CaClx reaction vessel of HVPE equipment and control method for controlling CaClx concentration

Abstract

The invention discloses HVPE equipment and a control method for controlling CaClx concentration, a CaClx reaction container comprises a material storage cavity, the material storage cavity is divided into a plurality of material storage sub-cavities in the horizontal direction, the plurality of material storage sub-cavities are used for containing gallium source liquid, and the gallium source liquid is separated from the material storage sub-cavities in the horizontal direction. When the depth of the gallium source liquid is greater than a preset height, gas flow and reaction spaces which are mutually independent are formed above the liquid level of the gallium source liquid, and the gas flow and reaction spaces are used for flowing chlorine source gas and providing spaces for the reaction of the chlorine source gas and a gallium source; a feeding hole, a liquid outlet and a first air outlet are formed in the cavity wall of each storage sub-cavity, and the first air outlet is positioned above the preset height relative to the bottom wall of the storage sub-cavity and is higher than the liquid outlet. Compared with the prior art, the flow field control capability of the HVPE equipment can be improved, more accurate regional control is realized, and GaClx with different flow rates, gas concentrations and valence states can be output through corresponding reactions.

Description

Technical Field

[0001] The present invention relates to the field of semiconductor substrate material manufacturing, and particularly to an apparatus and method for controlling the GaClx flow field applied in an HVPE apparatus. Background Art

[0002] Gallium nitride (GaN), as a leading material among the third-generation wide-bandgap semiconductor materials, its unique physical and chemical properties make it play an important role in the preparation of blue-light LEDs and high-temperature, high-frequency, high-power electronic devices. The popularization of blue-light LEDs and the development of high-performance electronic devices are both inseparable from the support of GaN materials.

[0003] Among the numerous methods for growing gallium nitride (GaN) single crystals, the hydride vapor phase epitaxy (HVPE) technology stands out with its significant advantages. Its growth rate is high, up to 800 μm / h at most, which makes it possible to mass-produce GaN single crystals. In addition, the production cost of the HVPE technology is relatively low, and the growth process is relatively simple, which is of great significance for reducing production costs, improving production efficiency, and promoting the popularization and application of GaN single crystal technology.

[0004] In an HVPE growth system, gallium chloride gas and ammonia gas undergo a near-equilibrium reaction at high temperature to form gallium nitride crystals. To industrialize GaN single crystals and mass-produce high-quality GaN single crystals, the key lies in obtaining a stable laminar flow field in the reactor. The stability of the laminar flow field is crucial for ensuring the uniformity of GaN single crystal growth, reducing growth defects, and improving crystal quality.

[0005] Generally, during the production process of using HVPE to prepare epitaxial wafer materials, after the precursor gas enters the reaction chamber through the intake pipe, it diffuses and mixes evenly throughout the reaction chamber. At present, a pain point of the HVPE apparatus is that the GaCLx flow field can only be controlled as a whole during the crystal growth process, but the local area cannot be controlled point by point. It is difficult to control the flow field morphology corresponding to the nozzle structure regionally, the process debugging is difficult, and the expansion is not good, resulting in great uncertainty in the quality of the grown single crystal products.

[0006] During the HVPE process, group III nitrides (such as GaN) are formed by the reaction of hot gaseous metal chlorides (such as GaCl) with ammonia gas (NH3) (refer to the following formula).

[0007] The metal chloride is produced by hot HCl gas passing through hot group III metals. All reactions are carried out in a temperature-controlled quartz furnace.

[0008] Generally, the reaction of gallium source and hydrochloric acid:

[0009] For example, hot HCl (gas) + Ga (liquid) ------> GaCl (gas);

[0010] Chemical reactions for gallium nitride growth:

[0011] GaCl (gas) + NH3 (gas) -------> GaN (solid) + HCl (gas) + H2 (gas);

[0012] At high temperatures, the activity of metallic gallium may increase, and the reaction rate with hydrogen chloride may accelerate. At the same time, high temperatures may also affect the stability of gallium chloride in the gaseous or solid state. However, in terms of the chemical equation, the reaction at high temperatures can also be expressed as:

[0013] 6HCl (gaseous) + 2Ga → 2GaCl3 + 3H2↑;

[0014] In high-temperature gaseous reactions, GaCl is more likely to be formed because it is more stable in the gaseous state.

[0015] In existing HVPE equipment, there are usually drawbacks in the flow field, such as poor uniformity of the GaClx gas source and difficulty in regional regulation restricted by the equipment structure. The problem of gas source uniformity here includes the uncontrollability or difficulty in controlling parameters such as different orders of GaClx gas sources, regional flow rates, and dilution concentrations of the gas source.

[0016] How to ensure a stable and controllable GaClx flow field in the reactor has become a technical problem that needs to be urgently solved by those skilled in the art. Summary of the Invention

[0017] The object of the present invention is to provide a CaClx reaction vessel for HVPE equipment and a control method for controlling the CaClx concentration, improve the flow field control ability of the HVPE equipment, achieve more precise regional control, and can output GaClx with different flow rates, gas concentrations, and different valence states through corresponding reactions.

[0018] To achieve the above object, the present invention provides a CaClx reaction vessel for HVPE equipment, including a storage chamber; the storage chamber is horizontally divided into a plurality of storage sub-chambers, and the plurality of storage sub-chambers are used to hold the gallium source liquid, and can form independent gas flow and reaction spaces above the liquid surface of the gallium source liquid when the depth of the gallium source liquid is greater than a preset height. The gas flow and reaction spaces are used to flow the chlorine source gas and provide a space for the reaction between the chlorine source gas and the gallium source; each storage sub-chamber has a feed port, a liquid outlet, and a first gas outlet on its chamber wall, and the first gas outlet is located above the preset height relative to the bottom wall of the storage sub-chamber and higher than the liquid outlet.

[0019] Preferably, the liquid outlet is located below the preset height.

[0020] Preferably, the material storage sub-chambers are separated by a partition on the chamber wall of the material storage chamber, and there is a gap with a preset height between the bottom of the partition and the material storage sub-chambers, so that the gallium source solutions in the multiple material storage sub-chambers are connected. This not only allows the gallium source liquid to be added to all the material storage sub-chambers through one feed port, but also makes the gallium source liquids in all the material storage sub-chambers at the same height.

[0021] Preferably, the CaClx reaction vessel further includes a reaction chamber located below the material storage chamber; the reaction chamber includes a plurality of independent reaction sub-chambers corresponding to the material storage sub-chambers. There is an infusion pipeline between the chamber wall of the material storage sub-chamber and the chamber wall of the corresponding reaction sub-chamber, which is connected to the liquid outlet to transport the gallium source liquid to the reaction sub-chamber. There is a gas transmission pipeline between the chamber wall of the material storage sub-chamber and the chamber wall of the corresponding reaction sub-chamber, which is connected to the first gas outlet to transport the chlorine source gas to the reaction sub-chamber, so that the chlorine source gas and the gallium source liquid react in the reaction sub-chamber to generate CaClx gas; there is a second gas outlet in the reaction sub-chamber for outputting CaClx gas, and the height of the second gas outlet is higher than the bottom wall of the reaction sub-chamber. This solution enables the HCl gas and the gallium source liquid to come into full contact in the reaction sub-chamber and undergo a chemical reaction to generate gallium chloride gas.

[0022] More preferably, a first valve for controlling the on-off of the gallium source liquid is provided on the infusion pipeline.

[0023] Preferably, the infusion pipeline extends into the reaction sub-chamber, and the distance between the outlet of the infusion pipeline and the bottom wall of the reaction sub-chamber is a first distance, and the distance between the second gas outlet and the bottom wall of the reaction sub-chamber is a second distance, and the first distance is lower than the second distance. This solution ensures that when the liquid level of the gallium source liquid is greater than a certain height, the liquid level of the gallium source liquid in the reaction chamber is controlled to be constant due to the balance of water pressure without the need for valve control, enabling the chlorine source gas and the gallium source liquid to come into more sufficient contact in the reaction sub-chamber.

[0024] Specifically, an air outlet pipe communicating with the outside protrudes from the bottom wall of the reaction sub-chamber, and the inlet of the air outlet pipe is the second gas outlet.

[0025] More preferably, the CaClx reaction vessel further includes a gas equalizing chamber, the gas equalizing chamber includes a plurality of independent gas equalizing sub-chambers corresponding to the reaction sub-chambers, and each gas equalizing sub-chamber has a gas equalizing outlet communicating with the outside, and the second gas outlet is correspondingly connected to the gas equalizing sub-chamber. The gas equalizing chamber can make the CaClx gas more uniform.

[0026] Preferably, the gas - equalizing cavity is separated into an upper cavity and a lower cavity by a gas - equalizing partition plate in the up - down direction. The upper cavity is communicated with the second air outlet. An air - equalizing outlet is formed on the cavity wall of the lower cavity, and an air - equalizing through - hole communicating the upper cavity and the lower cavity is provided on the gas - equalizing partition plate.

[0027] Specifically, a pipe fitting protruding upward into the upper cavity is provided on the hole wall of the air - equalizing through - hole, so that the inlet of the air - equalizing through - hole in the upper cavity protrudes on the bottom wall of the upper cavity. This solution can effectively intercept other structures in the CaClx gas that become liquid droplets due to condensation.

[0028] Preferably, the material - storage cavity, the reaction cavity, and the gas - equalizing cavity are separated by partition plates in the up - down direction and are arranged in sequence from top to bottom. A plurality of the reaction sub - cavities are separated from each other by partition plates in the horizontal direction, and a plurality of the gas - equalizing sub - cavities are separated from each other by partition plates in the horizontal direction. The structure is simple and compact.

[0029] Preferably, the CaClx reaction vessel further includes a plurality of nozzles corresponding to the gas - equalizing sub - cavities. The inlets of the nozzles are connected to the air - equalizing outlets, so that the CaClx gas is ejected outward in one direction.

[0030] Specifically, the nozzles are flat - shaped, circular, annular, triangular, etc.

[0031] Preferably, the number of the material - storage sub - cavities is 3, and the number of the reaction sub - cavities is 3.

[0032] Preferably, a plurality of the material - storage sub - cavities and a plurality of the reaction sub - cavities are uniformly separated by cylindrical chambers in the horizontal direction, saving space.

[0033] Preferably, a second valve is installed on the gas - transmission pipeline, which can flexibly and accurately control the air pressure in the material - storage cavity.

[0034] The present invention also provides a control method for controlling the CaClx concentration in an HVPE device. The HVPE device includes an epitaxial cavity, the CaClx reaction vessel as described above, and a carrier for carrying a semiconductor. The carrier is installed in the epitaxial cavity, and the CaClx reaction vessel is installed above the carrier and further includes a plurality of nozzles corresponding to the reaction sub - cavities and communicated with the first air outlet. The control method for controlling the CaClx concentration in the HVPE device includes: injecting a gallium - source liquid into the material - storage cavity from the feed port and making the height of the gallium - source liquid in each material - storage sub - cavity higher than a preset height; injecting a preset flow rate of a chlorine - source gas into each material - storage sub - cavity from the feed port. The preset flow rates of the chlorine - source gas in each material - storage sub - cavity are the same or different, so as to output CaClx gas with different concentrations or different flow rates to the carrier through the nozzles.

[0035] Preferably, while injecting a chlorine source gas into the feed port, a non-chlorine source gas is injected. The non-chlorine source gas is N2 or H2 gas, and the mixing ratio flow field of different valence states in the CaClx gas output by the nozzle is adjusted by controlling the ratio of the HCl gas and the non-chlorine source gas.

[0036] Compared with the prior art, in the CaClx reaction vessel of the present invention, the gas flow and the reaction space in different storage chambers are independent of each other. The CaClx gas with different flow rates and pressures can be controlled by inputting HCl gases with different flow rates and pressures, and the CaClx gas with different valence states can be controlled by inputting HCl gases and chlorine gas with different ratios. x is the valence state of the gallium chloride gas, thereby effectively improving the flow field control ability of the HVPE device and achieving more precise regional control. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 is a perspective view of the CaClx reaction vessel of the HVPE device in an embodiment of the present invention.

[0038] Figure 2 is a cross-sectional view of the CaClx reaction vessel of the HVPE device in an embodiment of the present invention.

[0039] Figure 3 is another cross-sectional view of the CaClx reaction vessel of the HVPE device in an embodiment of the present invention.

[0040] Figure 4 is Figure 3 an enlarged view of part a.

[0041] Figure 5 is still another cross-sectional view of the CaClx reaction vessel of the HVPE device in an embodiment of the present invention.

[0042] Figure 6 is yet another cross-sectional view of the CaClx reaction vessel of the HVPE device in an embodiment of the present invention.

[0043] Figure 7 is a cross-sectional view of the CaClx reaction vessel of the HVPE device in another embodiment of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0044] To describe in detail the technical content, structural features, achieved objectives and effects of the present invention, the following is a detailed description in conjunction with the embodiments and with reference to the drawings.

[0045] Reference Figures 1 to 4, the present invention discloses a CaClx reaction vessel 100 for an HVPE device, which includes an independent and closable housing. A storage cavity 10 is formed inside the housing. The storage cavity 10 is horizontally divided into a plurality of storage sub-cavities 11. The plurality of storage sub-cavities 11 are used to hold a gallium source liquid 200, and when the depth of the gallium source liquid 200 is greater than a preset height, an independent gas flow and reaction space 12 can be formed above the liquid surface of the gallium source liquid 200. The gas flow and reaction space 12 is used to store a chlorine source gas, flow the chlorine source gas, and provide a space for the reaction between the chlorine source gas and the gallium source. The chlorine source gas is a gas containing element Cl for generating CaClx, and the gallium source liquid 200 is a liquid containing element Cl for CaClx. Each of the cavity walls of the storage sub-cavity 11 has a feed port 13, a liquid outlet 14, and a first gas outlet 15. The first gas outlet 15 is located above the preset height relative to the bottom wall of the storage sub-cavity 11 and is higher than the liquid outlet 14. In this embodiment, the chlorine source gas is HCl gas. Of course, other Cl-containing gases can also be selected, not limited to HCl gas, such as chlorine gas.

[0046] Reference Figure 4 , the liquid outlet 14 is located below the preset height. Among them, the storage sub-cavity 11 is separated on the cavity wall of the storage cavity 10 by a partition 110, and there is a gap with a preset height between the bottom of the partition 110 and the storage sub-cavity 11, so that the gallium source solutions 200 in the plurality of storage sub-cavities 11 are connected. Not only can the gallium source liquid be added to all the storage sub-cavities 11 through one feed port 13, but also the gallium source liquids 200 in all the storage sub-cavities 11 can be at the same height.

[0047] Specifically, referring to Figure 5 , the number of the storage sub-cavities 11 is 3. Of course, the number of the storage sub-cavities 11 is not limited to 3, and can also be 2, 4, 5, etc. Preferably, in this embodiment, the plurality of storage sub-cavities 11 are evenly separated by a cylindrical chamber in the horizontal direction, saving space.

[0048] Reference Figure 2 and Figure 3 , the feed ports 13 are respectively formed on the top walls of the corresponding storage sub-cavities 11, the first gas outlets 15 are opened on the side walls of the corresponding storage sub-cavities 11, and the liquid outlets 14 are opened on the bottom walls of the storage sub-cavities 11. Of course, the gas inlet can also be arranged on the side wall of the storage sub-cavity 11, and the liquid outlet 14 can also be arranged on the side wall of the storage sub-cavity 11 or protrude on the bottom wall of the storage sub-cavity 11, preferably below the preset height.

[0049] Reference Figure 2 and Figure 3, the CaClx reaction vessel 100 further includes a reaction chamber 20 located below the storage chamber 10. A reaction chamber 20 is also formed inside the housing. The reaction chamber 20 includes a plurality of independent reaction sub-chambers 21 corresponding to the storage sub-chambers 11. There is an infusion pipeline 61 between the chamber wall of the storage sub-chamber 11 and the chamber wall of the corresponding reaction sub-chamber 21, which is communicated with the liquid outlet 14 to convey the gallium source liquid to the reaction sub-chamber 21. There is a gas transmission pipeline 62 between the chamber wall of the storage sub-chamber 11 and the chamber wall of the corresponding reaction sub-chamber 21, which is communicated with the first gas outlet 15 to convey HCl gas to the reaction sub-chamber 21, so that the HCl gas and the gallium source liquid react in the reaction sub-chamber 21 to generate CaClx gas. A first valve for controlling the on-off of the gallium source liquid is provided on the infusion pipeline 61.

[0050] Wherein, a second gas outlet 22 for outputting CaClx gas is provided in the reaction sub-chamber 21. The height of the second gas outlet 22 is higher than the bottom wall of the reaction sub-chamber 21, so that the gallium source liquid can be contained in the reaction sub-chamber 21. Furthermore, the HCl gas and the gallium source liquid can be in full contact in the reaction sub-chamber 21 and undergo a chemical reaction to generate gallium chloride gas.

[0051] Wherein, an air outlet pipe 23 communicating with the outside is convexly provided on the bottom wall of the reaction sub-chamber 21, and the inlet of the air outlet pipe 23 is the second gas outlet 22.

[0052] Wherein, the infusion pipeline 61 extends into the reaction sub-chamber 21, and the distance between the outlet of the infusion pipeline 61 and the bottom wall of the reaction sub-chamber 21 is a first distance, and the distance between the second gas outlet 22 and the bottom wall of the reaction sub-chamber 21 is a second distance. The first distance is lower than the second distance. This solution enables the liquid level of the gallium source liquid in the reaction sub-chamber 21 to be greater than a certain height, and the liquid level of the gallium source liquid in the reaction chamber 20 can be kept constant due to the air pressure of the hydrogen chloride gas, so that the HCl gas and the gallium source liquid can be in more sufficient contact in the reaction sub-chamber 21.

[0053] In this embodiment, the number of reaction sub-chambers 21 is equal to and corresponds one by one to the number of storage sub-chambers 11. The number of reaction sub-chambers 21 is 3.

[0054] Preferably, the reaction sub-chambers 21 are evenly separated by cylindrical chambers in the horizontal direction, saving space. Specifically, the partition plates between the reaction sub-chambers correspond to the partition plates between the storage sub-chambers 11.

[0055] Reference Figure 2 and Figure 3The CaClx reaction container 100 also includes a uniform gas chamber 30, which includes a plurality of uniform gas chambers 31 corresponding to the reaction chamber 21 and independent of each other, and each of the uniform gas chambers 31 has a uniform gas outlet 32 ​​connected to the outside on the chamber wall, and the second gas outlet 22 is connected to the uniform gas chamber.

[0056] The gas uniformity outlet 32 ​​is provided on the bottom wall of the gas uniformity chamber 31, and the opening for communicating the gas uniformity chamber 31 with the second gas outlet 22 is provided on the top wall of the gas uniformity chamber 31, so as to facilitate the flow of CaClx gas from bottom to top.

[0057] More preferably, the uniform gas chamber 31 is divided into an upper chamber 311 and a lower chamber 312 along the up and down directions by a uniform gas baffle 313, the upper chamber 311 is connected to the second air outlet, a uniform gas outlet 32 ​​is provided on the wall of the lower chamber 312, and the uniform gas baffle 313 has a uniform gas through hole 314 connecting the upper chamber 311 and the lower chamber 312.

[0058] Specifically, the hole wall of the gas uniforming hole 314 is protruded upward with a pipe 315 extending into the upper chamber 311, so that the gas uniforming hole 314 is protruded on the bottom wall of the upper chamber 311 at the entrance of the upper chamber 311. This solution can effectively intercept other structures mixed in the CaClx gas that become droplets due to condensation.

[0059] refer to Figure 1 , Figure 2 and Figure 6 The CaClx reaction container 100 further includes a plurality of nozzles 40 corresponding to the uniform gas chambers, and the inlets of the nozzles 40 are connected to the uniform gas outlets 32, so that the CaClx gas is ejected outward in one direction.

[0060] Among them, the storage chamber 10, the reaction chamber 20, and the uniform gas chamber 30 are separated by partitions in the up and down directions, and the shell is provided with multiple partitions in the up and down directions to separate the storage chamber 10, the reaction chamber 20, and the uniform gas chamber 30, and the uniform gas chamber 30 can also be divided in the up and down directions to separate a first uniform gas chamber composed of multiple upper chambers 311 and a second uniform gas chamber composed of multiple lower chambers 312. The first uniform gas chamber is divided into multiple upper chambers 311 in the horizontal direction, and the second uniform gas chamber is divided into multiple lower chambers 312 in the horizontal direction.

[0061] Therefore, the storage chamber 10, the reaction chamber 20, and the uniform gas chamber 30 are arranged in sequence from top to bottom, and the multiple reaction chambers 21 are separated from each other by partitions in the horizontal direction, and the multiple uniform gas chambers are separated from each other by partitions in the horizontal direction, and the structure is simple and compact.

[0062] Among them, the positions of the partition plates of the material storage cavity 11, the reaction cavity 20, and the upper separation cavity 311 correspond in the horizontal direction, and the separation method of the lower separation cavity 312 in the horizontal direction corresponds to the distribution of the nozzles 40. Refer to Figure 6 , in this embodiment, the nozzles 40 are flat and arranged side by side at equal intervals. A plurality of lower separation cavities 312 divide a circular area into a plurality corresponding to the material storage sub-cavities 11 and are arranged side by side.

[0063] Of course, the shape of the nozzles 40 is not limited to flat, and can also be circular or other shapes, such as square, triangular or annular, etc.

[0064] Among them, a second valve is installed on the gas transmission pipeline 62, which can flexibly and accurately control the air pressure in the material storage cavity 10.

[0065] Refer to Figure 7 , different from the above embodiment, in another embodiment, the liquid outlet 14 is not directly opened on the bottom wall of the material storage sub-cavity 11, but protrudes from the bottom wall of the material storage sub-cavity 11 through a pipeline, so that the liquid outlet 14 is located above the bottom wall and has a spacing from the bottom wall. In this embodiment, the air equalizing through hole 314 between the upper separation cavity 311 and the lower separation cavity 312 is a through hole opened on the partition plate 313, and no pipe fitting 16 protruding into the upper separation cavity 311 is provided thereon.

[0066] Refer to Figures 1 to 7 , describe the working process of the CaClx reaction vessel 100 of the HVPE device of the present invention, including the following steps:

[0067] (1) Inject gallium source liquid into the material storage cavity 10 from the feed port 13 so that the height of the gallium source liquid in each material storage sub-cavity 11 is higher than a preset height, so that a gas flow and reaction space 12 is formed on the material storage sub-cavity 11, and the gas flow and reaction spaces 12 of the plurality of material storage sub-cavities 11 are independent and isolated from each other.

[0068] (2) Inject a preset flow rate of HCl gas into the gas flow and reaction space 12 of each material storage sub-cavity 11 from the feed port 13, and the HCl gas is contained in the gas flow and reaction space 12. Among them, different gas flow and reaction spaces 12 can maintain environments of HCl gas with different concentrations and / or air pressures according to needs. In the gas flow and reaction space 12, the HCl gas and the gallium source liquid will undergo a preliminary reaction.

[0069] (3) Open the first valve so that the gallium source liquid is injected into the reaction sub-cavity 21 through the liquid outlet 14 and the liquid infusion pipeline 61 and is filled to a certain liquid level height in the reaction sub-cavity 21. Of course, the gallium source liquid can also be automatically flowed into the reaction sub-cavity 21 by water pressure control and the liquid level can be constantly maintained at a certain height.

[0070] (4) HCl gas enters the reaction sub - chamber 21 through the first gas outlet 15 and the gas transmission pipeline 61. In the reaction sub - chamber 21, the concentration of HCl gas in the storage sub - chamber 11 affects the flow rate and air pressure of the HCl gas flowing into the reaction sub - chamber 21. The flow rate and air pressure of the HCl gas in multiple reaction sub - chambers 21 can be adjusted according to the concentration and air pressure of the HCl gas in the storage sub - chamber 11, so that the HCl gas and the gallium source liquid can repeatedly and fully contact under different physical environments to react: hot HCl (gas) + Ga (liquid) ------> GaClx (gas), thus generating gallium chloride gas (CaClx gas), where x is the valence of gallium in the gallium chloride gas and can be 1, 3 or other valence states.

[0071] (5) The CaClx gas enters the first gas - equalizing sub - chamber 311 along the second gas outlet 22. After preliminary mixing in the first gas - equalizing sub - chamber 311, it passes through the gas - equalizing through - holes 314 and enters the first gas - equalizing sub - chamber 312 for further full mixing, so that the gallium chloride gases with different valence states in the CaClx gas are repeatedly mixed.

[0072] (6) The fully - mixed CaClx gas passes through the gas - equalizing outlet 32 and enters the nozzle 40, and then is sprayed from the nozzle 40 onto the carrier. Different nozzles 40 can output CaClx gas with different flow rates and air pressures, so as to obtain a variety of controllable flow fields of the CaClx gas through multiple output airflows with different sizes.

[0073] In summary, the present invention divides the gas path of the original mixed CaClx gas into multiple gas paths (3 in this embodiment), realizing the refinement of the local flow field control of the gallium chloride gas in the HVPE device. Among them, each gas path is a closed and independent gas path to realize the control of the flow rate and air pressure of the output gallium chloride gas by the flow rate and air pressure of the input hydrogen chloride gas.

[0074] Preferably, while inputting gallium chloride gas through the feed port 13, chlorine gas with a set proportion can be mixed, so as to adjust the valence proportion of the generated gallium chloride gas in the reaction sub - chamber 21, that is, the proportion of the x values of different valence states in the gallium chloride gas.

[0075] Compared with the prior art, in the CaClx reaction vessel 100 of the present invention, the gas flow and the reaction space 12 in different storage sub - chambers 11 are independent of each other. Different flow rates and air pressures of the CaClx gas output from the CaClx reaction vessel 100 can be controlled by inputting HCl gas with different flow rates and air pressures, and different valence states of the CaClx gas output from the CaClx reaction vessel 100 can also be controlled by inputting HCl gas and chlorine gas with different proportions, where x is the valence of the gallium chloride gas.

[0076] The present invention also discloses a control method for controlling the concentration of CaClx in an HVPE device. The HVPE device includes an epitaxial chamber, the CaClx reaction vessel 100 as described above, and a carrier for carrying a semiconductor. The carrier is installed in the epitaxial chamber, and the CaClx reaction vessel 100 is installed above the carrier and further includes a plurality of nozzles 40 corresponding to the reaction sub-chamber 21 and communicating with the first gas outlet 15.

[0077] The control method for controlling the concentration of CaClx in the HVPE device includes: injecting a gallium source liquid into the storage chamber 10 from the feed inlet 13 such that the height of the gallium source liquid in each storage sub-chamber 11 is higher than a preset height; injecting a preset flow rate of HCl gas into each storage sub-chamber 11 from the feed inlet 13, and the preset flow rates of the HCl gas in each storage sub-chamber 11 are the same or different, so as to output CaClx gas with different concentrations to the carrier through the nozzles, thereby obtaining a plurality of CaClx flow fields with different outputs, and further obtaining different distributions of the CaClx concentration in space, realizing a higher-precision concentration control of GaClx.

[0078] Among them, the CaClx gas output from the nozzle diffuses around, and the flow field change is controlled by controlling the flow velocity of each outlet of the nozzle to realize the control of the flow field morphology. For example, it gradually diffuses from the nozzle 40 to the carrier and slowly diffuses from the flat surface of the carrier to the periphery. At the same time, the rotation of the carrier is controlled to make the growth of the epitaxial layer on the carrier more uniform.

[0079] Among them, the carrier includes a plurality of semiconductor growth trays (such as graphite trays). Of course, different from this, the carrier can also be one, and there are a plurality of chip slots for installing growth substrates on the carrier. Preferably, a plurality of nozzles can correspond to a plurality of growth trays.

[0080] Among them, when injecting HCl gas into the feed inlet 13, a non-chlorine source gas is injected at the same time. The non-chlorine source gas is N2 or H2 gas, and the mixing ratio flow field of different valence states in the CaClx gas output from the nozzle is adjusted by controlling the ratio of the HCl gas and chlorine gas.

[0081] Furthermore, when the nozzle 40 outputs CaClx gas with a corresponding concentration to the growth substrate on the carrier, other gas paths (not shown in the figure) output ammonia gas (NH3) to the growth substrate on the carrier, and then the CaClx gas and ammonia gas react: GaCl (gas) + NH3 (gas) ---> GaN (solid) + HCl (gas) + H2 (gas), so as to deposit solid GaN on the growth substrate.

[0082] The above-disclosed are only the preferred embodiments of the present invention. Certainly, the scope of rights of the present invention cannot be limited thereby. Therefore, equivalent changes made according to the scope of the patent application of the present invention still fall within the scope covered by the present invention.

Claims

1. A CaClx reaction vessel for HVPE equipment, characterized in that: including a storage cavity; The storage chamber is divided into a plurality of storage sub-chambers in the horizontal direction, and the plurality of storage sub-chambers are used to hold gallium source liquid, and can form mutually independent gas flow and reaction spaces above the liquid surface of the gallium source liquid when the depth of the gallium source liquid is greater than a preset height, and the gas flow and reaction spaces are used to flow chlorine source gas and provide space for the chlorine source gas to react with the gallium source; A material inlet, a liquid outlet and a first air outlet are provided on the cavity wall of each material storage cavity. The first air outlet is located above the preset height relative to the bottom wall of the material storage cavity and higher than the liquid outlet.

2. The CaClx reaction vessel according to claim 1, characterized in that: The liquid outlet is located below the preset height.

3. The CaClx reaction vessel according to claim 1, characterized in that: The material storage chambers are separated by partitions on the chamber walls of the material storage chambers, and a gap of a preset height is provided between the bottom of the partitions and the material storage chambers so as to allow the gallium source solutions in the plurality of material storage chambers to communicate.

4. The CaClx reaction vessel according to claim 1, characterized in that: Also included is a reaction chamber located below the storage chamber; The reaction chamber comprises a plurality of mutually independent reaction sub-chambers corresponding to the material storage sub-chambers, a liquid delivery pipeline connected with the liquid outlet to deliver the gallium source liquid to the reaction sub-chamber is provided between the chamber wall of the material storage sub-chamber and the chamber wall corresponding to the reaction sub-chamber, and a gas delivery pipeline connected with the first gas outlet to deliver the chlorine source gas to the reaction sub-chamber is provided between the chamber wall of the material storage sub-chamber and the chamber wall corresponding to the reaction sub-chamber, so that the chlorine source gas and the gallium source liquid react in the reaction sub-chamber to generate CaClx gas; The reaction chamber has a second gas outlet for outputting CaClx gas, and the height of the second gas outlet is higher than the bottom wall of the reaction chamber.

5. The CaClx reaction vessel according to claim 4, characterized in that: The liquid infusion pipeline extends into the reaction chamber, and the distance between the outlet of the liquid infusion pipeline and the bottom wall of the reaction chamber is a first distance, and the distance between the second gas outlet and the bottom wall of the reaction chamber is a second distance, and the first distance is lower than the second distance.

6. The CaClx reaction vessel according to claim 4, characterized in that: The liquid infusion pipeline is provided with a first valve for controlling the on-off of the gallium source liquid.

7. The CaClx reaction vessel according to claim 4, characterized in that: An air outlet pipe communicating with the outside is protruded on the bottom wall of the reaction chamber, and the inlet of the air outlet pipe is the second air outlet.

8. The CaClx reaction vessel according to claim 4, characterized in that: It also includes a gas homogenizing chamber, which includes a plurality of gas homogenizing chambers corresponding to the reaction chambers and independent of each other, each gas homogenizing chamber has a gas homogenizing outlet connected to the outside on the chamber wall, and the second gas outlet is connected to the corresponding gas homogenizing chamber.

9. The CaClx reaction vessel of claim 8, wherein: The uniform gas chamber is divided into an upper chamber and a lower chamber by a uniform gas partition along the up and down directions. The upper chamber is connected to the second air outlet. A uniform gas outlet is provided on the chamber wall of the lower chamber. The uniform gas partition has a uniform gas through hole connecting the upper chamber and the lower chamber.

10. The CaClx reaction vessel according to claim 9, characterized in that: The hole wall of the gas uniforming hole is protruded upwardly with a pipe member extending into the upper chamber, so that the gas uniforming hole is protruded on the bottom wall of the upper chamber at the entrance of the upper chamber.

11. The CaClx reaction vessel of claim 8, wherein: The material storage chamber, reaction chamber, and gas homogenizing chamber are arranged in sequence from top to bottom and separated by partitions. The multiple reaction chambers are separated from each other by partitions in the horizontal direction, and the multiple gas homogenizing chambers are separated from each other by partitions in the horizontal direction.

12. The CaClx reaction vessel of claim 8, wherein: It also includes a plurality of nozzles corresponding to the gas-uniform chambers, and the inlets of the nozzles are connected to the gas-uniform outlets.

13. The CaClx reaction vessel according to claim 12, characterized in that: The nozzle is flat, circular, annular or triangular.

14. The CaClx reaction vessel of claim 1, wherein: The number of the material storage sub-chambers is 3, and the number of the reaction sub-chambers is 3.

15. The CaClx reaction vessel of claim 1, wherein: The plurality of material storage sub-chambers and the plurality of reaction sub-chambers are formed by evenly dividing cylindrical chambers in the horizontal direction.

16. A method for controlling CaClx concentration in an HVPE device, the HVPE device comprising an epitaxial chamber, a CaClx reaction container according to any one of claims 1 to 15, and a carrier for carrying a semiconductor wafer, the carrier being installed in the epitaxial chamber, the CaClx reaction container being installed above the carrier and further comprising a plurality of nozzles corresponding to the reaction chambers and connected to the first gas outlet; characterized in that: include: Inject gallium source liquid into the storage chamber from the feed inlet and make the height of the gallium source liquid in each storage chamber higher than a preset height; A chlorine source gas of a preset flow rate is injected into each of the storage chambers from the feed port, and the preset flow rate of the chlorine source gas in each of the storage chambers is the same or different, so that CaClx gas of different concentrations or different flow rates is output to the carrier through the nozzle.

17. The method for controlling the concentration of CaClx in the HVPE equipment according to claim 16, characterized in that: A non-chlorine source gas is injected into the feed port at the same time, wherein the non-chlorine source gas is N2 or H2 gas, and the mixing ratio flow field of different valence states in the CaClx gas output by the nozzle is adjusted by controlling the ratio of the HCl gas and the non-chlorine source gas.

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