an air extraction valve, filling nitrogen to a standard atmospheric pressure when the growth table is cooled to the room temperature, and taking out the wafer through an independent lifting mechanism of the sample table.
In actual use, the invention overcomes the defects of low deposition efficiency caused by etching pollution and microwave energy dispersion of a quartz sealing ring window in the production process in the existing device, excessive redundancy of an adjusting device, up-and-down jumping of plasma when a sample table is adjusted, low utilization rate of raw gas, and low yield of artificial diamond caused by uneven heat dissipation of the deposition table, and realizes the efficient and rapid preparation of the artificial diamond.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
The foregoing description of the preferred embodiment of the invention is not intended to be limiting, but rather to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (6)
1. The microwave plasma chemical vapor deposition device comprises a multi-medium transmission structure and is characterized in that: the multi-medium transmission structure comprises a microwave conversion assembly, an antenna terminal assembly connected with the microwave conversion assembly and a deposition furnace assembly connected with the antenna terminal assembly, wherein a lifting sample platform assembly is arranged in the deposition furnace assembly;
the microwave conversion assembly comprises a rectangular waveguide, a three-pin adapter arranged on the rectangular waveguide and a microwave mode converter arranged on the rectangular waveguide, wherein the microwave mode converter is used for converting TE10 modes in the rectangular waveguide into TEM modes in the coaxial waveguide;
the antenna terminal assembly comprises a first connecting piece, an inner conductor, an upper cover body, a disc antenna and a lower flange plate; the two ends of the first connecting piece are respectively connected with the rectangular waveguide and the upper cover body, the upper end of the inner conductor is connected with the microwave mode converter, an air channel is formed in the inner conductor, and a microwave channel is formed between the inner conductor and the first connecting piece; the inner conductor is fixedly connected with the disc antenna, the disc antenna is connected with the upper cover body through a supporting column, an annular air gathering groove communicated with the air channel is formed in the disc antenna, a first sealing groove is formed in the disc antenna, a second sealing groove is formed in the lower flange, a quartz sealing ring window is arranged between the disc antenna and the lower flange, the upper end and the lower end of the quartz sealing ring window are respectively located in the first sealing groove and the second sealing groove, and soft sealing materials are arranged in the first sealing groove and the second sealing groove; the lower flange plate is connected with the upper cover body and then fixes the quartz sealing ring window;
the deposition furnace component is connected with the lower flange plate, and the lifting sample platform component is installed in the deposition furnace component in a sliding and sealing manner;
the annular gas gathering groove is arranged at the lower end of the disc antenna, so that the uniformity of gas distribution on the sample growth table is improved, the waste of raw gas is reduced, and most of raw gas flows around the sample table; the quartz sealing ring window is positioned between the lower side of the disc antenna and the deposition cavity, so that a microwave strong electric field area is avoided, the problem of etching the quartz window by secondary plasma is avoided, and the relative position of the quartz sealing ring window and the disc antenna determines that the quartz sealing ring window avoids a main flowing area of raw gas and the problem of pollution etching is avoided;
the deposition furnace assembly comprises an inner cavity plate, a connecting plate and a vacuum cavity pipe, wherein two ends of the inner cavity plate are respectively connected with the connecting plate and the lower flange plate, a shell is arranged on the outer side of the inner cavity plate, and a third water-cooling interlayer for cooling water to flow is formed between the shell and the inner cavity plate; the vacuum cavity pipe is connected with the connecting plate and is communicated with the area above the connecting plate, and the lower end of the vacuum cavity is connected with the vacuum flange; the lifting sample platform component is arranged on the vacuum cavity tube, the upper end of the lifting sample platform component extends into a deposition cavity formed by the inner cavity plate,
the lifting sample platform assembly comprises a deposition cavity bottom plate with an inverted conical structure, a bottom plate support column connected with the deposition cavity bottom plate, a sample platform support column arranged in the bottom plate support column in a sliding manner, and a sample platform assembly arranged on the sample platform support column, wherein a sealing ring is arranged between the bottom plate support column and the sample platform support column; the bottom plate of the deposition cavity is slidably arranged on the connecting plate through an upper guide ring, and the sample stage support column is connected with a first driving mechanism which is used for driving the sample stage support column to move in the bottom plate support column; the bottom plate support column is connected with a second driving mechanism which is used for driving the bottom plate support column to move in the vacuum cavity tube and the deposition cavity;
the first driving mechanism comprises a corrugated pipe upper flange, a corrugated pipe lower flange, a corrugated pipe, a support, a screw rod nut and a motor, wherein the upper end of the corrugated pipe upper flange is connected with the vacuum flange, a bottom plate support column is in sliding connection with the corrugated pipe upper flange through a second guide ring, the corrugated pipe upper flange is arranged on the support, the upper end of the screw rod is rotatably arranged on the corrugated pipe upper flange, the lower end of the screw rod is rotatably arranged on the support, the motor is connected with the screw rod after being arranged on the support, the screw rod nut is arranged on the screw rod, the lower end of the sample table support column is connected with the corrugated pipe lower flange through a sealing plug, the corrugated pipe lower flange is connected with the screw rod nut, and the corrugated pipe upper flange is connected with the corrugated pipe lower flange through the corrugated pipe;
the second driving mechanism comprises a gear, a rack and a transmission shaft, the rack is fixedly arranged on the bottom plate supporting column, the transmission shaft is used for being rotationally and hermetically arranged on the vacuum cavity tube, the gear is positioned in the vacuum cavity tube and meshed with the rack, and one end, far away from the gear, of the transmission shaft is connected with a driving motor;
the sample table assembly comprises a table column arranged above the sample table supporting column and a sample table upper cover arranged on the table column; a positioning ring for placing a molybdenum support is arranged at the top of the upper cover of the sample table;
the bench post is provided with a mounting hole and a stepped through hole communicated with the mounting hole, a mounting area is formed between the mounting hole on the bench post and the upper cover of the sample bench, a waterway plate is arranged in the mounting area, a water inlet hole is arranged in the middle of the waterway plate, a plurality of first water tanks communicated with the water inlet hole are arranged at the top of the waterway plate, the lower end surface of the waterway plate is provided with a bulge corresponding to the stepped through hole, after the bulge on the waterway plate is matched with the bracket body through hole, the edge of the waterway plate and the edge of the mounting hole form a waterway, and the lower end surface of the waterway plate is provided with a plurality of second water tanks communicated with the waterway and the stepped through hole;
the lower end of the sample stage support column is provided with a plug, the water inlet hole is connected with a cooling water inlet pipe, the lower end of the cooling water inlet pipe penetrates through the plug, and the plug is provided with a cooling water outlet pipe.
2. A microwave plasma chemical vapor deposition apparatus according to claim 1, wherein: the microwave mode converter is a conical body made of copper or aluminum, the bottom edge of the conical body is tapped, the conical body is arranged in the rectangular waveguide, the upper end of the conical body is arranged at the opening of the upper end face of the rectangular waveguide, and the conical body is fixed through bolts; the middle part of the conical body is provided with a through hole, the upper end of the inner conductor is arranged in the through hole, a water cooling cavity is arranged in the conical body, and the cooling water inlet and the cooling water outlet are both positioned on the outer side of the upper end face of the rectangular waveguide and are communicated with the water cooling cavity.
3. A microwave plasma chemical vapor deposition apparatus according to claim 1, wherein: the middle part of the first connecting piece is an outer conductor, and a first water cooling interlayer for cooling water to flow is arranged on the outer side of the outer conductor.
4. A microwave plasma chemical vapor deposition apparatus according to claim 1, wherein: the outer side of the upper cover body of the sample table is provided with a second cooling interlayer for cooling water to flow.
5. A microwave plasma chemical vapor deposition apparatus according to claim 1, wherein: the outer side surface of the bottom plate of the deposition cavity is provided with a copper water-cooling coil pipe which is spirally arranged in a rising mode.
6. A microwave plasma chemical vapor deposition apparatus according to claim 5, wherein: the surface of the bottom plate support column, which is contacted with the sample platform support column, is provided with a dovetail groove, and the sealing ring is arranged in the dovetail groove.
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