Solid precursor feeding device and chemical vapor deposition system

Abstract

The utility model relates to the technical field of CVD (Chemical Vapor Deposition) ceramic coatings, in particular to a feeding device of a solid precursor and a chemical vapor deposition system. The feeding device of the solid precursor comprises an inert gas replacement part, a feeding part and a protective gas part, the inert gas replacement part is used for containing a solid precursor and replacing the atmosphere where the solid precursor is located with inert gas; the feeding part is used for receiving the solid precursor in the inert gas and conveying the solid precursor to the deposition furnace body; the protective gas part is used for enabling at least part of the feeding part to be located in protective gas. According to the embodiment of the invention, air carried by the solid precursor can be actively removed by adopting the inert gas replacement part, and the protective gas part enables a part of or the whole feeding part to be in a protective gas atmosphere, so that air invasion caused by leakage points is avoided, the content of air entering the deposition furnace body is further reduced, the oxygen content of water is reduced, and the deposition efficiency is improved. And further, the quality of the chemical vapor deposition ceramic coating can be improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of CVD deposition ceramic coating, and particularly relates to a feeding device of solid-state precursor and a chemical vapor deposition system. BACKGROUND

[0002] In the growth and epitaxy process of the third generation of wide band gap semiconductor single crystals (such as SiC, GaN and AlN), high temperature and corrosive atmosphere are often accompanied. The related growth and epitaxy equipment needs to have the characteristics of high temperature resistance and chemical corrosion resistance, and high-purity graphite becomes the only choice. However, even if the graphite material, it will be eroded by gas media such as Si vapor, NH3, H2 and Cl2 at high temperature. In order to improve the service life of the graphite, an effective method is to prepare ceramic coatings such as hafnium carbide (HfC), tantalum carbide (TaC), zirconium carbide (ZrC) and solid solutions therebetween on the graphite. The preparation methods of the graphite-based ceramic coating include slurry-sintering method, plasma spraying method, sol-gel method, physical vapor deposition method (PVD), chemical vapor deposition method (CVD) and chemical vapor infiltration method (CVI) and the like.

[0003] When the ceramic coating is prepared on the graphite by using the CVD process, taking the preparation of the ceramic coatings such as hafnium carbide (HfC), tantalum carbide (TaC) and zirconium carbide (ZrC) as an example, the precursors (such as HfCl4, TaCl5, TaF5, ZrCl4 and ZrF4) are solid particles at normal temperature and pressure. At present, the powder feeding device can be used to transport the precursor powder into the reaction furnace cavity. However, the precursor powder transported into the reaction furnace cavity by the powder feeding device will carry a large amount of air. The water vapor and oxygen in the air will cause the oxidation of the ceramic coating obtained by chemical vapor deposition, and the water and oxygen will also corrode the graphite electrode, the heat preservation felt and the like in the reaction furnace cavity, causing irreversible damage. In addition, the precursors are mostly metal chloride or fluoride salt substances, which have strong hygroscopicity, and the presence of water vapor will promote the hydrolysis thereof, and the hydrolysis product (namely HCl and HF) has strong corrosiveness and toxicity, which will cause great harm to the equipment and personnel.

[0004] It should be noted that the above content is not necessarily prior art, and is not used to limit the patent protection scope of the present application. CONTENT OF THE UTILITY MODEL

[0005] The embodiments of the present application provide a feeding device of solid-state precursor and a chemical vapor deposition system to solve or alleviate one or more technical problems proposed above.

[0006] As one aspect of the embodiments of the present application, the embodiments of the present application provide a feeding device of solid-state precursor, comprising:

[0007] An inert gas replacement part for containing the solid precursor and replacing the atmosphere in which the solid precursor is located with inert gas;

[0008] A feeding part for receiving the solid precursor in the inert gas and transporting the solid precursor to the deposition furnace;

[0009] A protective gas part for placing at least part of the feeding part in a protective gas.

[0010] In the first aspect of the present application, the inert gas replacement part can actively remove the air carried by the solid precursor, and the protective gas part places part or the whole feeding part in a protective gas atmosphere, avoiding the invasion of air due to the existence of leakage points, further reducing the air content entering the deposition furnace, thereby reducing the water vapor content, and thus improving the quality of the chemical vapor deposition ceramic coating.

[0011] Optionally, the feeding device of the solid precursor further comprises a flow rate adjusting part for adjusting the flow rate of the solid precursor into the feeding pipe. Thus, the powder feeding rate can be quantitatively adjusted to realize quick response of powder feeding opening and closing.

[0012] The second aspect of the present application provides a chemical vapor deposition system, comprising a deposition furnace and the feeding device of the solid precursor of the first aspect; the feeding device of the solid precursor is used to feed the solid precursor into the deposition furnace. Thus, the interference of water and oxygen on chemical vapor deposition can be greatly reduced. BRIEF DESCRIPTION OF DRAWINGS

[0013] In the drawings, like reference numerals refer to like elements throughout the various drawings. The drawings are not necessarily to scale, emphasis instead being placed on illustrating principles of the application. It should be understood that the drawings are merely depictions of some embodiments in accordance with the present disclosure and should not be construed as limiting the scope of the application.

[0014] Figure 1 is a structural schematic diagram of the feeding device of the solid precursor provided by the present application;

[0015] Figure 2 is a top view of the distribution tray provided by the present application;

[0016] Figure 3 is a top view of the distribution tray provided by another embodiment of the present application;

[0017] Figure 4 is a top view of the distribution tray provided by another embodiment of the present application;

[0018] Figure 5 is a top view of the distribution tray provided by another embodiment of the present application;

[0019] BRIEF DESCRIPTION OF DRAWINGS

[0020] 1 - replacement cabin; 2 - inert gas inlet; 3 - pressure gauge; 4 - pump; 5 - hopper; 6 - hopper cover; 7 - feeding pipeline; 8 - feeding pipeline; 9 - distribution disc; 10 - sealing cabin; 11 - pressure sensor; 12 - oxygen monitoring device; 13 - water content monitoring device; 14 - gas inlet; 15 - gas outlet; 16 - deposition furnace body; 01 - first valve; 02 - second valve; 03 - third valve; 04 - fourth valve; 05 - fifth valve; 06 - sixth valve; 07 - seventh valve; 08 - eighth valve. DETAILED DESCRIPTION

[0021] In order to make the purposes, technical solutions and advantages of the present application clearer, the present application will be further described in detail below with reference to the drawings and examples. It should be noted that the examples in the present application and the features in the examples can be combined with each other without conflict. The present application will be described in detail below with reference to the drawings and examples.

[0022] It should be noted that the terms "first", "second" and the like in the description and claims of the present application and the above drawings are used to distinguish similar objects, and do not necessarily indicate a specific order or sequence. It should be understood that the terms thus used can be interchanged under appropriate circumstances, so that the embodiments of the present application described herein can be implemented in an order other than that illustrated or described herein. In addition, the terms "include" and "have" and any variations thereof are intended to cover non-exclusive inclusion, for example, a process, method, system, product or device that includes a series of steps or units does not necessarily have to include only those steps or units clearly listed, but can include other steps or units that are not clearly listed or inherent to such a process, method, product or device.

[0023] In the present application, when a numerical interval (i.e., a numerical range) is involved, the distribution of the optional numbers in the numerical interval is considered to be continuous and includes both numerical endpoints (i.e., the minimum value and the maximum value) of the numerical interval and each number between the two numerical endpoints, unless otherwise specified. When a numerical interval refers only to integers within the numerical interval, including both endpoint integers and each integer between the two endpoints, it is equivalent to directly listing each integer, unless otherwise specified. When multiple numerical ranges are provided to describe a feature or characteristic, the numerical ranges can be combined. In other words, unless otherwise indicated, the numerical ranges disclosed in the present application should be understood to include any and all sub-ranges encompassed therein. The "numbers" in the numerical interval can be any quantitative value, such as a number, a percentage, a ratio, etc. The "numerical interval" is intended to broadly include quantitative intervals such as percentage intervals, ratio intervals, and value intervals.

[0024] The embodiment of the present application provides a feeding device of solid-state precursor and a chemical vapor deposition system technical scheme. Based on this, the problem of excessive air carried by the solid-state precursor causing oxidation of the deposited ceramic coating is solved. See the following.

[0025] In the following, exemplary embodiments according to the present application will be described in more detail with reference to the accompanying drawings. It should be understood that these exemplary embodiments can be implemented in many different forms and should not be construed as being limited to the embodiments set forth herein.

[0026] The first aspect of the embodiment of the present application provides a feeding device of solid-state precursor.

[0027] In some embodiments, the feeding device of solid-state precursor comprises an inert gas replacement part, a feeding part, and a protective gas part.

[0028] In an optional embodiment, the inert gas replacement part is used to hold the solid-state precursor and replace the atmosphere in which the solid-state precursor is located with inert gas. In this way, a large amount of air carried in the solid-state precursor can be replaced with inert gas, avoiding a series of problems caused by subsequent air entering the deposition furnace body 16.

[0029] Optionally, the inert gas replacement part comprises a replacement cabin 1, the top of the replacement cabin 1 is provided with a feeding port, the bottom of the replacement cabin 1 is provided with a discharging port, the replacement cabin 1 is provided with an inert gas inlet port 2 and a pressure gauge 3, and the replacement cabin 1 is further connected with a pump 4. In this way, the solid-state precursor can enter the replacement cabin 1 through the feeding port, the replacement cabin 1 is pumped to a vacuum state by the pump 4, and then the inert gas is filled through the inert gas inlet port 2 until the air pressure in the replacement cabin 1 is one atmosphere. The real-time pressure in the replacement cabin 1 can be obtained by observing the pressure gauge 3.

[0030] Further, the first valve 01 is arranged on the connecting pipeline between the hopper 5 and the feeding port; the first inert gas source is connected to the inert gas inlet, and the second valve 02 is arranged on the connecting pipeline between the inert gas inlet and the inert gas source; the third valve 03 is arranged on the connecting pipeline between the displacement cabin 1 and the pump 4; the discharge pipeline is arranged on the discharge port, and the fourth valve 04 is arranged on the discharge pipeline. In this way, the third valve 03 is in an open state, and the first valve 01, the second valve 02 and the fourth valve 04 are in a closed state, so that the vacuumizing can be performed; the second valve 02 is in an open state, and the first valve 01, the third valve 03 and the fourth valve 04 are in a closed state, so that the inert gas can be filled; correspondingly, the first valve 01 and the fourth valve 04 can be controlled to be opened and closed so as to control the feeding and discharging.

[0031] Optionally, the hopper 5 is arranged at the feeding port. In this way, the feeding can be performed through the hopper 5.

[0032] Optionally, the hopper door 6 is arranged on the hopper 5.

[0033] In the optional embodiment, the feeding part is used for receiving the solid precursor in the inert gas and conveying the solid precursor to the deposition furnace body 16; in this way, the solid precursor is sent into the deposition furnace body 16.

[0034] In some specific embodiments, the feeding part includes the feeding pipeline 7 and the feeding pipeline 8; one end of the feeding pipeline 7 is connected to the discharge pipeline, and the other end of the feeding pipeline 7 is connected to the feeding pipeline 8; one end of the feeding pipeline 8 is used for connecting the feeding gas source, and the other end of the feeding pipeline 8 is used for connecting the deposition furnace body 16. In this way, the discharge pipeline of the inert gas displacement part enters the feeding pipeline 8 through the feeding pipeline 7, and the solid precursor in the feeding pipeline 8 can be blown into the deposition furnace body 16 through the feeding gas.

[0035] Optionally, the feeding gas can be argon or / and nitrogen.

[0036] Further, the fifth valve 05 is arranged on the feeding pipeline 8 connected to the feeding gas source, so as to control the on-off of the feeding gas source.

[0037] Further, the sixth valve 06 is arranged on the feeding pipeline 8 connected to the deposition furnace body 16, so as to control the on-off of the feeding pipeline 8 and the deposition furnace body 16.

[0038] In the optional embodiment, the protective gas part is used for making at least part of the feeding part in the protective gas. In this way, the whole or part of the feeding part is made in the protective gas, so as to prevent the additional introduction of air due to the leakage point.

[0039] In some embodiments, the protective gas part comprises a sealed cabin 10, and the sealed cabin 10 is provided with a pressure sensor 11, an oxygen monitoring device 12 and a water content monitoring device 13; the oxygen monitoring device 12 is used to monitor the oxygen content in the sealed cabin 10 and maintain the oxygen content below a first preset value; the water content monitoring device 13 is used to monitor the water content in the sealed cabin 10 and maintain the water content below a second preset value; the sealed cabin 10 is provided with an air inlet 14 connected with a second inert gas source; and the sealed cabin 10 is provided with an air outlet 15. Thus, the presence of the oxygen monitoring device 12 and the water content monitoring device 13 can realize the control of the oxygen content and the water content, so as to make the feeding part in the protective gas and prevent the feeding part from introducing additional air due to the leakage point.

[0040] It is worth noting that the inert gas in the first inert gas source and the second inert gas source is a gas that does not affect CVD and does not react with each mechanism in the deposition furnace body 16. Alternatively, the first inert gas source and the second inert gas source are independently argon or / and nitrogen.

[0041] Further, the oxygen monitoring device 12 can be composed of an oxygen probe and an oxygen removal device. The oxygen probe is used to detect the oxygen content, and when the oxygen content is detected to be higher than the first preset value, the oxygen removal device works to remove oxygen until the oxygen content is below the first preset value.

[0042] Further, the oxygen probe can be an oxygen meter; and the oxygen removal device can adopt an oxygen adsorption tower, which is provided with a heating coil and high-purity iron powder or / and copper powder. The iron powder and the copper powder can combine with oxygen to form iron oxide and copper oxide when heated, so as to achieve the purpose of removing oxygen.

[0043] Further, the water content monitoring device 13 can be composed of a water probe and a water removal device. The water probe is used to detect the water content, and when the water content is detected to be higher than the second preset value, the water removal device works to remove water until the water content is below the second preset value.

[0044] Further, the water probe can be a humidity meter; and the water removal device can adopt a water absorption tower provided with molecular sieve to efficiently absorb water.

[0045] Further, the air inlet 14 is provided with a seventh valve 07, and the air outlet 15 is provided with an eighth valve 08. Optionally, the seventh valve 07 and the eighth valve 08 are both solenoid valves. Thus, the automatic control of the pressure in the sealed cabin 10 can be realized through the combination of the pressure sensor 11, the seventh valve 07 and the eighth valve 08.

[0046] Preferably, the pressure in the sealed cabin 10 is higher than one atmosphere to prevent external air from entering.

[0047] In some embodiments, the solid precursor feeding device further comprises a flow rate adjusting part for adjusting the flow rate of the solid precursor into the feeding pipe 7. Thus, the feeding rate can be quantitatively adjusted, and the feeding can be quickly turned on and off.

[0048] Optionally, the flow rate adjusting part comprises a rotating distribution disc 9 provided with a plurality of through holes; the distribution disc 9 is arranged at the connection between the feeding pipe 7 and the discharging pipe, and when the through hole of the distribution disc 9 is located at the connection between the feeding pipe 7 and the discharging pipe, the discharging pipe and the feeding pipe 7 are in a communication state; otherwise, the discharging pipe and the feeding pipe 7 are in an isolation state. Thus, the speed of the solid precursor into the feeding pipe 7 can be adjusted by controlling the rotating speed of the distribution disc 9 and the size and distribution of the through holes.

[0049] It is worth mentioning that the upper surface of the distribution disc 9 directly contacts the discharging pipe, and the lower surface of the distribution disc 9 directly contacts the feeding pipe 7, thereby realizing the on-off of the two.

[0050] Referring to Figure 2 , Figure 2 is a top view of the distribution disc according to an embodiment of the present application. The distribution disc 9 is disc-shaped, and the through holes comprise six radially distributed circular holes.

[0051] Further, Figure 3 is a top view of the distribution disc according to another embodiment of the present application. The distribution disc 9 is disc-shaped, and the through holes comprise three radially distributed strip-shaped holes.

[0052] The second aspect of the embodiments of the present application provides a chemical vapor deposition system comprising a deposition furnace body 16 and the solid precursor feeding device of the first aspect; the solid precursor feeding device is used for feeding the solid precursor into the deposition furnace body 16. Thus, the interference of water vapor on the chemical vapor deposition can be greatly reduced.

[0053] Embodiments

[0054] The solid precursor feeding device according to the embodiments of the present application is used for feeding TaCl5, wherein the atmosphere in which the TaCl5 powder in the replacement cabin 1 is replaced by nitrogen, while the oxygen in the sealed cabin 10 is kept at less than 0.1 ppm, the water content is kept at less than 0.1 ppm, and the sealed cabin 10 is always filled with more than one atmosphere of argon, the relevant valves are controlled, the TaCl5 powder is fed into the deposition furnace body 16, and the tantalum carbide ceramic coating is deposited on the graphite piece substrate.

[0055] Comparative Example

[0056] The TaCl5 powder is directly fed into the deposition furnace body 16 through the feeding part, and the tantalum carbide ceramic coating is obtained by using the same process as in Embodiment 1.

[0057] Test Example

[0058] The morphology of the obtained tantalum carbide ceramic coating of the examples and the comparative examples was characterized, and the results are shown in Figure 4 and Figure 5 The tantalum carbide coating obtained by feeding the powder of the solid precursor of the examples and then depositing is dense and bright, and the color is uniform; while the color of the tantalum carbide coating of the comparative examples is not uniform, because part of the tantalum carbide coating is oxidized, and part of the tantalum carbide coating has fallen off. As can be seen from Figure 4 and Figure 5 , the tantalum carbide coating of the examples is dense, while the tantalum carbide coating of the comparative examples has cracks. This is because the feeding device of the solid precursor of the examples of the present application can significantly reduce the air content (water and oxygen content) of the precursor powder entering the deposition furnace 16, thereby improving the quality of the tantalum carbide ceramic coating.

[0059] It should be noted that the terms used herein are only intended to describe specific embodiments and are not intended to limit the exemplary embodiments according to the present application. As used herein, the singular form is intended to include the plural form, unless the context clearly indicates otherwise, and it should also be understood that the terms "comprise" and / or "include" as used in the specification indicate the presence of the features, steps, operations, devices, components and / or combinations thereof.

[0060] For ease of description, the orientation words such as "front, back, up, down, left, right", "transverse, vertical, perpendicular, horizontal" and "top, bottom" and the like indicate the orientation or positional relationship shown in the drawings, which are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation or be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the scope of protection of the present application; the orientation words "inner, outer" refer to the inner and outer relative to the contour of each component itself. For example, if the devices in the drawings are inverted, the devices described as "above" or "on" other devices or structures will be positioned "below" or "under" the other devices or structures. Thus, the exemplary term "above" can include both "above" and "below" orientations. The devices can also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatial relative descriptions used herein are interpreted accordingly.

[0061] Unless otherwise clearly indicated, the term "mounting", "connected", "connecting", "fixed", "fixedly connected" and like terms are to be construed broadly, for example, they can be fixed connections, or detachable connections, or integral; they can be mechanical connections, or electrical connections, or communication connections; they can be direct connections, or indirect connections through intermediaries; they can be two elements inside each other, or the interaction between two elements. The specific meaning of the above terms in the present application can be understood according to the specific circumstances by those skilled in the art.

[0062] Unless otherwise clearly indicated, "on" or "under" of a first feature to a second feature can include that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, "on", "above" and "over" of a first feature to a second feature includes that the first feature is directly above and obliquely above the second feature, or only means that the first feature is higher than the second feature in horizontal height. "Under", "below" and "underneath" of a first feature to a second feature includes that the first feature is directly above and obliquely above the second feature, or only means that the first feature is lower than the second feature in horizontal height.

[0063] Unless otherwise specifically stated, the relative arrangement of components and steps, numerical expressions, and numerical values set forth in these embodiments do not limit the scope of the application. At the same time, it should be understood that the size of each part shown in the drawings is not drawn in accordance with the actual proportion relationship for the convenience of description. The technology, methods and devices known to those skilled in the relevant art can not be discussed in detail, but should be considered as part of the authorized description under appropriate circumstances. In all examples shown and discussed here, any specific value should be interpreted as merely exemplary, and not as a limitation. Therefore, other examples of exemplary embodiments can have different values. It should be noted that similar reference numerals and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further discussed in subsequent drawings.

[0064] It should also be noted that "one embodiment", "another embodiment", "embodiment" and the like in the present specification refer to specific features, structures or characteristics described in connection with the embodiment, which are included in at least one embodiment generally described in the present application. The same expression appears in several places in the specification does not necessarily refer to the same embodiment. Further, when a specific feature, structure or characteristic is described in connection with any embodiment, it is claimed that the implementation of such feature, structure or characteristic in connection with other embodiments also falls within the scope of the present application.

[0065] In the above embodiments, the description of each embodiment has its own focus, and the parts not described in detail in a certain embodiment can be referred to the relevant description of other embodiments.

Claims

1. A feed device for solid precursors, characterized in that The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device.

2. The solid-state precursor feed apparatus of claim 1, wherein, The application relates to a solid-state precursor feeding device.

3. The solid-state precursor feed apparatus of claim 2, wherein, The application relates to a solid-state precursor feeding device.

4. The solid-state precursor feed apparatus of claim 3, wherein, The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device.

5. The solid-state precursor feed apparatus of claim 4, wherein, The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device.

6. The solid-state precursor feed apparatus of claim 5, wherein, The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device.

7. The solid-state precursor feed apparatus of claim 6, wherein, The application relates to a solid-state precursor feeding device.

8. The solid-state precursor feed apparatus of claim 5, wherein, The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device.

9. The solid-state precursor feed apparatus of claim 8, wherein, The application relates to a solid-state precursor feeding device. The application relates to a solid-state precursor feeding device.

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