CN114351117B - Spray plate, MOCVD reaction system with spray plate and use method of MOCVD reaction system - Google Patents
Spray plate, MOCVD reaction system with spray plate and use method of MOCVD reaction system Download PDFInfo
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- CN114351117B CN114351117B CN202011091246.6A CN202011091246A CN114351117B CN 114351117 B CN114351117 B CN 114351117B CN 202011091246 A CN202011091246 A CN 202011091246A CN 114351117 B CN114351117 B CN 114351117B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
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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
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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
- C23C16/54—Apparatus specially adapted for continuous coating
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
- H01B12/02—Superconductive or hyperconductive conductors, cables, or transmission lines characterised by their form
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
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Abstract
The application relates to a spray plate, an MOCVD reaction system with the spray plate and a using method thereof, wherein the MOCVD reaction system comprises: heating a substrate, a spray plate, an MOCVD reaction chamber, a cooler and an extraction opening; the spraying plate is internally provided with a source reaction gas channel which is positioned in the middle of the width of the spraying plate and extends along the length direction of the spraying plate, and the inner wall surfaces of the source reaction gas channel are respectively provided with a plurality of source reaction gas spray holes which extend downwards to the lower surface of the spraying plate. The method and the device can improve the mixing uniformity of the metal organic source gas and the source reaction gas in the reaction cavity and the temperature uniformity of the spraying plate, and further improve the production quality of the superconducting tape.
Description
Technical Field
The application relates to the field of superconducting strip manufacturing, in particular to a spray plate, an MOCVD reaction system with the spray plate and a using method of the MOCVD reaction system.
Background
The second generation high temperature superconducting tape has zero resistance characteristic, so the current carrying capacity of the formed superconducting cable is 5-10 times of that of the existing copper cable, the volume and weight of the manufactured superconducting motor can be reduced to 1/4 of the original weight, revolutionary revolution and industrial upgrading are brought in many fields, and the superconducting motor has great market potential.
The high-temperature superconducting tape is prepared by depositing a high-temperature superconducting film on an inexpensive and flexible metal substrate. The metal base tape is typically several thousand to several hundred meters long, several tens of microns thick, and 10-20 millimeters wide. And performing high-temperature epitaxial deposition on the textured strip by adopting a roll-to-roll MOCVD method to form the superconducting strip.
To assist the reader in understanding, fig. 1 is a schematic diagram of MOCVD deposition of high temperature superconducting tapes, in roll-to-roll deposition, a tape 11 is controlled by a tape transport system, enters a deposition chamber (or MOCVD reaction chamber), moves on a heated substrate 2 at a certain speed, the upper surface of the heated substrate 2 is arc-shaped, and the temperature of the heated substrate 2 is derived from a heating element 8 below. Under the tension of the tape transport system 10, the tape 11 and the heated substrate 2 are in intimate contact, resulting in precise high temperature control. The source gas from the sprayer 3 reacts with the source reaction gas on the surface of the strip to form the superconducting film. The source reactant gas is typically oxygen. The superconducting film is deposited to 2 microns. In order to make full use of the deposition zone, which is 60-130 mm wide and typically more than one meter long, a strip winding system consisting of a plurality of sets of guide wheels is used to pass the strip continuously through the heated substrate a number of times, in order to achieve the production rate required for industrialization.
The metal organic source such as Zr, Y, gd, ba, cu, etc. required for the superconducting thin film is solid at normal temperature, and needs to be evaporated into an organic source gas in the source evaporator, and the organic source gas is injected into a gas distributor (or called a sprayer) through a source gas transmission pipeline. Before the organic source gas reaches the strip material for reaction, the organic source gas needs to be uniformly mixed with the source reaction gas, namely oxygen, so that uniform deposition can be formed on the surface of the strip material. Conventionally, the organic source gas and the oxygen gas are mixed in a shower or a source pipe, which ensures sufficient and uniform mixing of the organic source gas and the oxygen gas. However, this approach requires a high degree of accuracy in temperature control of the source transport pipe and the shower because, at low temperatures, organic source gases condense on the inner surfaces of the source transport pipe and the shower. At high temperatures, the organic source gas and oxygen pre-react in the source line and the shower, causing the superconducting film composition to be difficult to control and the line and shower to become clogged.
In view of the above problem, chinese patent publication No. CN205329157 teaches a method of reducing pre-reaction by providing an oxygen introducing mechanism, oxygen plate 6, under a cooling plate as shown in fig. 5. However, this method causes a serious problem of non-uniform mixing of the oxygen gas and the organic source gas. Especially for the winding deposition system with a large number of winding tracks (more than 8 tracks), the deposition area is wide, and the problem is very serious and cannot be used. For the deposition of the high-temperature superconducting film, the concentration of oxygen is an important parameter, and the uneven distribution of oxygen makes it impossible to obtain the optimal deposition conditions on each winding path, resulting in a narrow process window. If the process window is narrow and the system drifts very little, the drift of the performance of the superconducting film is serious, and the yield of the strip material is low.
A further problem with the current configuration is that the shower plate is heated by thermal radiation from the underlying heated substrate (high temperature of 1000 c), with high temperatures in the middle and low temperatures on the sides, with a temperature difference of over 30 c across the width of the shower plate, as shown in figure 4. It is known that the organic source gas required for deposition of high temperature superconducting thin film is very strict in temperature control, cannot be high or low, and the temperature of the shower plate is not uniform, so that the shower plate is formed, the organic source gas is decomposed in the middle (even if oxygen is not present, the organic source gas is decomposed due to reaching the decomposition temperature) if the middle temperature is too high, and the organic source gas is not condensed on the edge if the temperature is too low. In both cases, the spray holes are blocked, and the composition of the superconducting film is changed, so that the performance of the superconducting film is reduced. Cleaning the spray plate of the oxide that blocks up, need to use acid bubble, therefore spray plate need to use the stainless steel material that the anticorrosion is good. To reduce clogging, the spray holes cannot be too long, so the spray plate is as thin as possible, typically 2-3 mm thick. However, stainless steel has poor heat conduction, thin plates also have poor heat conduction, and the temperature uniformity of the shower plate is also poor.
Disclosure of Invention
The technical problem that this application will solve is: in order to solve the problems, a spray plate, an MOCVD reaction system with the spray plate and a using method of the MOCVD reaction system are provided, and the purpose is to improve the mixing uniformity of metal organic source gas and source reaction gas in a reaction cavity and the temperature uniformity of the spray plate, and further improve the production quality of superconducting tapes.
The technical scheme of the application is as follows:
an MOCVD reaction system, comprising:
an MOCVD reaction chamber;
a heated substrate disposed within the MOCVD reaction chamber;
a shower plate disposed above the heating substrate and having a plurality of organic source gas injection holes, the shower plate having a length extending in a tape running direction and a width perpendicular to the length;
a cooler thermally connected to both sides of the width of the shower plate, and
the extraction openings are communicated with the MOCVD reaction cavity and are positioned on two sides of the width of the spray plate;
the spraying plate is internally provided with a source reaction gas channel which is positioned in the middle of the width of the spraying plate and extends along the length direction of the spraying plate, and the inner wall surface of the source reaction gas channel is provided with a plurality of source reaction gas spray holes which extend downwards to the lower surface of the spraying plate.
On the basis of the technical scheme, the MOCVD system further comprises the following preferred scheme:
the plurality of source reaction gas injection holes are arranged at intervals along the length direction of the source reaction gas flow channel.
The lower end orifice of at least one source reaction gas jet orifice is an outward-expanding horn mouth.
And the spray plate is fixedly connected with a guide plate positioned below the source reaction gas spray holes.
The width of the guide plate is larger than the diameter of the lower orifice of any source reaction gas jet hole in the source reaction gas jet holes.
Two source reaction gas auxiliary channels which are respectively positioned at two radial sides of the source reaction gas channel are also arranged in the spraying plate, and a plurality of source reaction gas auxiliary spray holes which extend downwards to the lower surface of the spraying plate are formed in the inner wall surface of each source reaction gas auxiliary channel.
The two source reaction gas secondary flow channels are arranged in parallel with the source reaction gas flow channel, and the two source reaction gas secondary flow channels are symmetrically arranged on two radial sides of the source reaction gas flow channel.
A use method of the MOCVD reaction system comprises the following steps:
and introducing mixed gas which is lower in temperature than the spraying plate and is composed of oxygen and inert gas into the source reaction gas channel, and adjusting the proportion of the inert gas in the mixed gas to ensure that the temperature of the middle part of the spraying plate is basically equal to the temperature of the left side part and the right side part of the spraying plate.
A shower plate for an MOCVD system, comprising:
upper and lower surfaces facing away from each other, an
A plurality of organic source gas injection holes penetrating from the upper surface to the lower surface;
the spraying plate is internally provided with a source reaction gas channel which is positioned in the middle of the width of the spraying plate and extends along the length direction of the spraying plate, and the inner wall surface of the source reaction gas channel is provided with a plurality of source reaction gas spray holes which extend downwards to the lower surface of the spraying plate.
On the basis of the technical scheme, the spray plate further comprises the following preferable scheme:
and the spray plate is fixedly connected with a guide plate positioned below the source reaction gas spray holes.
Two source reaction gas auxiliary channels respectively positioned at two radial sides of the source reaction gas channel are also formed in the spray plate, and a plurality of source reaction gas auxiliary spray holes extending downwards to the lower surface of the spray plate are formed in the inner wall surface of each source reaction gas auxiliary channel.
The beneficial effect of this application:
1. the source reaction gas channel is arranged in the middle of the width of the spray plate and extends along the length direction of the spray plate, and a plurality of source reaction gas spray holes extending downwards to the lower surface of the spray plate are formed in the inner wall surface of the source reaction gas channel. In practical application, the source reaction gas and the metal organic source gas are not mixed before entering the MOCVD reaction cavity, so that pre-reaction cannot occur, the problem of blockage of the spray plate is further solved, the spray plate does not need to be cleaned frequently, only alcohol is needed to be used for scrubbing during cleaning every time, acid bubbles are not needed, and the maintenance cost and time are reduced.
The source reaction gas flow channel is arranged in the middle of the spray plate, so the source reaction gas sprayed out from each source reaction gas spray hole is firstly positioned in the middle of the MOCVD reaction cavity, and the pumping holes are arranged at the left side and the right side of the non-middle part of the MOCVD reaction cavity. Therefore, the gas pressure in the middle of the MOCVD reaction cavity is high, the gas pressures on the two sides are low, and the source reaction gas just sprayed out from the source reaction gas spray holes can be naturally diffused to the two sides (periphery), so that the source reaction gas is fully and uniformly mixed and reacted with the metal organic source gas in the MOCVD reaction cavity, and a uniform high-quality superconducting thin film is formed on the surface of the strip.
Even though the oxygen concentration in the middle of the reaction chamber is slightly higher than that in the side part in practical application, because the flow field flows outwards, the oxygen is introduced in the middle, and the uniformity of the oxygen concentration is much better than that obtained by the prior art. Further, the inventors' studies have found that the deposition rate is highest in the middle of the deposition region, indicating that the middle is the region where the source gas concentration is highest, and therefore, the optimum chemical reaction conditions also require that the oxygen concentration in the middle be correspondingly high.
2. In practical application, the source reactant gas fed into the source reactant gas flow channel can absorb the temperature of the middle area of the spray plate, so that the problems that the temperature of the middle part of the traditional spray plate is high and the temperature of two sides of the traditional spray plate is low due to the fact that the coolers are arranged on two sides of the traditional spray plate can be solved, the temperature of each part of the spray plate tends to be uniform, and the temperature of the metal organic source gas sprayed from each organic source gas spray hole tends to be equal.
3. In practical applications, not only the necessary oxygen gas but also an inert gas, such as argon, which does not react with the metal organic source gas may be introduced into the source reactant gas flow channel. That is, the source reaction gas may be a mixed gas of oxygen and an inert gas. Therefore, under the condition that the source reaction gas meets the required temperature and the oxygen in the source reaction gas meets the required flow, the flow of the inert gas in the source reaction gas is increased to absorb the heat in the middle of the spraying plate, so that the temperature in the middle of the spraying plate is basically equal to the temperature of the left side part and the right side part of the spraying plate, and the temperature uniformity of the spraying plate is improved.
4. The source reaction gas spray holes are arranged at intervals along the length direction of the source reaction gas flow channel, so that the source reaction gas sprayed out of each source reaction gas spray hole can uniformly flow to the MOCVD reaction cavity as far as possible, and the production quality of the superconducting tape is further improved.
5. The lower end orifices of the source reaction gas spraying holes are flared bell mouths, when the source reaction gas is sprayed out of the source reaction gas spraying holes, the gas pressure is suddenly reduced, the gas expands to form high transverse velocity components, oxygen can be favorably diffused towards two sides, and the mixing uniformity of the source reaction gas and the metal organic source gas in the MOCVD reaction cavity is improved.
6. And a guide plate positioned below each source reaction gas spray hole can be fixedly connected to the spray plate. When the metal organic source gas spraying device works, source reaction gas sprayed out of the source reaction gas spraying holes flows towards two sides under the blocking of the guide plates, so that the transverse flow of the source reaction gas, particularly oxygen, is increased, the oxygen can be favorably diffused towards two sides, and the mixing uniformity of the source reaction gas and the metal organic source gas in the MOCVD reaction cavity is improved.
7. Two source reaction gas auxiliary channels which are respectively positioned at two radial sides of the source reaction gas channel are arranged in the spray plate, a plurality of source reaction gas auxiliary spray holes which extend downwards to the lower surface of the spray plate are formed in the inner wall surface of each source reaction gas auxiliary channel, and when the spray plate works, source reaction gas containing oxygen is introduced into each source reaction gas auxiliary channel, so that the temperature uniformity of the spray plate and the oxygen uniformity in a reaction cavity are further improved, and the spray plate is particularly suitable for processing a plurality of strips.
8. Under the technical improvement of the application, the critical current Ic of the prepared superconducting tape is improved by 30 percent. More importantly, the process window is greatly expanded, and the yield is greatly improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings of the embodiments will be briefly introduced below, and it is apparent that the drawings in the following description only relate to some embodiments of the present application and are not limiting on the present application.
Fig. 1 is one of the structural schematic diagrams of a conventional MOCVD reaction system.
Fig. 2 is a cross-sectional view of the lower half in fig. 1 in a left side view.
FIG. 3 is a second schematic diagram of a conventional MOCVD reaction system.
Fig. 4 is a graph showing temperature profiles of different width positions on a shower plate in a conventional MOCVD reaction system, wherein the horizontal axis W represents the width position of the shower plate, and the vertical axis T represents the temperature.
FIG. 5 is a schematic structural diagram of an MOCVD reaction system disclosed in Chinese patent publication No. CN 205329157.
Fig. 6 is a schematic structural diagram of an MOCVD reaction system in the first embodiment of the present application.
Fig. 7 is a comparison graph of temperature profiles of different width positions on the shower plate in the conventional MOCVD reaction system and the first embodiment, in which the horizontal axis W represents the width position of the shower plate, the vertical axis T represents the temperature, the solid line is the first embodiment, and the dotted line is the conventional MOCVD reaction system.
Fig. 8 is a schematic structural diagram of an MOCVD reaction system in the second embodiment of the present application.
Fig. 9 is a cross-sectional view of the upper half of fig. 8.
Fig. 10 is a schematic structural diagram of an MOCVD reaction system in the third embodiment of the present application.
Fig. 11 is a comparison graph of temperature profiles of different width positions on the shower plate in the conventional MOCVD reaction system, the first embodiment, and the third embodiment, in which the horizontal axis W represents the width position of the shower plate, the vertical axis T represents the temperature, the solid line is the third embodiment, the uppermost dotted line is the conventional MOCVD reaction system, and the middle dotted line is the first embodiment.
Wherein: 1-MOCVD reaction chamber, 2-heating substrate, 3-spraying plate, 4-guide plate, 5-cooler, 6-oxygen plate, 7-temperature measuring element, 8-heating element, 9-heat insulation layer, 10-strip winding system, 11-strip, 12-organic source gas inlet, 13-oxygen inlet, 14-spraying chamber, 15-tape reel;
301-organic source gas orifice, 302-source reactant gas flow channel, 303-source reactant gas orifice, 304-source reactant gas secondary flow channel, 305-source reactant gas secondary orifice, 601-oxygen supply orifice.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings of the embodiments of the present application. It should be apparent that the described embodiments are only some of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the application without any inventive step, are within the scope of protection of the application.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this application belongs. The use of the terms "a" or "an" and the like in the description and in the claims of the present application do not denote a limitation of quantity, but rather denote the presence of at least one.
In the description of the present application and claims, the terms "upper", "lower", "horizontal", and the like indicate orientations or positional relationships based on orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of the description, but do not indicate or imply that the referred device or unit must have a specific orientation, be constructed in a specific orientation, and operate, and thus, should not be construed as limiting the present application.
Embodiments of the present application will now be described with reference to the accompanying drawings.
The first embodiment is as follows:
referring to fig. 6, like the conventional MOCVD reaction system, the MOCVD reaction system of the present embodiment also includes: the device comprises an MOCVD reaction chamber 1, a heating substrate 2 arranged in the MOCVD reaction chamber, and a spray plate 3 positioned above the heating substrate. For convenience of description of the technical solution of the present application, the length dimension of the shower plate 3 is defined as a dimension along the traveling direction of the strip 11 (i.e., the inside and outside directions perpendicular to the paper surface in fig. 6) at the time of the deposition work, and the width dimension of the shower plate 3 is defined as a dimension along the width direction of the strip 11 (i.e., the left and right directions parallel to the paper surface in fig. 6) at the time of the deposition work. It is apparent that the width of the shower plate 3 is perpendicular to the length. And the foregoing definitions of shower plate 3 length and width are consistent with conventional understanding in the art.
The key improvement of this embodiment is that the source reaction gas channel 302 is formed in the shower plate 3 and extends along the length direction of the shower plate, and the inner wall surface of the source reaction gas channel 302 is formed with a plurality of source reaction gas nozzles 303 extending downward to the lower surface of the shower plate 3.
When the metal organic source gas spraying device works, the strip is attached to the upper surface of the heating substrate 2 and walks along the length direction of the spraying plate 3, the metal organic source gas supplied at the upstream passes through the spraying plate 3 and is sprayed into an MOCVD reaction cavity from the organic source gas spraying hole 301, and the source reaction gas supplied at the upstream is firstly sent into the source reaction gas flow channel 302 and then is sprayed into the MOCVD reaction cavity from the source reaction gas spraying hole 303. It can be seen that, only the metal organic source gas passes through each organic source gas nozzle hole 301 of the shower plate 3, and the source reactant gas and the metal organic source gas are not mixed before entering the MOCVD reaction chamber, so that the reaction is not possible. The source reaction gas flow channel 302 is disposed in the middle of the shower plate 3, so that the source reaction gas ejected from each source reaction gas ejection hole 303 is first in the middle of the MOCVD reaction chamber, and the pumping holes are disposed on the left and right sides of the non-middle portion of the MOCVD reaction chamber. Therefore, the gas pressure in the middle of the MOCVD reaction chamber is high, the gas pressures on both sides are low, and the source reaction gas just sprayed from the source reaction gas spraying holes 303 can be diffused to both sides (periphery) very naturally, so that the source reaction gas is fully and uniformly mixed and reacted with the metal organic source gas in the MOCVD reaction chamber, and a uniform high-quality superconducting thin film is formed on the surface of the strip.
As with conventional techniques, the source reactant gas is oxygen. Also, in practical use, the temperature of the source reactant gas fed into the source reactant gas flow field 302 does not need to be high, so that it can absorb the temperature of the central region of the shower plate 3. Therefore, the problems that the temperature of the middle part of the traditional spray plate is high and the temperature of the two sides of the traditional spray plate is low due to the fact that the coolers 5 are arranged on the two sides of the traditional spray plate can be solved, namely, the temperature of each part of the spray plate 3 tends to be uniform, and the temperature of the metal organic source gas sprayed from each organic source gas spray hole 301 tends to be equal, as shown in fig. 7.
However, it is known that the flow of oxygen fed into the MOCVD reactor should be adapted to the flow of the source reaction gas in order to obtain the desired superconducting tape quality. In the case of a defined source reactant gas flow, the oxygen flow should also be defined, and it is not possible to reduce the temperature of the supplied oxygen indefinitely in order to balance the temperature throughout the shower plate. In this regard, we have conceived a very smart approach: in practice, not only the necessary oxygen gas but also an inert gas, such as argon, which does not react with the metal organic source gas is introduced into the source reactant gas flow field 302. That is, the source reaction gas may be a mixed gas of oxygen and an inert gas. Therefore, under the condition that the source reaction gas meets the required temperature and the oxygen in the source reaction gas meets the required flow, the flow of the inert gas in the source reaction gas is improved to absorb the heat in the middle of the spray plate 3, so that the temperature in the middle of the spray plate 3 is basically equal to the temperature of the left side part and the right side part of the spray plate 3.
The source reaction gas nozzles 303 are arranged at intervals along the length direction of the source reaction gas flow channel 302, so that the source reaction gas ejected from each source reaction gas nozzle 303 can uniformly flow into the MOCVD reaction chamber, and the production quality of the superconducting tape is further improved.
The lower end orifice of each source reaction gas jet hole 303 is an outward-expanding bell mouth, and when the source reaction gas is discharged from the source reaction gas jet holes 303, the gas pressure suddenly becomes very small, the gas expands to form a very high transverse velocity component, which is helpful for oxygen to diffuse towards two sides.
In order to facilitate the fabrication of the source reaction gas channel 302 in the shower plate 3, the shower plate 3 is thickened in this embodiment to a thickness of 6mm. The source reaction gas flow channel 302 has a diameter of 3mm. The second embodiment:
as shown in fig. 8 and 9, the MOCVD reaction system of the present embodiment has substantially the same structure as that of the first embodiment, except that: in this embodiment, a baffle plate 4 located below each source reaction gas injection hole 303 is fixedly connected to the shower plate 3.
When the device works, the source reaction gas sprayed out of the source reaction gas spray holes 303 flows towards two sides under the blocking of the guide plate 4, and the transverse flow of the source reaction gas, particularly oxygen, is increased.
The width of the guide plate 4 is 3.5mm, which is larger than the diameter of the lower orifice of any source reaction gas jet hole 303. And the guide plate 4 is fixed on the spray plate 3 by locking screws with the diameter of 2 mm.
Example three:
in order to improve the productivity and deposition efficiency, it is desirable that the number of winding system tracks (i.e. the number of heating strip material tracks on the substrate) is as large as possible, but the problems become more and more serious, one of the main problems is the problem of the uniformity of oxygen distribution in the MOCVD reaction chamber, and for the MOCVD reaction system with a very large number of winding system tracks, the problem is to further improve the temperature uniformity of the shower plate 3 and the uniformity of oxygen in the reaction chamber. In this embodiment, two source reactant gas sub-channels 304 respectively located at two radial sides of the source reactant gas channel 302 are further formed in the shower plate 3, and a plurality of source reactant gas sub-orifices 305 extending downward to the lower surface of the shower plate 3 are formed on the inner wall surface of each source reactant gas sub-channel 304, as shown in fig. 10.
In operation, each of the source reactant gas sub-channels 304 is also fed with a source reactant gas comprising oxygen.
In this embodiment, the two source reactant gas sub-channels 304 are disposed in parallel with the source reactant gas channel 302, and the two source reactant gas sub-channels 304 are symmetrically disposed on two radial sides of the source reactant gas channel 302.
The above are exemplary embodiments of the present application only, and are not intended to limit the scope of the present application, which is defined by the appended claims.
Claims (10)
1. An MOCVD reaction system, comprising:
an MOCVD reaction chamber (1);
a heated substrate (2) disposed within the MOCVD reaction chamber;
a shower plate (3) disposed above the heating substrate and having a plurality of organic source gas injection holes (301), the shower plate (3) having a length extending in a traveling direction of the strip and a width perpendicular to the length;
coolers (5) thermally connected to both sides of the width of the shower plate, and
the pumping ports are communicated with the MOCVD reaction cavity and are positioned at two sides of the width of the spraying plate;
the device is characterized in that a source reaction gas channel (302) which is located in the middle of the width of the spray plate and extends along the length direction of the spray plate is formed in the spray plate (3), and a plurality of source reaction gas spray holes (303) which extend downwards to the lower surface of the spray plate (3) are formed in the inner wall surface of each source reaction gas channel (302).
2. The MOCVD reaction system of claim 1, wherein the plurality of source reaction gas orifices (303) are spaced along a length direction of the source reaction gas flow channel (302).
3. The MOCVD reaction system of claim 1, wherein a lower end orifice of at least one of the source reaction gas injection orifices (303) is a flared bell.
4. MOCVD reaction system according to any one of claims 1 to 3, characterized in that a flow guide plate (4) is fixedly connected to the shower plate (3) below the source reaction gas nozzles (303).
5. The MOCVD reaction system of claim 4, wherein the width of the flow guide plate (4) is larger than a lower orifice diameter of any one of the plurality of source reaction gas injection orifices (303).
6. The MOCVD reaction system according to any one of claims 1 to 3, wherein two source reaction gas secondary flow channels (304) respectively located at two radial sides of the source reaction gas flow channel (302) are further formed in the spray plate (3), and a plurality of source reaction gas secondary nozzles (305) extending downward to the lower surface of the spray plate (3) are formed in an inner wall surface of each source reaction gas secondary flow channel (304).
7. A method of using the MOCVD reactor system of any one of claims 1 to 6, comprising:
and introducing mixed gas which is lower in temperature than the spraying plate (3) and is composed of oxygen and inert gas into the source reaction gas flow channel (302), and adjusting the proportion of the inert gas in the mixed gas to enable the temperature of the middle part of the spraying plate (3) to be equal to the temperature of the left side part and the right side part of the spraying plate (3).
8. A shower plate for an MOCVD system, comprising:
an upper surface and a lower surface facing away from each other, an
A plurality of organic source gas injection holes (301) extending from the upper surface to the lower surface;
the device is characterized in that a source reaction gas channel (302) which is located in the middle of the width of the spray plate and extends along the length direction of the spray plate is formed in the spray plate (3), and a plurality of source reaction gas spray holes (303) which extend downwards to the lower surface of the spray plate (3) are formed in the inner wall surface of each source reaction gas channel (302).
9. The shower plate according to claim 8, wherein a baffle plate (4) is fixedly attached to the shower plate (3) below the plurality of source reactant gas injection holes (303).
10. The shower plate according to claim 8, wherein two source reaction gas sub-runners (304) are formed in the shower plate (3) and located at both sides of the source reaction gas runner (302) in the radial direction, and a plurality of source reaction gas sub-orifices (305) extending downward to the lower surface of the shower plate (3) are formed in an inner wall surface of each source reaction gas sub-runner (304).
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011091246.6A CN114351117B (en) | 2020-10-13 | 2020-10-13 | Spray plate, MOCVD reaction system with spray plate and use method of MOCVD reaction system |
| PCT/CN2020/126447 WO2022077637A1 (en) | 2020-10-13 | 2020-11-04 | Spraying plate, mocvd reaction system having spraying plate, and use method thereof |
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| CN202011091246.6A CN114351117B (en) | 2020-10-13 | 2020-10-13 | Spray plate, MOCVD reaction system with spray plate and use method of MOCVD reaction system |
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| CN114990528B (en) * | 2022-05-16 | 2023-11-03 | 武汉理工大学 | Device and method for improving temperature field in cavity of CVD equipment |
| CN115110064A (en) * | 2022-07-15 | 2022-09-27 | 长鑫存储技术有限公司 | Gas input equipment and gas input method |
| CN115206845B (en) * | 2022-07-22 | 2023-03-07 | 盛吉盛半导体科技(北京)有限公司 | Gas inlet device for semiconductor reaction equipment and semiconductor reaction equipment |
| CN115341197B (en) * | 2022-09-15 | 2023-08-11 | 东部超导科技（苏州）有限公司 | Spray cooling integrated plate and spray system for metal organic chemical vapor deposition |
| CN116240525A (en) * | 2022-12-15 | 2023-06-09 | 江苏微导纳米科技股份有限公司 | Spray plate, spray method and treatment device |
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| CN114351117A (en) | 2022-04-15 |
| WO2022077637A1 (en) | 2022-04-21 |
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