MO source system for chemical vapor deposition equipment

By introducing a MO source system with components such as a pressure reducing valve and Sorce-MFC into the chemical vapor deposition equipment, the problem of uneven reaction gas during the MO source growth process was solved, the stable supply and uniform distribution of the MO source were achieved, and the production efficiency and product quality of the CVD equipment were improved.

CN120683476APending Publication Date: 2025-09-23NANJING EXTREMO TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510910763.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-02
Publication Date
2025-09-23

AI Technical Summary

Technical Problem

Existing chemical vapor deposition equipment cannot achieve uniform intake of reaction gases when using metal organic (MO) sources, resulting in uneven material growth, pressure fluctuations, and difficulty in accurately controlling the flow rate with a single mass flow controller. Dead volume during gas line switching destroys flow field stability, and uneven heating of the source bottle leads to differences in evaporation rates.

Method used

The MO source system, consisting of components such as a pressure reducing valve, Sorce-MFC, Push-MFC, pressure controller, Line valve, RUN valve, exhaust valve and manual valve, achieves a stable supply and uniform distribution of MO source by precisely controlling pressure and flow, ensuring the stability and flexible switching of gas parameters.

Benefits of technology

It improves the production efficiency and product quality of CVD equipment, avoids cross contamination between MO sources, enhances the stability and reliability of the system, meets the needs of different process environments, and improves the quality and efficiency of vapor deposition.

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Abstract

The invention discloses an MO source system for chemical vapor deposition equipment, the MO source system comprises a pressure reducing valve, a Sorce-MFC, a Push-MFC, a pressure controller, a Line valve, an RUN valve, an extraction valve and a manual valve, the pressure reducing valve is used for controlling the gas inlet pressure of a single-path MO source system, the Sorce-MFC is used for controlling carrier gas flowing into a source bottle, the Push-MFC is used for further adding the carrier gas to dilute the carrier gas flowing out of the source bottle, and the pressure controller is used for controlling the gas inlet pressure of the single-path MO source system. And the pressure controller is used for controlling the pressure of the flowing-out gas. The MO source in the MOCVD system is independent and connected into the corresponding CVD equipment process environment, the use process of the MO source is greatly simplified, continuous supply, temperature control and precise regulation and control of the MO source are achieved, precise control over the flow and pressure of the MO source and carrier gas is achieved through the pressure reducing valve, the Sorce-MFC and the Push-MFC, and the service life of the MO source is prolonged. Therefore, stable supply and uniform distribution of the MO source in the CVD equipment are ensured, and the production efficiency and the product quality of the CVD equipment are improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of MO source systems for chemical vapor deposition equipment, and in particular to an MO source system for chemical vapor deposition equipment. Background Art

[0002] Chemical vapor deposition (CVD) is an efficient and low-cost method that can control not only the size but also the morphology of materials by adjusting CVD equipment parameters. It is the main method for thin films. However, achieving uniform growth of large-scale wafers of two-dimensional transition metal sulfide compounds mainly requires controlling the delivery of reactive gases. However, existing CVD equipment cannot achieve uniform reactive gas flow, which makes it difficult to grow uniform materials. Although CVD equipment can achieve material growth, it is often difficult to achieve the desired results in growth processes involving metal organic (MO) sources due to the following reasons: First, pressure fluctuations can cause the pressure of the carrier gas supply source to be unstable, causing the flow rate at the source bottle outlet to be sometimes fast and sometimes slow; Secondly, a single mass flow controller (MFC) is difficult to accurately control the flow of the source bottle gas and the dilution gas at the same time, which can easily cause the flow to be out of control; Third, during the source switching operation or gas path switching process, the dead volume formed by the residual gas will destroy the stability of the flow field and cause gas path interference; Finally, uneven heating of the source bottle can lead to local differences in the evaporation rate of the MO material, which can easily form a temperature gradient.

[0003] In summary, the present invention provides an MO source system for chemical vapor deposition equipment to solve the above problems. Summary of the Invention

[0004] The purpose of the present invention is to provide an MO source system for chemical vapor deposition equipment, which has the advantages of controlling the parameters of the MO source during the material growth process by controlling the pressure flow, and realizing the switching and use process of the MO source through the MO source system, thereby solving the problem that the existing CVD equipment cannot achieve uniform intake of reaction gas, which makes it difficult to grow materials uniformly. Although the CVD equipment can grow materials, it cannot achieve the expected effect in the related growth process involving the MO source.

[0005] To achieve the above objectives, the present invention provides the following technical solutions: a MO source system for chemical vapor deposition equipment, comprising a pressure reducing valve, a Sorce-MFC, a Push-MFC, a pressure controller, a Line valve, a RUN valve, an exhaust valve, and a manual valve, wherein the pressure reducing valve is used to control the inlet pressure of the single-channel MO source system; The Sorce-MFC is used to control the carrier gas flowing into the source bottle; The Push-MFC is used to further add carrier gas to dilute the carrier gas flowing out of the source bottle; The pressure controller is used to control the pressure of the outflowing gas; The Line valve is used to control whether the carrier gas flows through the source bottle, open for flow, closed for bypass; The RUN valve is used to control whether the carrier gas is connected to the machine for use. When it is open, it is connected to the machine, and when it is closed, it is connected to the exhaust system. The air extraction valve is used to evacuate the pipeline when changing the source; The manual valve is used to cut the pipeline into the exhaust system when changing the source; The system also includes a water bath, a flow meter and a pressure gauge, and the MO source cylinder is located in the water bath. The flow meter and pressure gauge are respectively used to monitor and control the flow and pressure of the carrier gas in real time.

[0006] Preferably, the Line valve is a two-position four-way solenoid valve, and the RUN valve is a two-position five-way solenoid valve.

[0007] Preferably, the pressure reducing valve is installed at the gas inlet, with its input connected to the carrier gas supply source and its output connected to the subsequent Sorce-MFC.

[0008] Preferably, the input end of the Sorce-MFC is connected to the output end of the pressure reducing valve, and its output end is connected to the source bottle. The input end of the Push-MFC is connected to the carrier gas supply source, which can be shared with the carrier gas supply before the pressure reducing valve, and its output end is connected to the outflow pipeline of the source bottle for diluting the carrier gas flowing out of the source bottle.

[0009] Preferably, the pressure controller is installed on the outflow pipeline of the source bottle and is located at the outlet of the source bottle, and is used to monitor and control the pressure of the outflowing gas in real time.

[0010] Preferably, the Line valve is installed on the connecting pipeline between the carrier gas and the source bottle to control whether the carrier gas flows through the source bottle; the RUN valve is installed at the output end of the system and connected to the exhaust system.

[0011] Preferably, the exhaust valve is connected to the exhaust pipeline to facilitate evacuating the pipeline when changing the source, and a normally closed pneumatic valve is also installed on the exhaust pipeline. The manual valve cuts the pipeline into the exhaust system when changing the source.

[0012] Compared with the prior art, the present invention has the following beneficial effects: 1. The present invention greatly simplifies the use process of the MO source by isolating the MO source in the MOCVD system and connecting it to the corresponding CVD equipment process environment, thereby realizing the continuous supply, temperature control and precise regulation of the MO source. The provided pressure reducing valve, Sorce-MFC and Push-MFC realize precise control of the flow and pressure of the MO source and the carrier gas, thereby ensuring the stable supply and uniform distribution of the MO source in the CVD equipment, improving the production efficiency and product quality of the CVD equipment. The provided Line valve and RUN valve can conveniently control the flow path of the carrier gas, realize flexible switching and precise control of the MO source supply, and meet the requirements of different process environments for MO sources. The provided pressure controller and exhaust valve assembly can monitor and control the pressure of the outflowing gas in real time, and quickly evacuate the pipeline when changing the source, avoiding cross contamination between different MO sources and improving the stability and reliability of the system.

[0013] 2. The present invention can accurately control the inlet pressure, flow rate and pressure of the outflowing gas of the carrier gas through the coordinated work of the pressure reducing valve, Sorce-MFC, Push-MFC, pressure controller, flow meter and pressure gauge in the system, thereby ensuring the stability of gas parameters throughout the entire vapor deposition process, which is beneficial to improving the quality and efficiency of chemical vapor deposition. In addition, the setting of the Line valve and the RUN valve gives the carrier gas flow direction a high degree of flexibility. The Line valve can control whether the carrier gas flows through the source bottle, realizing the switching of flow through or bypass. The RUN valve can control whether the carrier gas is connected to the machine for use or to the exhaust system. Through flexible control methods, the system can quickly adjust the flow direction and usage of the gas according to different process stages and requirements, thereby improving the adaptability of the system and the diversity of the process. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 This is a schematic diagram of a single-channel MO source of the present invention; Figure 2 This is a schematic diagram of the main structure of the present invention; Figure 3 Schematic diagram of the initial state of the system of the present invention; Figure 4 Schematic diagram of the gas entering the exhaust system through the source bottle of the present invention; Figure 5 Schematic diagram of the gas entering the machine through the source bottle of the present invention. DETAILED DESCRIPTION

[0015] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0016] Example 1 like Figure 1-2 FIG. 1 shows a first embodiment of the present invention, which provides a MO source system for a chemical vapor deposition device, including a pressure reducing valve, a Sorce-MFC, a Push-MFC, a pressure controller, a Line valve, a RUN valve, an exhaust valve, and a manual valve. The pressure reducing valve is used to control the inlet pressure of the single-channel MO source system. Sorce-MFC is used to control the carrier gas flowing into the source bottle; Push-MFC is used to further add carrier gas to dilute the carrier gas flowing out of the source bottle; The pressure controller is used to control the pressure of the outflowing gas; The Line valve is used to control whether the carrier gas flows through the source bottle. Open means flow through, and closed means bypass. The RUN valve is used to control whether the carrier gas is connected to the machine. If it is open, it is connected to the machine, and if it is closed, it is connected to the exhaust system. The air extraction valve is used to evacuate the pipeline when changing the source; The manual valve is used to cut the pipeline into the exhaust system when changing the source; The system also includes a water bath, a flow meter and a pressure gauge, and the MO source cylinder is located in the water bath. The flow meter and pressure gauge are used to monitor and control the flow and pressure of the carrier gas in real time, respectively.

[0017] like Figure 1-2 As shown in the figure, the pressure reducing valve is located at the gas inlet and serves as the first-stage pressure regulating device of the system. It is responsible for reducing the high-pressure gas of the carrier gas supply source to the required working pressure. The pressure controller is installed at the outlet of the source bottle. Through closed-loop control technology, the pressure of the output gas is ensured to be stable, avoiding pressure fluctuations that interfere with the uniformity of deposition. The pressure reducing valve performs coarse adjustment of the inlet pressure, while the pressure controller performs closed-loop control at the outlet of the source bottle, jointly constructing a two-stage pressure stabilization system. The response time of the pressure controller is less than 50 milliseconds, and it can control pressure fluctuations within ±0.5%. Sorce-MFC precisely controls the flow of carrier gas into the source bottle to ensure stable evaporation of MO material in the source bottle. Push-MFC is independent of the main gas line and adjusts the concentration of the gas flowing out of the source bottle through the dilution gas, realizing flexible adjustment of process parameters and avoiding the limitation of the single MFC range. Under the coordinated control of dual MFCs, Sorce-MFC focuses on source bottle inlet control, while Push-MFC independently adjusts the dilution gas, forming a master-slave flow control structure. The total flow calculation formula is total flow = Sorce flow / (1 + dilution ratio). By adjusting the dilution ratio, fine control of the concentration from 0.1% to 100% can be achieved; The Line valve controls whether the carrier gas flows through the source bottle, enabling switching between straight-through and bypass modes for quick source switching or maintenance. The RUN valve determines whether the gas flows to the machine or exhaust system, supporting rapid switching between process status and safety exhaust. The exhaust valve, used in conjunction with the normally closed pneumatic valve, evacuates the pipeline during source changes to prevent residual gas from contaminating the new source or causing pressure shock. The manual valve can be manually switched to the exhaust system in an emergency, providing additional safety. When the Sorce-MFC adjusts the carrier gas flow, the Push-MFC will synchronously adjust the dilution gas flow to maintain a stable total flow. An interlocking logic is set between the pressure controller and the MFC to automatically adjust the MFC output when the pressure is abnormal to prevent equipment overload. The Line valve switches faster than the RUN valve to avoid pressure pulses when switching gas lines. Through precise solenoid valve control, pressure-flow coordinated regulation and safety interlock design, the accuracy and reliability of MO source delivery are significantly improved, providing hardware support for high-quality CVD thin film preparation.

[0018] Example 2 Reference Figure 1-5 , which is the second embodiment of the present invention, and this embodiment is based on the previous embodiment.

[0019] In this embodiment, the Line valve is a two-position four-way solenoid valve, and the RUN valve is a two-position five-way solenoid valve.

[0020] The pressure reducing valve is installed at the gas inlet, with its input connected to the carrier gas supply source and its output connected to the subsequent Sorce-MFC.

[0021] The input end of the Sorce-MFC is connected to the output end of the pressure reducing valve, and its output end is connected to the source bottle. The input end of the Push-MFC is connected to the carrier gas supply source, which can be shared with the carrier gas supply before the pressure reducing valve. Its output end is connected to the outflow pipeline of the source bottle to dilute the carrier gas flowing out of the source bottle.

[0022] The pressure controller is installed on the pipeline outflowing from the source bottle and is located at the outlet of the source bottle. It is used to monitor and control the pressure of the outflowing gas in real time.

[0023] The Line valve is installed on the connecting pipeline between the carrier gas and the source bottle to control whether the carrier gas flows through the source bottle; the RUN valve is installed at the output end of the system and connected to the exhaust system.

[0024] The exhaust valve is connected to the exhaust pipeline to facilitate evacuating the pipeline when changing the source. A normally closed pneumatic valve is also installed on the exhaust pipeline, and a manual valve cuts the pipeline into the exhaust system when changing the source.

[0025] like Figure 1-5 As shown in the figure, the pressure reducing valve, Sorce-MFC, Push-MFC, pressure controller, flow meter and pressure gauge work together to precisely control the inlet pressure and flow rate of the carrier gas and the pressure of the outflowing gas. Among them, the pressure reducing valve is used to control the inlet pressure of the single-channel MO source system, the Sorce-MFC is responsible for adjusting the flow rate of the carrier gas flowing into the source bottle, and the pressure controller monitors and controls the pressure of the outflowing gas in real time. The synergistic effect of these components ensures the stability of gas parameters during the vapor deposition process, thereby improving the quality and efficiency of chemical vapor deposition. In addition, the settings of the Line valve and RUN valve give the carrier gas flow a high degree of flexibility. The Line valve can control whether the carrier gas flows through the source bottle, realizing the switching of flow through or bypass. The RUN valve can control whether the carrier gas is connected to the machine for use or to the exhaust system. Through this flexible control method, the flow direction and usage of the gas can be quickly adjusted according to different process stages and needs, thereby improving the adaptability of the system and the diversity of processes. When the carrier gas does not need to pass through the source bottle, the Line valve can be closed to bypass the carrier gas, avoiding unnecessary gas consumption and affecting the substances in the source bottle. The design of the air extraction valve and manual valve further facilitates the source change operation. The air extraction valve is used to evacuate the pipeline when changing the source, while the manual valve can cut the pipeline into the exhaust system when changing the source, effectively preventing mutual contamination between different sources, ensuring the smooth progress of the source change process, reducing the source change time and the impact on production. At the same time, the normally closed pneumatic valve installed on the air extraction pipeline further improves the safety and reliability of the source change operation; The MO source cylinder is located in a water bath, which provides a relatively stable temperature environment for the source bottle. Temperature stability is crucial to the stability of the physical and chemical properties of the MO source, and helps ensure the stability of the MO source carried by the carrier gas, thereby improving the stability and repeatability of the chemical vapor deposition process.

[0026] When in use, the carrier gas enters the system from the supply source and first passes through the pressure reducing valve installed at the air inlet. The main function of the pressure reducing valve is to adjust the air inlet pressure of the single-channel MO source system to ensure that the carrier gas pressure entering the subsequent system remains stable. The carrier gas output by the pressure reducing valve then enters the Sorce-MFC. The Sorce-MFC is used to accurately control the carrier gas flow rate flowing into the source bottle. By accurately adjusting the carrier gas flow rate, an appropriate amount of carrier gas can be allowed to enter the MO source cylinder located in the water bath, thereby carrying the MO source vapor. The water bath can maintain the temperature of the MO source cylinder to ensure the stability and volatility of the MO source. The carrier gas flowing out of the source bottle may have a high concentration. At this time, the Push-MF C begins to work. The air inlet of Push-MFC is connected to the carrier gas supply source and can be shared with the carrier gas supply before the pressure reducing valve. Its output end is connected to the outflow pipeline of the source bottle. The carrier gas flowing out of the source bottle is diluted by further adding carrier gas to achieve a suitable concentration. A pressure controller is installed at the outlet of the source bottle on the outflow pipeline of the source bottle. The controller is used to monitor and control the pressure of the outflowing gas in real time to ensure that the pressure of the outflowing carrier gas is stable and meets the use requirements of the chemical vapor deposition equipment. The Line valve is installed on the connecting pipeline between the carrier gas and the source bottle. A two-position four-way solenoid valve is used. By controlling the on / off state of the Line valve, it can be controlled whether the carrier gas flows through the source bottle. When the Line valve is open, the carrier gas flows through the source bottle. When the Line valve is closed, the carrier gas bypasses the source bottle. The RUN valve is installed at the output end of the system and connected to the exhaust system. It uses a two-position five-way solenoid valve. The RUN valve is used to control whether the carrier gas is connected to the machine for use. When the RUN valve is open, the carrier gas is connected to the machine; when the RUN valve is closed, the carrier gas is connected to the exhaust system. The exhaust valve is connected to the exhaust pipeline to facilitate evacuation of the pipeline when changing the source. A normally closed pneumatic valve is also installed on the exhaust pipeline. The Tongyuan process flow is as follows: 1) The initial state of the system is that the Line valve is closed and the Run valve is closed. At this time, the carrier gas bypasses the Line valve and enters the exhaust system; 2) After opening the Line valve, the gas passes through the source bottle and enters the exhaust system, and the pre-flow source begins; 3) Open the RUN valve. The carrier gas passes through the source bottle and enters the machine through the RUN valve. 4) After use, close the RUN valve and cut into the exhaust system; 5) Close the Line valve and the system returns to its initial state; The source change process is as follows: when changing the source, first open the manual air extraction valve, then open the normally closed pneumatic valve, start to extract air, then open the Line valve, start to replenish air, and after completion, cycle 30 times before changing the source.

[0027] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply the existence of any such actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article, or device comprising a series of elements includes not only those elements, but also other elements not explicitly listed, or elements inherent to such process, method, article, or device. In the absence of further limitations, an element defined by the phrase "comprising a ..." does not exclude the presence of other identical elements in the process, method, article, or device comprising the element.

[0028] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A MO source system for chemical vapor deposition equipment, comprising a pressure reducing valve, a Sorce-MFC, a Push-MFC, a pressure controller, a Line valve, a RUN valve, an exhaust valve, and a manual valve, characterized in that: The pressure reducing valve is used to control the intake pressure of the single-channel MO source system; The Sorce-MFC is used to control the carrier gas flowing into the source bottle; The Push-MFC is used to further add carrier gas to dilute the carrier gas flowing out of the source bottle; The pressure controller is used to control the pressure of the outflowing gas; The Line valve is used to control whether the carrier gas flows through the source bottle, open for flow, closed for bypass; The RUN valve is used to control whether the carrier gas is connected to the machine for use. When it is open, it is connected to the machine, and when it is closed, it is connected to the exhaust system. The air extraction valve is used to evacuate the pipeline when changing the source; The manual valve is used to cut the pipeline into the exhaust system when changing the source; The system also includes a water bath, a flow meter and a pressure gauge, and the MO source cylinder is located in the water bath. The flow meter and pressure gauge are respectively used to monitor and control the flow and pressure of the carrier gas in real time.

2. The MO source system for chemical vapor deposition equipment according to claim 1, characterized in that: The Line valve is a two-position four-way solenoid valve, and the RUN valve is a two-position five-way solenoid valve.

3. The MO source system for chemical vapor deposition equipment according to claim 1, characterized in that: The pressure reducing valve is installed at the gas inlet, with its input connected to the carrier gas supply source and its output connected to the subsequent Sorce-MFC.

4. The MO source system for chemical vapor deposition equipment according to claim 1, characterized in that: The input end of the Sorce-MFC is connected to the output end of the pressure reducing valve, and its output end is connected to the source bottle. The input end of the Push-MFC is connected to the carrier gas supply source, which can be shared with the carrier gas supply before the pressure reducing valve, and its output end is connected to the outflow pipeline of the source bottle for diluting the carrier gas flowing out of the source bottle.

5. The MO source system for chemical vapor deposition equipment according to claim 1, characterized in that: The pressure controller is installed on the pipeline outflowing from the source bottle and is located at the outlet of the source bottle, and is used to monitor and control the pressure of the outflowing gas in real time.

6. The MO source system for chemical vapor deposition equipment according to claim 1, characterized in that: The Line valve is installed on the connecting pipeline between the carrier gas and the source bottle to control whether the carrier gas flows through the source bottle; the RUN valve is installed at the output end of the system and connected to the exhaust system.

7. The MO source system for chemical vapor deposition equipment according to claim 1, characterized in that: The exhaust valve is connected to the exhaust pipeline to facilitate evacuating the pipeline when changing the source, and a normally closed pneumatic valve is also installed on the exhaust pipeline. The manual valve cuts the pipeline into the exhaust system when changing the source.

Citation Information

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