Precursor premixing and packaging device and vapor deposition system
By designing a precursor premix packaging device, the problem of changes in precursor performance under traditional packaging methods is solved, stable mixing and continuous supply of precursors are achieved, and the stability of the vapor deposition process and product quality are improved.
Patent Information
- Application Number
- CN202421465601.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-25
- Publication Date
- 2025-06-17
- Estimated Expiration
- 2034-06-25
AI Technical Summary
The traditional precursor packaging method cannot effectively control the mixing and environmental conditions of the precursor, resulting in changes in the performance of the precursor and affecting the stability of the vapor deposition process and product quality.
A precursor premix packaging device is designed, including a plurality of communicating containers and flow guide structures for mixing solid and liquid precursors before the reaction begins, forming liquid self-assembled compounds, and achieving a stable supply of precursors through a buffer chamber and a control valve.
By premixing the precursor, the performance changes of the liquid precursor before being installed on the vapor deposition equipment are avoided, the stability and repeatability of the reaction are ensured, and the efficiency of preparing high-quality compounds is improved.
Smart Images

Figure CN222990204U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of semiconductor preparation, in particular to a precursor pre-mixing and encapsulation device and a chemical vapor deposition system. Background Art
[0002] With the development of technologies in the field of semiconductor preparation, chemical vapor deposition technologies (CVD and ALD) have emerged. These technologies are well-known for their highly precise thin-film deposition, good controllability, and wide application fields. However, these technologies have high requirements for the quality and stability of precursors.
[0003] In traditional technologies, precursors are usually provided by suppliers and encapsulated in simple sealed containers. However, since this encapsulation method cannot effectively control the mixing of precursors and environmental conditions, the precursors in the precursor encapsulation container may experience performance changes before being installed in the chemical vapor deposition equipment, which in turn affects the stability of the chemical vapor deposition process and the product quality, restricting the further application and development of chemical vapor deposition technologies. Summary of the Utility Model
[0004] Based on this, it is necessary to provide a precursor pre-mixing and encapsulation device and a chemical vapor deposition system for the problem that the performance of precursors in the encapsulation container may change before being installed in the chemical vapor deposition equipment.
[0005] The present application provides a precursor pre-mixing and encapsulation device, comprising:
[0006] A first container having a first accommodating cavity for accommodating a liquid precursor;
[0007] A second container disposed on the first container and communicating with the first container, the second container being used for accommodating a precursor solution and providing a buffer space;
[0008] A third container disposed on the second container and communicating with the second container, for accommodating a solid precursor and / or a liquid precursor;
[0009] An intake pipe and an exhaust pipe, the intake pipe communicating with the first accommodating cavity, and the exhaust pipe communicating with the first accommodating cavity.
[0010] In one embodiment, the third container has a second accommodating cavity and a third accommodating cavity that communicate with each other, the second accommodating cavity is used for accommodating a solid precursor, the third accommodating cavity is used for accommodating a liquid precursor, the vertical projections of the second accommodating cavity and the third accommodating cavity on a horizontal plane coincide, and the third accommodating cavity is disposed on a side of the second accommodating cavity away from the first accommodating cavity;
[0011] A flow guiding structure is provided in the second accommodating cavity. The flow guiding structure is used to change the flow direction of the liquid precursor flowing into the second accommodating cavity, so as to guide the liquid precursor to mix with the solid precursor.
[0012] In one embodiment, the third container has at least two bottle bodies. Any one of the bottle bodies has a second accommodating cavity and a third accommodating cavity that communicate with each other. A plurality of the bottle bodies are all arranged at one end of the second container away from the first accommodating cavity.
[0013] In one embodiment, the second container at least includes a first buffer cavity and a second buffer cavity. The vertical projections of the first buffer cavity and the second buffer cavity on the horizontal plane coincide, and the first buffer cavity communicates with the second buffer cavity.
[0014] In one embodiment, the third container and the second container are detachably connected;
[0015] The second buffer cavity has a plurality of independent chambers, and a plurality of the chambers are respectively connected to a plurality of the bottle bodies correspondingly.
[0016] In one embodiment, it further includes a valve body. The valve body includes a first control valve arranged at the connection between the first container and the second container, a second control valve, a third control valve arranged at the connection between the second container and the third container, a fourth control valve arranged at the connection between the first buffer cavity and the second buffer cavity, and a fifth control valve arranged at the connection between the second accommodating cavity and the third accommodating cavity;
[0017] The first control valve, the second control valve, the third control valve, the fourth control valve, and the fifth control valve are independently controlled from each other.
[0018] In one embodiment, the third container, the second container, and the first container are arranged in sequence along the direction of gravity.
[0019] In one embodiment, the intake pipe and the exhaust pipe are arranged at one end of the first container close to the second container.
[0020] In one embodiment, one end of the intake pipe is used to connect to a gas supply device, and the other end extends to the side of the first accommodating cavity far from the second container to be immersed in the precursor solution;
[0021] One end of the exhaust pipe is arranged in the first accommodating cavity, and the other end is used to communicate with a chemical vapor deposition device.
[0022] A vapor deposition system includes a gas supply device, a precursor premixing and encapsulation device, and a vapor deposition device. The precursor premixing and encapsulation device is connected to the gas supply device and the vapor deposition device, and the precursor premixing and encapsulation device is the above-mentioned precursor premixing and encapsulation device;
[0023] The vapor deposition system further includes:
[0024] A pressure control device, which is respectively connected to the second accommodation chamber, the third accommodation chamber, the first buffer chamber and the second buffer chamber. Under the adjustment of the pressure control device, the pressure in the third accommodation chamber, the second accommodation chamber, the second buffer chamber and the first buffer chamber decreases in the direction of gravity;
[0025] A temperature control device, which is respectively connected to the first container, the second container and the third container, and is used to adjust the temperatures in the first container, the second container and the third container.
[0026] The above-mentioned precursor premixing and encapsulation device. Specifically, in this embodiment, the third container independently accommodates a solid precursor and a liquid precursor. The solid precursor and the liquid precursor are respectively placed in the third container, and the third container is operated to mix the solid precursor and the liquid precursor to form a liquid self-assembled compound, which is then transported to the second container for buffering, and then transported to the first accommodation chamber of the first container to supplement the precursor solution consumed in the reaction in the first accommodation chamber. The precursor premixing and encapsulation device provided in this embodiment mixes the solid precursor and the liquid precursor before the reaction starts, avoiding possible performance changes of the liquid precursor before being installed in the vapor deposition device, which helps to ensure the stability and repeatability of the reaction, thereby improving the efficiency of preparing high-quality compounds.
[0027] In the above-mentioned vapor deposition system, the gas supply device is used to connect to the inlet pipe of the encapsulation container, so that the gas flows into the encapsulation container, and then carries the precursor vapor and flows out from the outlet pipe, and enters the reaction chamber of the vapor deposition device through the process pipeline of the vapor deposition device to participate in the vapor deposition process; the precursor premixing and encapsulation device is used to mix and proportion the solid precursor and the liquid precursor before the meteorological process deposition, ensuring the continuous supply and stable transportation of the precursor. The vapor deposition device is used to deposit the precursor into a thin film or a coating in a gas phase environment. This structure of the vapor deposition system fully considers the stability and continuous supply of the precursor, while ensuring the stability and controllability in the vapor deposition process, it also simplifies the operation process, improves the efficiency of the process and the performance of the product. Description of the Drawings
[0028] Figure 1 It is a schematic diagram of the overall structure of the precursor premixing and encapsulation device provided by an embodiment of the present application;
[0029] Figure 2 Schematic diagram of the internal structure of a precursor premixing and encapsulation device provided by an embodiment of the present application;
[0030] Figure 3 Schematic diagram of a diversion structure in the second accommodating cavity of a precursor premixing and encapsulation device provided by an embodiment of the present application;
[0031] Figure 4 Another schematic diagram of the diversion structure in the second accommodating cavity of a precursor premixing and encapsulation device provided by an embodiment of the present application;
[0032] Figure 5 Another schematic diagram of the diversion structure in the second accommodating cavity of a precursor premixing and encapsulation device provided by an embodiment of the present application;
[0033] Figure 6 Schematic diagram of the structure of the second buffer cavity with a partition of a precursor premixing and encapsulation device provided by an embodiment of the present application.
[0034] Explanation of reference numerals:
[0035] 100 - First container; 110 - First accommodating cavity;
[0036] 200 - Second container; 210 - First buffer cavity; 220 - Second buffer cavity;
[0037] 300 - Third container; 310 - Second accommodating cavity; 320 - Third accommodating cavity;
[0038] 400 - Inlet pipe;
[0039] 500 - Exhaust pipe;
[0040] 600 - Valve body; 610 - First control valve; 620 - Second control valve; 630 - Third control valve; 640 - Fourth control valve; 650 - Fifth control valve. Detailed implementation manners
[0041] In order to make the above - mentioned objects, features and advantages of the present utility model more obvious and understandable, the following detailed description of the specific implementation manners of the present utility model will be given with reference to the accompanying drawings. Many specific details are set forth in the following description in order to fully understand the present utility model. However, the present utility model can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the connotation of the present utility model. Therefore, the present utility model is not limited by the specific embodiments disclosed below.
[0042] In the description of the present utility model, it should be understood that the orientation or positional relationship indicated by the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. is based on the orientation or positional relationship shown in the drawings. It is only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on the present utility model.
[0043] In addition, the terms "first" and "second" are only used for descriptive purposes and should not be construed as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one such feature. In the description of the present utility model, the meaning of "a plurality" is at least two, such as two, three, etc., unless otherwise specifically and clearly defined.
[0044] In the present utility model, unless otherwise clearly specified and defined, the terms "mounted", "connected", "coupled", "fixed", etc. should be understood in a broad sense. For example, it may be a fixed connection, a detachable connection, or integrated; it may be a mechanical connection or an electrical connection; it may be directly connected or indirectly connected through an intermediate medium, and it may be the communication inside two elements or the interaction relationship between two elements, unless otherwise clearly defined. For those of ordinary skill in the art, the specific meanings of the above terms in the present utility model can be understood according to specific circumstances.
[0045] In the present utility model, unless otherwise clearly specified and defined, the first feature being "on" or "under" the second feature may be that the first and second features are in direct contact, or the first and second features are indirectly in contact through an intermediate medium. Moreover, the first feature being "above", "over" and "on top of" the second feature may be that the first feature is directly above or obliquely above the second feature, or merely indicates that the first feature has a higher horizontal height than the second feature. The first feature being "under", "beneath" and "underneath" the second feature may be that the first feature is directly below or obliquely below the second feature, or merely indicates that the first feature has a lower horizontal height than the second feature.
[0046] It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it can be directly on the other element or there may also be an intermediate element. When an element is considered to be "connected to" another element, it can be directly connected to the other element or there may be an intermediate element at the same time. The terms "vertical", "horizontal", "upper", "lower", "left", "right" and similar expressions used herein are for illustrative purposes only and do not represent the only implementation.
[0047] Referring to Figure 1 and Figure 2 , an embodiment of the present utility model provides a precursor premixing and encapsulating device, which includes a first container 100, a second container 200, a third container 300, an intake pipe 400 and an exhaust pipe 500. The first container 100 has a first accommodating cavity 110 for accommodating a liquid precursor. The second container 200 is disposed on the first container 100 and communicates with the first container 100, and is used for accommodating a precursor solution and providing a buffer space. The third container 300 is disposed on the second container 200 and communicates with the second container 200, and is used for accommodating a solid precursor and / or a liquid precursor. The intake pipe 400 communicates with the first accommodating cavity 110, and the exhaust pipe 500 also communicates with the first accommodating cavity 110.
[0048] Specifically, in this embodiment, the third container 300 independently accommodates the solid precursor and the liquid precursor. The solid precursor and the liquid precursor are respectively placed into the third container 300, and the third container 300 is operated to mix the solid precursor and the liquid precursor to form a liquid self-assembled compound, which is then transported to the second container 200 for buffering, and then transported into the first accommodating cavity 110 of the first container 100 to supplement the precursor solution consumed in the reaction in the first accommodating cavity 110. The precursor premixing and encapsulating device provided in this embodiment mixes the solid precursor and the liquid precursor before the reaction starts, avoiding possible performance changes of the liquid precursor before being installed in the chemical vapor deposition equipment, which helps to ensure the stability and repeatability of the reaction, thereby improving the efficiency of preparing high-quality compounds. It should be noted that the volume ratio of the third container 300 to the second container 200 in this embodiment can be set according to the characteristics of the solid precursor in 310 and the liquid precursor in 320 in practice.
[0049] The temperature environment for storing the precursor after encapsulation is different from that required for the chemical vapor deposition process. During the handling and transportation of the precursor encapsulation container, factors such as impacts, vibrations, and long-term non-use due to changes in the temperature environment may cause changes in the structure, composition, and morphology of the precursor material. The change in the precursor performance will affect the stability of the chemical vapor deposition process and the performance of the product. Therefore, it is necessary to reach and continuously maintain the temperature requirements for the chemical vapor deposition process in a timely manner after filling the precursor into the precursor encapsulation container, which is of great significance for the preparation of semiconductor materials by the chemical vapor deposition process.
[0050] Refer to Figure 2 , in one embodiment, the third container 300 has a second accommodation cavity 310 and a third accommodation cavity 320 that communicate with each other. The second accommodation cavity 310 is used to accommodate the solid precursor, and the third accommodation cavity 320 is used to accommodate the liquid precursor. The vertical projections of the second accommodation cavity 310 and the third accommodation cavity 320 on the horizontal plane coincide, and the third accommodation cavity 320 is disposed on a side of the second accommodation cavity 310 away from the first accommodation cavity 110; a diversion structure is provided in the second accommodation cavity 310, and the diversion structure is used to change the flow direction of the liquid precursor flowing into the second accommodation cavity 310 to guide the liquid precursor to mix with the solid precursor.
[0051] Specifically, in this embodiment, the mutually communicating second accommodation cavity 310 and third accommodation cavity 320 are arranged vertically, the third accommodation cavity 320 is disposed above the second accommodation cavity 310, the third accommodation cavity 320 is used to accommodate the liquid precursor, and the second accommodation cavity 310 is used to accommodate the solid precursor. The liquid precursor in the third accommodation cavity 320 flows into the second accommodation cavity under the action of gravity and mixes with the solid precursor to form a liquid self-assembled compound.
[0052] Refer to Figures 3 to 5 , in this embodiment, a diversion structure is provided on a side of the second accommodation cavity 310 close to the third accommodation cavity 320, specifically at the interface between the second accommodation cavity 310 and the third accommodation cavity 320. The diversion structure is used to change the flow direction of the liquid precursor flowing into the second accommodation cavity 310 from the third accommodation cavity 320, so that the liquid precursor diffuses in the solid precursor during the flow process, accelerating the solid-liquid mixing and achieving uniform diffusion.
[0053] Refer to Figure 3 and Figure 4 , specifically, in this embodiment, the diversion structure may be a perforated plate, and the aperture of the perforated plate is less than 1.5 mm, and the aperture increases sequentially in the direction away from the center, so that the liquid precursor can be uniformly diffused in the direction away from the center in the transverse direction.
[0054] Refer to Figure 5, in another embodiment, the diversion structure may also be a deflector plate. A plurality of deflector plates are symmetrically arranged, with a 1.5-mm gap in the middle. The gaps increase successively in the direction away from the center, enabling the uniform diffusion of the liquid precursor in the lateral direction in the direction away from the center.
[0055] Refer to Figure 2 , in one embodiment, the third container 300 has at least two bottle bodies. Any one of the bottle bodies has a second accommodation cavity 310 and a third accommodation cavity 320 that communicate with each other. A plurality of bottle bodies are all arranged at one end of the second container 200 away from the first accommodation cavity 110.
[0056] Specifically in this embodiment, the third container 300 has two bottle bodies, namely a first bottle body and a second bottle body, both of which are connected to the second container 200. Vertically arranged second accommodation cavities 310 and third accommodation cavities 320 are provided in both bottle bodies. The setting and mixing method of the precursor in each bottle body are the same as those described above. By providing a plurality of bottle bodies, mutual supplementation between the precursor accommodation containers is achieved. During the operation, the precursor in the first bottle body is first mixed and then transported to the second container 200 and the first container 100. When the precursor in the first bottle body is consumed or nearly consumed, the second bottle body is opened to continue transporting to the second container 200 and the first container 100. At this time, the first bottle body can be removed for replenishment, realizing the uninterrupted supply of the precursor.
[0057] During the use of a conventional encapsulation container, when the precursor has been used for a certain period of time, the precursor encapsulation container needs to be replaced regularly. Especially as the size of the reaction chamber of the chemical vapor deposition equipment continues to increase, the amount of consumed precursor also continues to increase, which shortens the replacement cycle and increases the replacement frequency of the precursor encapsulation container. This embodiment improves the effective use of the chemical vapor deposition equipment and improves the production efficiency.
[0058] Refer to Figure 2 , in one embodiment, the second container 200 at least includes a first buffer cavity 210 and a second buffer cavity 220. The vertical projections of the first buffer cavity 210 and the second buffer cavity 220 on the horizontal plane coincide, and the first buffer cavity 210 communicates with the second buffer cavity 220.
[0059] Specifically, in this embodiment, the second container 200 includes two buffer chambers, a first buffer chamber 210 and a second buffer chamber 220. The two buffer chambers are arranged vertically. The vertically arranged two buffer chambers ensure that after the precursor solution in the third container 300 is delivered to the second buffer chamber 220, it can enter the first buffer chamber 210 under the action of gravity and then enter the first accommodation chamber 110. In addition, setting the first buffer chamber 210 and the second buffer chamber 220 can also increase the accommodation space for the precursor solution. The precursor solution mixed in the third container 300 can be stored in the first buffer chamber 210 and the second buffer chamber 220 first. When the remaining amount of the precursor solution in the first accommodation chamber 110 is not enough to support the production of the chemical vapor deposition process, the first buffer chamber 210 and the second buffer chamber 220 are controlled to supplement the precursor solution into the first accommodation chamber 110.
[0060] In this embodiment, a U-shaped curved surface structure is provided at the bottom of the inner cavities of the second buffer chamber 220 and the first buffer chamber 210, and this structure can accelerate the flow of the self-assembled liquid precursor in the second buffer chamber 220 and the first buffer chamber 210.
[0061] In one of the embodiments, the third container 300 and the second container 200 are detachably connected. The second buffer chamber 220 has a number of independent chambers, and the several chambers are respectively connected to several bottles.
[0062] Specifically, in this embodiment, the top of the cavity of the second buffer chamber 220 is provided with two through holes and the connecting parts outside the through holes, so that the bottle of the third container 300 and the outside of the through holes of the second container 200 can be connected and fixed by bolts and nuts; in addition, according to the actual situation, the connection between the third container 300 and the second container 200 can also be fixed and sealed by setting a clamp. During the sealing process, a sealing ring can also be additionally added at the connection to increase the airtightness.
[0063] In this embodiment, by adopting the above connection method, each control valve can adopt the same specification to control the flow or closing of the precursor.
[0064] In the above connection method of this embodiment, before the third container 300 and the second buffer chamber 220 are disassembled, all the self-assembled liquid in another third container 300 that has not been removed needs to be transferred to the first container 100, and the second buffer chamber 220 needs to be inflated and evacuated for multiple cycles to exhaust the precursor vapor inside the second buffer chamber 220, so as to prevent the second container 200 from being exposed to air when the third container 300 is disassembled, and the remaining precursor reacts violently with the air, causing dangers such as combustion or even explosion; in addition, after the installation and connection are completed, the second buffer chamber 220 needs to be inflated and evacuated for multiple cycles to exhaust the air inside the second container 200, and prevent the self-assembled liquid precursor formed in the newly installed third container 300 from flowing into the second buffer chamber 220 and being contaminated;
[0065] Refer to Figure 6 , as an optimized embodiment, the second buffer chamber 220 is divided into two independent chambers and connected to two independent bottles of the third container 300, so that the two independent chambers of the second buffer chamber 220 can complete independent self-assembly liquid precursor transfer, gas charging and gas pumping operations.
[0066] Refer to Figure 2 , in one of the embodiments, it further includes a valve body 600. The valve body 600 includes a first control valve 610 disposed at the connection between the first container 100 and the second container 200, a second control valve 620 and a third control valve 630 disposed at the connection between the second container 200 and the third container 300, a fourth control valve 640 disposed at the connection between the first buffer chamber 210 and the second buffer chamber 220, and a fifth control valve 650 disposed at the connection between the second accommodating chamber 310 and the third accommodating chamber 320; the first control valve 610, the second control valve 620, the third control valve 630, the fourth control valve 640 and the fifth control valve 650 are independently controlled from each other.
[0067] By providing the first control valve 610, the second control valve 620, the third control valve 630, the fourth control valve 640 and the fifth control valve 650, each control valve independently controls the on-off state of the corresponding connection, so that each accommodating chamber or buffer chamber in the precursor premixing and encapsulating device can be independently controlled, thereby making the regulation of the reaction process provided by this embodiment more flexible, contributing to optimizing the reaction conditions and improving the product quality. In addition, by controlling the on-off state of each accommodating chamber or buffer chamber, the delivery rate and delivery amount of the precursor can be adjusted to achieve optimized regulation of the reaction parameters to meet the requirements under different reaction conditions. Independently controlling the on-off state of each accommodating chamber or buffer chamber can also effectively prevent cross-contamination between different precursors, maintain the purity of the reaction system, and improve the purity of the product.
[0068] Refer to Figure 1 , in one of the embodiments, the third container 300, the second container 200 and the first container 100 are sequentially arranged along the direction of the gravity action. Specifically, in this embodiment, the third container 300, the second container 200 and the first container 100 are sequentially arranged along the direction of the gravity action, that is, the first container 100 is arranged at the bottommost, the second container 200 is arranged above it, and the third container 300 is arranged above the second container 200. Such an arrangement enables the liquid precursor and the mixed precursor solution to automatically migrate to the container corresponding to the next process under the action of gravity without external intervention, realizing automatic delivery of the precursor and simplifying the operation process. In addition, using the gravity action to achieve the delivery of the precursor does not require additional energy consumption, saving energy costs and reducing operation costs.
[0069] Refer to Figure 1 , in one embodiment, the intake pipe 400 and the exhaust pipe 500 are disposed at one end of the first container 100 close to the second container 200.
[0070] Refer to Figure 1 , in one embodiment, one end of the intake pipe 400 is used to connect to a gas supply device, and the other end extends to a side of the first accommodation cavity 110 far from the second container 200 to be immersed in the precursor solution; one end of the exhaust pipe 500 is disposed in the first accommodation cavity 110, and the other end is used to communicate with a chemical vapor deposition device. The intake pipe 400 is connected to the gas supply device to introduce gas into the first accommodation cavity 110. The other end of the intake pipe 400 extends into the precursor solution in the first accommodation cavity 110, so that the gas can be fully immersed in the precursor solution, realizing the mixing and dissolution of the gas and the precursor, and providing sufficient conditions for the reaction. The exhaust pipe 500 is connected to the chemical vapor deposition device to discharge the used gas, ensuring that the waste gas generated during the reaction process can be effectively discharged, and avoiding the accumulation of gas in the reaction container resulting in uncontrolled reaction.
[0071] Specifically in this embodiment, the precursor premixing and encapsulation device provided in this embodiment is applicable to encapsulation of precursor materials such as two independent precursors like solid trimethylindium TMIn and liquid triethylindium TEIIn, which can form a liquid precursor after mixing.
[0072] The operation method of the precursor premixing and encapsulation device provided in this embodiment is as follows:
[0073] At the beginning of the process, the encapsulation container filled with the precursor material is connected to the chemical vapor deposition device. The intake pipe 400 is connected to the carrier gas end of the chemical vapor deposition device, which is the gas supply device, and the exhaust pipe 500 is connected to the process pipeline of the chemical vapor deposition device. The first accommodation cavity 110 is filled with the mixed liquid In precursor, the second accommodation cavity 310 is filled with the solid TMIn precursor material, the third accommodation cavity 320 is filled with the liquid TEIn precursor material, and the mass ratio of TMIn to TEIn is 2:1;
[0074] As the process progresses, the precursor in the first accommodation cavity 110 is continuously consumed. According to the consumption progress of the precursor in the first accommodation cavity 110, the fifth control valve 650 of the first bottle body is opened 24 to 72 hours in advance. The liquid precursor inside the third accommodation cavity 320 of the first bottle body flows into the second accommodation cavity 310 through the fifth control valve 650 and mixes with the solid precursor filled inside to form a self-assembled liquid precursor. When the remaining amount of the precursor in the first accommodation cavity 110 is insufficient to support the chemical vapor deposition process production, the second control valve 620, the fourth control valve 640 and the first control valve 610 are opened, and the liquid precursor realizes the transfer from the second container 200 to the first accommodation cavity 110;
[0075] As the process further progresses, the precursor in the first accommodation cavity 110 is continuously consumed. According to the consumption progress of the precursor in the first accommodation cavity 110, the fifth control valve 650 of the second bottle body is opened 24 to 72 hours in advance to form a self-assembled liquid precursor in the second accommodation cavity 310 of the second bottle body. According to actual requirements, before the liquid precursor in the second accommodation cavity 310 of the second bottle body is transferred into the first accommodation cavity 110, the second accommodation cavity 310 of the first bottle body can be filled with a solid precursor, and the third accommodation cavity 320 of the first bottle body can be filled with a liquid precursor;
[0076] As the process progresses, the precursor in the first accommodation cavity 110 is continuously consumed. By repeating the above steps, the transfer of the precursor is achieved.
[0077] The encapsulation container of the present application can, under the environmental conditions required for the chemical vapor deposition process, form a liquid self-assembled compound by connecting solid precursor molecules and second liquid precursor molecules through coordination bonds and secondary bonds before the chemical vapor deposition process for the solid precursor and the liquid precursor, avoiding the change in the performance of the precursor caused by placing the precursor encapsulation device in different environments after the precursor supplier manufactures the precursor into a liquid precursor, thereby affecting the stability of the chemical vapor deposition process and the performance of the product.
[0078] In this embodiment, a solid precursor identical to that in the third accommodation cavity 320 can be filled in the buffer cavity 210 according to process requirements. The presence of the solid precursor vapor can cause the self-assembled liquid precursor in the pipeline to be supersaturated as a whole, so that decomposition does not occur, further ensuring the stability of the liquid precursor.
[0079] An embodiment of the present invention further provides a chemical vapor deposition system, including a gas supply device, a precursor premixing and encapsulation device, and a chemical vapor deposition device. The precursor premixing and encapsulation device is connected to the gas supply device and the chemical vapor deposition device, and the precursor premixing and encapsulation device is the precursor premixing and encapsulation device provided in the above embodiment.
[0080] The above chemical vapor deposition system further includes a pressure control device and a temperature control device. The pressure control device is respectively connected to the second accommodation cavity 310, the third accommodation cavity 320, the first buffer cavity 210, and the second buffer cavity 220. Under the adjustment of the pressure control device, the pressures of the third accommodation cavity 320, the second accommodation cavity 310, the second buffer cavity 220, and the first buffer cavity 210 decrease in the direction of gravity.
[0081] The temperature control device is respectively connected to the first container 100, the second container 200, and the third container 300 for adjusting the temperatures in the first container 100, the second container 200, and the third container 300.
[0082] The gas supply device in this embodiment is used to transport the gases required for various processes to the chemical vapor deposition equipment. Here, the gas mainly refers to the carrier gas of the precursor. The carrier gas flows into the precursor encapsulation container through the inlet pipe of the precursor encapsulation container, and then the carrier gas carries the precursor vapor and flows out through the outlet pipe, and enters the chemical vapor deposition equipment through the process pipeline of the chemical vapor deposition equipment. The precursor premixing and encapsulation device in this embodiment is the precursor premixing and encapsulation device in the foregoing embodiment, which is used to mix and proportion the solid precursor and the liquid precursor before the meteorological process deposition, ensuring the continuous supply and stable transportation of the precursor. The chemical vapor deposition equipment generally includes equipment such as a reaction chamber, a heating device, and a substrate support, which are used to deposit the precursor into a thin film or a coating in a gas phase environment.
[0083] The design of the chemical vapor deposition system provided in this embodiment fully considers the stability and continuous supply of the precursor. While ensuring the stability and controllability during the chemical vapor deposition process, it also simplifies the operation process, improves the efficiency of the process and the performance of the product.
[0084] The synthesis temperature of the self-assembled liquid precursor generally needs to be greater than 40 °C. However, due to safety, cost, and vapor pressure stability requirements, the storage temperature requirement of the precursor in the chemical vapor deposition process is generally lower than 30 °C. This requires that the temperature needs to be set to meet the process requirements after the self-assembled liquid precursor is formed. In the actual production process, the precursor is stored in the encapsulation container, and the precursor encapsulation container is often made to be in a constant temperature environment through external temperature setting, so as to ensure that the internal precursor reaches the constant temperature required by the process, thereby ensuring the precursor vapor pressure required by the process.
[0085] In this embodiment, the chemical vapor deposition system has a temperature control device. Specifically, heat preservation units are provided on the first container 100, the second container 200, and the third container 300, so that the first container 100, the second container 200, and the third container 300 are at a constant set temperature. The heat preservation unit can be one of a water bath tank, a heating table, a heating box, or a heating belt.
[0086] In one of the embodiments, the first container 100 is placed in a constant temperature water bath tank, and the second container 200 and the third container 300 are covered by an outer heating belt; the temperature of the first buffer chamber 210 is set to be the same as the temperature of the first container 100, and the temperature of the second buffer chamber 220 is set to be between the temperature of the first buffer chamber 210 and the temperature of the third container 300.
[0087] In this embodiment, the second buffer chamber 220 is used to achieve the post-transfer synthesis of the self-assembled liquid precursor, and at the same time, the self-assembled liquid precursor realizes the temperature buffer transition from the temperature in the second buffer chamber 220 to the precursor in the first accommodation chamber 110; the first buffer chamber 210 is used to balance the temperature of the self-assembled liquid precursor and the temperature of the liquid precursor in the first accommodation chamber 110; to avoid large fluctuations in the amount of precursor carried by the carrier gas due to fluctuations in the vapor pressure of the precursor in the first accommodation chamber 110 caused by the temperature difference between the self-assembled liquid precursor and the liquid precursor in the first accommodation chamber 110, which may affect the chemical vapor deposition process.
[0088] In this embodiment, the chemical vapor deposition system further includes a pressure control device for improving the fluidity of the self-assembled liquid precursor. The pressure control device specifically includes an intake pipe and a pressure control unit. By means of the intake pipe and the pressure control unit, the internal pressures of the third accommodation chamber 320, the second accommodation chamber 310, the second buffer chamber 220, and the first buffer chamber 210 decrease in sequence, thereby accelerating the flow of the liquid precursor in the third accommodation chamber 320 and the self-assembled liquid precursor in the second buffer chamber 220 and the first buffer chamber 210.
[0089] In one of the embodiments, the present application further provides a method for preparing a high-quality nitride epitaxial wafer, using a self-assembled liquid indium precursor formed by mixing TMIn and TEIn, including the following steps:
[0090] Before the chemical vapor deposition process starts, connect the encapsulated container filled with the precursor material to the chemical vapor deposition equipment;
[0091] When the chemical vapor deposition process starts, the carrier gas enters the first accommodation chamber through the intake pipe, carries the precursor vapor into the process pipeline of the chemical vapor deposition equipment from the exhaust pipe, and then enters the reaction chamber of the chemical vapor deposition equipment to grow a multi-quantum well light-emitting structure layer with 2-20 cycles of nitride quantum barriers and In-containing nitride quantum well layers.
[0092] Among them, the thickness of the nitride quantum barrier layer is 6-30 nm, the thickness of the In-containing nitride quantum well layer is 1-6 nm, and the emission wavelength of the multi-quantum well light-emitting structure layer is 390-780 nm;
[0093] Compared with the conventional solid-state TMIn packaging container, when growing the same multi-quantum well light-emitting structure layer and under the same wavelength condition, the light-emitting intensity of the present application is increased by more than 20%. The method for preparing the high-quality nitride epitaxial wafer provided in this embodiment, on the one hand, realizes a great improvement in the self-assembled liquid precursor through the improved packaging container, improves the stability of the self-assembled liquid precursor, and improves the uniformity of the components of the multi-quantum well light-emitting structure layer. By using the self-assembled precursor to reduce the methyl group -CH3 in the solid precursor, the C incorporation in the epitaxial layer is reduced, and the defects and non-radiative recombination in the epitaxial layer are reduced, which can improve the optoelectronic properties of the epitaxial wafer.
[0094] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity of description, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, it should be considered as the scope described in this specification.
[0095] The above-described embodiments only represent several implementation manners of the present invention, and the description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the utility model patent. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the utility model patent shall be subject to the appended claims.
Claims
1. A precursor premixing packaging device, characterized in that: include: A first container (100) has a first containing cavity (110) for containing a liquid precursor; a second container (200), the second container (200) being disposed on the first container (100) and being in communication with the first container (100), the second container (200) being used to contain a precursor solution and provide a buffer space; a third container (300), the third container (300) being disposed on the second container (200) and communicating with the second container (200), and being used for containing a solid precursor and / or a liquid precursor; An air intake pipe (400) and an exhaust pipe (500), wherein the air intake pipe (400) is in communication with the first accommodating chamber (110), and the exhaust pipe (500) is in communication with the first accommodating chamber (110); The third container (300) comprises a second accommodating chamber (310) and a third accommodating chamber (320) which are interconnected, the second accommodating chamber (310) is used to accommodate a solid precursor, the third accommodating chamber (320) is used to accommodate a liquid precursor, the vertical projections of the second accommodating chamber (310) and the third accommodating chamber (320) on a horizontal plane overlap, and the third accommodating chamber (320) is arranged on a side of the second accommodating chamber (310) away from the first accommodating chamber (110); A flow guiding structure is provided in the second accommodating chamber (310), and the flow guiding structure is used to change the flow direction of the liquid precursor flowing into the second accommodating chamber (310) so as to guide the liquid precursor to mix with the solid precursor.
2. The precursor premix packaging device according to claim 1, characterized in that: The third container (300) has at least two bottle bodies, any of which has a second accommodating cavity (310) and a third accommodating cavity (320) that are interconnected, and a plurality of the bottle bodies are arranged at one end of the second container (200) away from the first accommodating cavity (110).
3. The precursor premix packaging device according to claim 1, characterized in that: The second container (200) comprises at least a first buffer cavity (210) and a second buffer cavity (220); the vertical projections of the first buffer cavity (210) and the second buffer cavity (220) on a horizontal plane overlap; and the first buffer cavity (210) is connected to the second buffer cavity (220).
4. The precursor premix packaging device according to claim 3, characterized in that: The third container (300) is detachably connected to the second container (200); The second buffer chamber (220) has a plurality of independent chambers, and the plurality of chambers are respectively connected to a plurality of bottle bodies of the third container (300).
5. The precursor premix packaging device according to claim 2, characterized in that: The invention also includes a valve body (600), wherein the valve body (600) includes a first control valve (610) arranged at the connection between the first container (100) and the second container (200), a second control valve (620) and a third control valve (630) arranged at the connection between the second container (200) and the third container (300), a fourth control valve (640) arranged at the connection between the first buffer chamber (210) of the second container (200) and the second buffer chamber (220) of the second container (200), and a fifth control valve (650) arranged at the connection between the second accommodating chamber (310) and the third accommodating chamber (320); The first control valve (610), the second control valve (620), the third control valve (630), the fourth control valve (640) and the fifth control valve (650) are independently controlled from one another.
6. The precursor premix packaging device according to claim 1, characterized in that: The third container (300), the second container (200) and the first container (100) are arranged in sequence along the direction of gravity.
7. The precursor premix packaging device according to claim 1, characterized in that: The air inlet pipe (400) and the air outlet pipe (500) are arranged on one end of the first container (100) close to the second container (200).
8. The precursor premix packaging device according to claim 7, characterized in that: One end of the air inlet pipe (400) is used to connect to a gas supply device, and the other end extends to a side of the first accommodating chamber (110) away from the second container (200) so as to be immersed in the precursor solution; One end of the exhaust pipe (500) is arranged in the first accommodating chamber (110), and the other end is used to connect to the vapor deposition equipment.
9. A vapor deposition system, characterized in that: It comprises a gas supply device, a precursor premix packaging device and a vapor deposition device, wherein the precursor premix packaging device is connected to the gas supply device and the vapor deposition device, and the precursor premix packaging device is the precursor premix packaging device according to any one of claims 1 to 8; The vapor deposition system further comprises: a pressure control device, the pressure control device being connected to the second accommodating chamber (310), the third accommodating chamber (320), the first buffer chamber (210) and the second buffer chamber (220) respectively, and under the adjustment of the pressure control device, the pressure of the third accommodating chamber (320), the second accommodating chamber (310), the second buffer chamber (220) and the first buffer chamber (210) decreases gradually along the gravity direction; A temperature control device is connected to the first container (100), the second container (200) and the third container (300) respectively, and is used to adjust the temperature inside the first container (100), the second container (200) and the third container (300).