CN114892144B - Atomization-assisted CVD reaction cavity - Google Patents
Atomization-assisted CVD reaction cavity Download PDFInfo
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- CN114892144B CN114892144B CN202210391451.7A CN202210391451A CN114892144B CN 114892144 B CN114892144 B CN 114892144B CN 202210391451 A CN202210391451 A CN 202210391451A CN 114892144 B CN114892144 B CN 114892144B
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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
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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
- C23C16/448—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4486—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by producing an aerosol and subsequent evaporation of the droplets or particles
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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
- C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45502—Flow conditions in reaction chamber
- C23C16/45504—Laminar flow
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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
- C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45587—Mechanical means for changing the gas flow
- C23C16/45591—Fixed means, e.g. wings, baffles
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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
- C23C16/458—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
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- 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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Abstract
The invention discloses an atomization-assisted CVD reaction cavity, which comprises a cavity, wherein the cavity is formed by bonding a cavity bottom plate, a cavity front cover plate, a cavity rear cover plate and a reaction zone cover plate, the reaction zone cover plate is arranged between the cavity front cover plate and the cavity rear cover plate, the reaction zone cover plate can be used for conveniently placing a substrate template in a high-temperature reaction zone in the cavity, the cavity bottom plate, the cavity front cover plate, the cavity rear cover plate and the reaction zone cover plate are all made of quartz materials, a plurality of thermocouples are arranged below the high-temperature reaction zone corresponding to the cavity, the inlet end of the cavity is communicated with a buffer cavity, and a water cooling device is further arranged at a position close to the inlet end of the cavity. The reaction cavity is made of quartz material, the high-temperature reaction area is transparent, the detail condition of the reaction area can be directly observed, and the introduction of light radiation in the film growth area can be conveniently realized, so that the method is not only beneficial to discussing a film forming mechanism, but also is a technical means of process optimization.
Description
Technical Field
The invention relates to the technical field of film preparation, in particular to an atomization-assisted CVD reaction cavity.
Background
Chemical vapor deposition (Chemical Vapor Deposition, CVD) is currently a widely used method for film preparation, particularly in the semiconductor industry. CVD is a general term for a large class of thin film production methods, and is basically characterized in that a gas phase or vapor phase source substance chemically reacts on a hot solid surface or near-surface region to form a thin film material, and there are several tens of specific CVD methods depending on the classification. New CVD methods and apparatus are also constantly being developed. The atomization-assisted CVD method is a novel CVD technology which has been widely focused in recent years after being developed for decades, and a large number of publicly published research documents show that the method is very suitable for preparing electronic grade high-quality single crystal films, in particular gallium oxide and zinc oxide materials. The most outstanding advantage of atomization-assisted CVD is that it operates at normal pressure without vacuum equipment, and compared with the current mainstream MOCVD technology in the semiconductor industry, only the energy consumption cost can be reduced by more than about 50%.
In CVD technology, the design of the reaction chamber is critical, and no matter scientific research or production, a good CVD chamber is an important guarantee for outputting high quality samples, and atomization-assisted CVD is no exception. However, the detailed mechanism of film growth at present, including mass transport, energy transport, chemical reaction power system of film growth, etc., is not very clear, and a great deal of experimental and theoretical research work is still carried out because the principle of optimal cavity design and optimal cavity parameters cannot be given from the theoretical angle. In experimental research, it is necessary to continuously adjust and optimize the environment in the cavity in order to further explore the mechanism of film growth. It is uneconomical, both from a capital and from a time point of view, if each adjustment requires a new cavity to be manufactured. Moreover, the process stability and repeatability of the processing cannot be guaranteed by the customized processing, so that the reliability of the contrast analysis of the generated experimental data is reduced, and the meaning of the contrast analysis is even completely lost.
It is therefore necessary to design and manufacture a reusable chamber for exploring the mechanism of film growth.
Disclosure of Invention
Aiming at the technical problems existing at present, the invention provides an atomization-assisted CVD reaction cavity to solve the problems in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the utility model provides an auxiliary CVD reaction cavity of atomizing, includes the cavity, and this cavity is formed after bonding by cavity bottom plate, cavity front shroud, cavity back shroud and reaction zone apron, and this reaction zone apron is established between cavity front shroud and the cavity back shroud, the setting of reaction zone apron can be convenient place the substrate template high temperature reaction zone in the cavity, cavity bottom plate, cavity front shroud, cavity back shroud and reaction zone apron all adopt quartz material to make, in the below position that corresponds the high temperature reaction zone of cavity is equipped with a plurality of thermocouples, the entrance point and the buffer chamber intercommunication of cavity, and still be equipped with water cooling plant in the position that is close to its entrance point, the exit end of cavity is the exhaust emission mouth.
Preferably, the positions on the two sides of the cavity bottom plate are respectively provided with a special-shaped side edge strip, V-shaped grooves are distributed on one side of the special-shaped side edge strip, which faces the cavity bottom plate, high-temperature glue is filled in the V-shaped grooves to bond the special-shaped side edge strips with the cavity bottom plate, and the other side of the special-shaped side edge strip is bonded with the cavity front cover plate, the cavity rear cover plate and the reaction area cover plate at corresponding positions.
By the arrangement, the structural stability of the cavity can be enhanced, and the air tightness of the joint can be improved.
Preferably, the special-shaped side strip is embedded with a first side filling block at a position corresponding to the high-temperature reaction zone.
In the experimental process, the high-temperature reaction area can deposit a film together with the side area so as to pollute the special-shaped side strip, so that the first side filling block is embedded in the area, and the pollution of the deposited film to the special-shaped side strip is reduced.
Preferably, the position corresponding to the tail gas transport area on the special-shaped side strip is embedded with a second side filling block, and the second side filling block is of a trapezoid structure, so that precursor liquid aerosol condensed into liquid drops is conveniently drained to the middle of the cavity, and corrosion to the junction of the special-shaped side strip and the cavity bottom plate is reduced.
So set up, precursor liquid aerosol can condense into liquid drop corruption dysmorphism side bar and cavity bottom plate juncture through high temperature reaction zone entering low temperature tail gas transport zone in the experiment, so low temperature tail gas transport zone embedding second side filler in dysmorphism side bar, the condensation liquid drop hangs in cavity inner space upper portion generally, then drip naturally through the action of gravity, the trapezium structural design of second side filler makes things convenient for liquid drop to the cavity or cavity bottom plate middle gathering, has increased the space distance between dysmorphism side bar and the cavity bottom plate juncture and the liquid drop, improve cavity life.
Preferably, the reaction area cover plate comprises a reaction area upper cover plate and a flow field modulation wedge bonded below the reaction area upper cover plate, the wedge of the flow field modulation wedge faces to the inlet end of the cavity, the length of the reaction area upper cover plate is larger than that of the flow field modulation wedge, and two ends of the reaction area upper cover plate are bonded with the cavity front cover plate and the cavity rear cover plate at corresponding ends respectively.
The reaction zone cover plate is connected with the cavity front cover plate and the cavity rear cover plate in an adhesive manner, so that the disassembly and the assembly are convenient; the flow field modulation wedge can effectively regulate and control the deposition position of the precursor liquid aerosol, and has the function of converging the precursor liquid aerosol along the flow field modulation wedge direction, so that the deposition efficiency is improved, and meanwhile, the flow field modulation wedge is adhered to the upper cover plate of the reaction zone, so that different flow field modulation wedges are convenient to replace, and the influence research of different wedge angles on the air flow field and the film structure can be rapidly realized.
Preferably, airtight grooves are distributed on the upper cover plate of the reaction zone at the positions where the upper cover plate of the reaction zone is bonded with the front cover plate of the chamber and the rear cover plate of the chamber, and high-temperature glue is filled in the airtight grooves to improve the air tightness of the bonding position.
Preferably, the distance between the bottom surface of the flow field modulation wedge and the upper surface of the substrate template is 1.1-1.3mm.
Laminar flow can be stably maintained in the range of the distance, and samples with better quality can be successfully prepared.
Preferably, the thermocouple is fixed below the cavity bottom plate through a thermocouple temperature measuring end fixing plate and a thermocouple wire harness fixing plate.
Preferably, the lower end face of the chamber bottom plate is provided with an inwards concave groove, and the thermocouple temperature measuring end fixing plate and the thermocouple wire harness fixing plate are embedded in the groove.
Compared with the prior art, the invention has the beneficial effects that:
(1) The reaction cavity is made of quartz, the high-temperature reaction area is transparent, the detail condition of the reaction area can be directly observed, the introduction of light radiation in the film growth area can be conveniently realized, and the method is not only beneficial to discussing a film forming mechanism, but also is a technical means of process optimization;
(2) The chamber is formed by bonding the chamber bottom plate, the chamber front cover plate, the chamber rear cover plate and the reaction zone cover plate, the sample is conveniently taken and placed through the installation and the disassembly of the reaction zone cover plate, the substrate template is also conveniently replaced, the deposition reaction of different substrate templates can be adapted, the application range is wide, and the reusability is also improved;
(3) The scheme designs the water cooling module, so that the temperature of a cavity body in a water cooling module area is close to room temperature, the transportation characteristic of liquid aerosol entering the space from a buffer cavity body to a deposition reaction high-temperature area can be optimized, the service life of liquid aerosol particles is regulated and controlled, and the stability of process parameters of film deposition and the repeatability of film properties are improved;
(4) The flow field modulation wedge provided by the scheme is combined with the upper cover plate of the reaction area in an adhesion mode, is convenient to detach and replace, and can realize the influence study of different wedge angles on the air flow field and the film structure.
Description of the drawings:
FIG. 1 is a top view of the present invention;
FIG. 2 is a bottom view of FIG. 1;
FIG. 3 is an internal cross-sectional view of FIG. 1;
FIG. 4 is a cross-sectional view A-A of FIG. 1;
FIG. 5 is a cross-sectional view B-B of FIG. 1;
FIG. 6 is a schematic structural view of the reaction zone cover plate of FIG. 1;
fig. 7 is a schematic structural view of the thermocouple wire harness fixing piece in fig. 1.
Detailed Description
The present invention will be described in further detail with reference to test examples and specific embodiments. It should not be construed that the scope of the above subject matter of the present invention is limited to the following embodiments, and all techniques realized based on the present invention are within the scope of the present invention.
In the description of the present invention, it should be understood that the terms "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate describing the present invention and simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
In the description of the present invention, unless otherwise specified and defined, it should be noted that the terms "mounted," "connected," and "coupled" are to be construed broadly, and may be, for example, mechanical or electrical, or may be in communication with each other between two elements, directly or indirectly through intermediaries, as would be understood by those skilled in the art, in view of the specific meaning of the terms described above.
The atomization-assisted CVD reaction cavity comprises a cavity 1, wherein the cavity 1 is formed by bonding a cavity bottom plate 11, a cavity front cover plate 12, a cavity rear cover plate 13 and a reaction area cover plate 2, the bonded cavity 1 is of a horizontal rectangular cavity structure and is sequentially divided into a low-temperature conveying area from front to back, a high-temperature reaction area and a tail gas conveying area, the reaction area cover plate 2 is arranged between the cavity front cover plate 12 and the cavity rear cover plate 13 and can be detached, a substrate template 3 can be conveniently placed in the high-temperature reaction area in the cavity 1 through detachment, a heating mechanism is arranged at the position corresponding to the reaction area cover plate 2 in the experimental process, the high-temperature reaction area is formed, the cavity bottom plate 11, the cavity front cover plate 12, the cavity rear cover plate 13 and the reaction area cover plate 2 are all made of quartz materials, the inlet end of the cavity 1 is communicated with a buffer cavity 5, a water cooling device 4 is further arranged at the position close to the inlet end of the cavity, the water cooling device 4 is connected with a water pump through a pipeline, and the water pump drives cooling water close to room temperature to circulate, so that the temperature of the cavity of the water cooling device 4 area is close to the room temperature, and the room temperature is guaranteed, and precursor liquid aerosol is guaranteed not to be excessively lost in the low-temperature area. The outlet end of the chamber 1 is a tail gas discharge port, the outlet end and the inlet end of the chamber 1 are similar, and each chamber comprises a brass metal fixing piece and a rubber airtight gasket, and the brass metal fixing piece extrudes the rubber airtight gasket to deform the rubber airtight gasket, so that a good airtight effect is achieved. The buffer cavity 5 is a cylindrical cavity, so that the precursor liquid aerosol airflow is ensured to be uniform and stable, and precursor liquid aerosol particles with the same diameter can be screened out and enter the cavity 1.
The high-temperature reaction area of the cavity is transparent, can be used for directly observing the detail condition of the reaction area, can conveniently realize the introduction of optical radiation in the film growth area, such as ultraviolet light introduction, has strong chemical activity, is beneficial to discussing a film forming mechanism, and is also a possible technical means for process optimization.
As can be seen from fig. 5 in combination with fig. 3, the reaction zone cover plate 2 includes a reaction zone upper cover plate 21 and a flow field modulation wedge 23 adhered below the reaction zone upper cover plate 21, a wedge 24 of the flow field modulation wedge 23 faces to an inlet end of the chamber 1, and in a high-temperature reaction zone, precursor liquid aerosol is generally subjected to comprehensive modulation of a flow field, a gravity field and a temperature field, the deposition effect and the deposition position of the precursor liquid aerosol are difficult to effectively control, and the flow field modulation wedge 23 can effectively regulate and control the deposition position of the precursor liquid aerosol and acts on the precursor liquid aerosol in a converging way along the wedge direction, so that the deposition efficiency is improved. In the experiment, the precursor liquid aerosol flow field is required to be laminar, so that vortex is avoided. The thickness of the flow field modulation wedge 23 is designed to be 4.5mm, the inclination angle of the wedge 24 is designed to be 10 degrees, the distance between the bottom end of the flow field modulation wedge 23 and the upper surface of the substrate template 3 is 0.8-1.5mm, preferably 1.2mm, and experimental results show that laminar flow can be stably maintained under the thickness design, samples with better quality can be successfully prepared, and thickness and angle parameters can be improved according to practical requirements.
The length of the reaction area upper cover plate 21 is larger than that of the flow field modulation oblique wedge 23, and two ends of the reaction area upper cover plate 21 extend out of the flow field modulation oblique wedge 23, and are respectively bonded with the chamber front cover plate 12 and the chamber rear cover plate 13 at the corresponding ends. And airtight grooves 22 are distributed on the upper cover plate 21 of the reaction zone at the positions bonded with the front cover plate 12 and the rear cover plate 13 of the chamber, high-temperature glue is filled before the experiment begins, the cover plate of the reaction zone is covered, and the air tightness of the joint is further improved. 45-degree chamfer surfaces are designed on the front side and the rear side of the upper cover plate 21 of the reaction zone, and when the upper cover plate 21 of the reaction zone is disassembled, the upper cover plate 21 of the reaction zone can be taken out more easily by applying acting force according to the cutting direction, so that the reusability of the upper cover plate 21 of the reaction zone is realized. Meanwhile, the reaction area cover plate 2 is arranged in an adhering mode, so that samples can be conveniently taken and placed, and the flow field modulation wedge 23 can be conveniently replaced.
The two sides of the upper surface of the cavity bottom plate 11 are respectively connected with the special-shaped side strips 7 through the heights Wen Jiaofen, and the junction of the special-shaped side strips 7 and the cavity bottom plate 11 is more easily corroded compared with the junction of the special-shaped side strips 7 and the cavity front cover plate 12 and the cavity rear cover plate 13, so that V-shaped grooves 71 are designed at the junction of the special-shaped side strips 7 and the cavity bottom plate 11, and high-temperature glue is filled in the V-shaped grooves 71 for enhancing the structural stability of the cavity 1 and improving the air tightness of the junction. The surface of the special-shaped side edge strip 7 opposite to the V-shaped notch 71 is bonded with the chamber front cover plate 12, the chamber rear cover plate 13 and the reaction zone cover plate 2 by a height Wen Jiaofen. In the experiment, precursor liquid aerosol enters a tail gas conveying area through a high-temperature reaction area and is condensed into liquid drops to corrode the junction of the special-shaped side strip 7 and the chamber bottom plate 11, so that a second side filling block 9 is embedded in the position of the special-shaped side strip 7 in the tail gas conveying area, the second side filling block 9 is of a trapezoid structure, condensed liquid drops are normally suspended in the upper space in the chamber 1, naturally drip under the action of gravity, the precursor liquid aerosol condensed into the liquid drops can be conveniently drained to the middle part of the chamber 1 through the second side filling block 9 of the trapezoid structure, the liquid drops are converged in the chamber 1, the space distance between the junction of the special-shaped side strip 7 and the chamber bottom plate 11 and the liquid drops is increased, corrosion to the junction of the special-shaped side strip 7 and the chamber bottom plate 11 is reduced, and the service life of the chamber 1 is prolonged. The high temperature reaction zone is a film deposition zone, and the phenomenon of the film deposition zone is required to be observed continuously and clearly in experiments. But in the experimental process, the high-temperature reaction area can deposit a film together with the side area and then pollute the special-shaped side strip 7, so that the first side filling block 8 is embedded in the high-temperature reaction area and the low-temperature conveying area of the special-shaped side strip 7, the polluted special-shaped side strip is conveniently replaced, the experimental requirement is met, and the loss degree of the whole structure of the chamber 1 is reduced.
A plurality of thermocouples are arranged at the lower position of the high-temperature reaction zone corresponding to the chamber 1, and the thermocouples are fixed below the chamber bottom plate 11 through a thermocouple temperature measuring end fixing plate 62 and a thermocouple wire harness fixing plate 61.
Specifically, an inward concave groove is formed in the lower end face of the chamber bottom plate 11, a thermocouple temperature measuring end fixing plate 62 and a thermocouple wire harness fixing plate 61 are embedded in the groove, the stability between the thermocouple temperature measuring end fixing plate 62 and the thermocouple wire harness fixing plate 61 and the chamber bottom plate 11 is improved, the inner surface of the groove is subjected to rough passivation treatment, a high heat conducting plate 63 is embedded in the groove close to one side of the water cooling device, the high heat conducting plate 63 is arranged below a low-temperature conveying area to ensure that precursor liquid aerosol is not consumed, the chamber bottom plate 11 is connected with the water cooling device 4, and heat energy is more quickly conducted to the water cooling device 4 through the high heat conducting plate 63, so that loss of the precursor liquid aerosol in the low-temperature conveying area is reduced.
As can be seen from fig. 7, the thermocouple wire harness fixing piece 61 is distributed with wire harness fixing grooves 611, in order to improve the reusability of the components of the chamber 1, 45 ° inclined planes 612 are designed on two side edges of the thermocouple wire harness fixing piece 61 and the thermocouple temperature measuring end fixing piece 62, and when the fixing piece is disassembled, the fixing piece can be removed more easily by applying force along the cutting direction, so that the reusability of the components of the chamber is realized.
The position of the thermocouple temperature measuring end stator 62 is extremely important in experiments. According to the analysis design of the practical experimental result, when the current three thermocouple temperature measuring end fixing plates 62 are respectively designed at the lower front part, the lower part and the lower rear part of the position of the flow field modulation wedge 23, the practical temperature at the film deposition area of the high-temperature reaction area can be more accurately and comprehensively reflected, and the number of thermocouples and the number of temperature measuring end fixing plates can be increased according to specific requirements. The low temperature transport region is the transport end of the precursor liquid aerosol, but the temperature field of the high temperature reaction region can lead the precursor liquid aerosol to start to evaporate in the low temperature transport region.
The substrate template 3 is arranged on the chamber bottom plate 11, the c-plane sapphire substrate is embedded in the substrate template 3, and the substrate placing area is arranged below the flow field modulation wedge 23. Since the deposition of the thin film in the high temperature reaction zone is performed simultaneously in the experiment, the high temperature reaction zone on the upper surface of the chamber bottom plate 11 is gradually contaminated due to the deposition of the thin film. The substrate template 3 can replace the upper surface of the chamber bottom plate 11 to bear pollution, and the substrate template 3 is replaced through the reaction area cover plate 2 area, so that the continuous and long-term use of the chamber 1 is realized. In the experiment, the prepared film is required to be a two-dimensional material, and the side edge of the c-plane sapphire substrate cannot be deposited. The substrate template 3 replaces the function of pre-substrate, so that the surface of the c-plane sapphire substrate is smoothly jointed with the surface of the substrate template 3, and the preparation requirement of the two-dimensional film material is met. And an electrode (the lower surface of the substrate template 3 and one surface of the flow field modulation wedge facing the sample) can be arranged in the high-temperature reaction area, so that the electric field loading of the film deposition area can be realized.
The operation steps of the device are as follows:
step 1: respectively ultrasonically cleaning a substrate template 3, a c-plane sapphire substrate, a first side filling block 8 and a second side filling block 9 by deionized water, acetone, ethanol and deionized water for 10 minutes, and drying by nitrogen;
step 2: opening a reaction area cover plate 2, respectively installing a first side filling block 8 and a second side filling block 9 in a high-temperature reaction area and a tail gas conveying area, installing a c-plane sapphire substrate in a substrate placing area of a substrate template 3, installing the substrate template 3 in the high-temperature reaction area in a cavity 1, and positioning the substrate template placing area below the position of a flow field modulation wedge 23;
step 3: coating a layer of high-temperature glue in the airtight groove of the reaction area cover plate 2, and covering the reaction area cover plate 2 on the high-temperature reaction area of the chamber 1;
step 4: deposition reactions were performed and the relevant data was observed.
The foregoing describes preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention by one of ordinary skill in the art without undue burden. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (9)
1. An atomization-assisted CVD reaction chamber, characterized in that: including cavity (1), this cavity (1) is formed by cavity bottom plate (11), cavity front shroud (12), cavity back shroud (13) and reaction zone apron (2) bonding back, and this reaction zone apron (2) are established between cavity front shroud (12) and cavity back shroud (13), the setting of reaction zone apron (2) can conveniently place substrate template (3) the high temperature reaction zone in cavity (1), cavity bottom plate (11), cavity front shroud (12), cavity back shroud (13) and reaction zone apron (2) all adopt quartz material to make, correspond the below of the high temperature reaction zone of cavity (1) is equipped with a plurality of thermocouples, the entrance point and the buffer chamber (5) intercommunication of cavity (1), and still be equipped with water cooling plant (4) in the position that is close to its entrance point, the exit end of cavity (1) is the tail gas emission mouth.
2. An atomising assisted CVD reactor according to claim 1, wherein: the position that lies in its both sides on cavity bottom plate (11) is equipped with dysmorphism side bar (7) respectively, dysmorphism side bar (7) orientation one side of cavity bottom plate (11) distributes has V type groove (71), and this V type groove (71) intussuseption is filled with high temperature glue, realizes with cavity bottom plate (11) bonding, the opposite side of dysmorphism side bar (7) with corresponding position cavity front shroud (12), cavity back shroud (13) and reaction zone apron (2) bond.
3. An atomising assisted CVD reactor according to claim 2, wherein: and a first side filling block (8) is embedded in the special-shaped side strip (7) at a position corresponding to the high-temperature reaction zone.
4. An atomising assisted CVD reactor according to claim 2, wherein: the position corresponding to the tail gas transport area on the special-shaped side strip (7) is embedded with a second side filling block (9), the second side filling block (9) is of a trapezoid structure, precursor liquid aerosol condensed into liquid drops is conveniently drained to the middle of the cavity (1), and corrosion to the junction of the special-shaped side strip (7) and the cavity bottom plate (11) is reduced.
5. An atomising assisted CVD reactor according to claim 1, wherein: the reaction zone cover plate (2) comprises a reaction zone upper cover plate (21) and a flow field modulation oblique wedge (23) adhered below the reaction zone upper cover plate (21), a wedge (24) of the flow field modulation oblique wedge (23) faces to the inlet end of the chamber (1), the length of the reaction zone upper cover plate (21) is larger than that of the flow field modulation oblique wedge (23), and two ends of the reaction zone upper cover plate (21) are adhered to a chamber front cover plate (12) and a chamber rear cover plate (13) at corresponding ends respectively.
6. An atomization-assisted CVD reactor chamber as claimed in claim 5 wherein: and airtight grooves (22) are distributed on the upper cover plate (21) of the reaction zone at the positions bonded with the front cover plate (12) and the rear cover plate (13) of the cavity, and the airtight grooves (22) are filled with high-temperature glue, so that the air tightness of the joint is improved.
7. An atomising assisted CVD reactor according to claim 6, wherein: the distance between the bottom surface of the flow field modulation wedge (23) and the upper surface of the substrate template (3) is 0.8-1.5mm.
8. An atomising assisted CVD reactor according to claim 1, wherein: the thermocouple is fixed below the chamber bottom plate (11) through a thermocouple temperature measuring end fixing plate (62) and a thermocouple wire harness fixing plate (61).
9. An atomising assisted CVD reactor according to claim 8, wherein: the lower end face of the chamber bottom plate (11) is provided with an inwards concave groove, and the thermocouple temperature measuring end fixing plate (62) and the thermocouple wire harness fixing plate (61) are embedded in the groove.
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