A solid precursor delivery system and method
By designing a solid precursor delivery system, the problems of insufficient sublimation of solid precursors and condensation into particles were solved, efficient thin film deposition and precise flow control were achieved, and production efficiency and product quality were significantly improved.
Patent Information
- Application Number
- CN202510185650.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-20
- Publication Date
- 2025-09-09
- Estimated Expiration
- 2045-02-20
AI Technical Summary
How to effectively sublimate solid precursors and avoid condensation into particles during transportation to prevent contamination of precision components and reaction chambers, especially in the preparation of metal thin films Mo, the application of MoO2Cl2 or MoCl5.
A solid-state precursor delivery system was designed, including a precursor source bottle, a source bottle valve group, a pre-gasification pipeline, a buffer, an inert gas pipeline, a preheating device and a mass flow meter. Heating and filtering were used to ensure that the precursor was fully sublimated and maintained in the gas phase during the delivery process. A buffer was used to stabilize the gas pressure, and a preheating device was used to eliminate particles, ensuring gas purity and precise flow control.
It improves the sublimation rate of solid precursors, reduces pipeline blockage and reaction chamber pollution, extends the service life of the flow meter, and improves the yield rate and production efficiency of thin film deposition.
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Figure CN119932535B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of furnace tube type vacuum coating equipment, and in particular to a solid precursor delivery system and method. Background Art
[0002] The fabrication of semiconductor devices and integrated circuits typically requires vapor deposition of materials onto suitable substrates. Chemical vapor deposition (CVD) precursors, including ALD and CVD, are liquid or solid at ambient temperature and pressure. They sublime into gases upon heating, with the heating temperature depending on the precursor's properties. With technological advancements, a growing number of precursor source materials have been developed for use in semiconductor thin film manufacturing. Solid precursors, in particular, are required for the preparation of some metal thin films. Solid precursors have lower vapor pressures than liquid precursors, making efficient sublimation a major technical challenge. To allow the solid precursor to enter the reaction chamber, heating within the piping and container is required to effectively sublimate the solid precursor, thereby reducing the freezing point and leading to particle generation. Particles in the piping can cause irreversible damage to precision components (valves, flowmeters, etc.) and can also contaminate the reaction chamber.
[0003] In the preparation of Mo thin films, the precursors are typically MoO2Cl2 or MoCl5, which are solid at room temperature. Therefore, when using this precursor in the ALD process, it must be sublimated into a gaseous state before being transported. This presents a technical challenge: ensuring that the Mo source is fully sublimated and prevented from condensing into solid particles in the downstream transport system. Summary of the Invention
[0004] The purpose of the present invention is to provide a solid precursor delivery system and method to solve the problems raised in the above background technology.
[0005] The above technical objectives of the present invention are achieved through the following technical solutions:
[0006] A solid precursor delivery system includes a precursor source bottle, a source bottle valve group, a precursor pre-gasification pipeline, a buffer, an inert gas pipeline, a first preheating device, a first mass flow meter, a second preheating device and a reaction chamber. The source bottle valve group is installed on the inlet and outlet ends of the precursor source bottle, the precursor pre-gasification pipeline is connected to the outlet end of the source bottle valve group, the buffer is provided with two air inlet ends, the precursor pre-gasification pipeline and the inert gas pipeline are respectively connected to the two air inlet ends of the buffer, the buffer is connected to the reaction chamber through a pipeline, the first preheating device, the first mass flow meter and the second preheating device are all installed on the pipeline, the first preheating device is located at the front end of the first mass flow meter, the second preheating device is located at the rear end of the first mass flow meter, and the second preheating device is located at the inlet end of the reaction chamber. The first preheating device and the second preheating device have the same structure.
[0007] Preferably, the precursor source bottle includes a steel cylinder, a side heating belt and a bottom heating belt, the side heating belt is installed on the outside of the steel cylinder, the bottom heating belt is installed on the bottom of the steel cylinder, and a temperature measuring point is also provided on the outside of the steel cylinder.
[0008] Preferably, the source bottle valve group includes a first diaphragm valve, a second diaphragm valve, a third diaphragm valve, a heating component, an inlet connector and an outlet connector. The first diaphragm valve and the third diaphragm valve are both connected to the precursor source bottle through a pipeline. The second diaphragm valve is connected to the first diaphragm valve and the third diaphragm valve through a pipeline. The inlet connector and the outlet connector are respectively installed on the pipelines on both sides of the second diaphragm valve. The inlet connector is externally connected to an inert gas pipe. An electromagnetic control valve is installed on the inlet connector. The heating component is arranged between the first diaphragm valve, the second diaphragm valve and the third diaphragm valve. The heating component is used to heat the first diaphragm valve, the second diaphragm valve, the third diaphragm valve and the connected pipelines. The heating component can be a wrapped heating belt or a heating rod structure. The outlet connector is connected to the precursor pre-gasification pipeline.
[0009] Preferably, the precursor pre-gasification pipeline is provided with a heating component, and the precursor pre-gasification pipeline includes a filter, a fourth diaphragm valve, a fifth diaphragm valve and a first pressure gauge. The filter is installed at the inlet end of the precursor pre-gasification pipeline, and the first pressure gauge is installed between the fourth diaphragm valve and the fifth diaphragm valve. The first pressure gauge is used to detect the saturated vapor pressure from the precursor source bottle. An exhaust pipeline is also provided between the filter and the fourth diaphragm valve, and a sixth diaphragm valve is installed on the exhaust pipeline. The exhaust pipeline is a bypass branch.
[0010] Preferably, the fifth diaphragm valve is connected to the buffer via a pipeline, and a second pressure gauge is installed on the buffer.
[0011] Preferably, the inert gas pipeline includes a second mass flow meter and a gas heating device, the second mass flow meter is arranged in front of the gas heating device, the gas heating device is connected to the buffer through a pipeline, and the second mass flow meter is used to control the gas flow entering the buffer.
[0012] Preferably, the first preheating device includes an air flow channel, a heating wire and a reflective plate. The cavity of the air flow channel is made of light-transmitting quartz material. Staggered baffles are arranged in the air flow channel, and the baffles are welded to the air flow channel. The heating wire is arranged on both sides of the air flow channel, and the reflective plate is arranged on the outside of the heating wire. The heating wire generates heat radiation and transmits it to the process gas in the air flow channel. A temperature sensor is also provided on the air flow channel.
[0013] A solid precursor delivery method, the delivery method comprising:
[0014] S1 Precursor Sublimation: The precursor source bottle and source bottle valve group heat the precursor to sublime the solid precursor. The sublimated gaseous precursor is filtered through the filter and then enters the buffer;
[0015] S2 Precursor Storage: The buffer stores gaseous precursors and heated inert gases, maintaining constant pressure and temperature to ensure a large-dose supply of process gases to the furnace equipment.
[0016] S3 Precursor metering: The process gas is preheated by the first preheating device to ensure that there are no particles, and then the flow rate is controlled by the first mass flow meter;
[0017] S4 Precursor enters the chamber: After passing through the second preheating device to ensure that there are no particles, the process gas enters the reaction chamber for thin film deposition reaction.
[0018] Beneficial effects: The present invention solves the problem of insufficient sublimation of solid precursors, increases the content of gas-phase process materials entering the reaction chamber, and improves the thin film deposition rate and the utilization rate of the precursor.
[0019] The present invention solves the problem of unsublimated solid precursors clogging precision components in pipelines, causing frequent malfunctions and inaccurate control of the precursor delivery system. It ensures that the gas flowing through the mass flow meter is completely vaporized and sublimated, achieving precise flow control without deviation.
[0020] The present invention solves the problem that precursor particles that are not completely vaporized before entering the reactor may pollute the process chamber. Before the pipeline enters the reaction chamber, a heating component is added to fully vaporize it, thereby reducing the number of particles entering the chamber. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 It is a structural diagram of an embodiment;
[0022] Figure 2 This is a schematic diagram showing a precursor source bottle and a valve assembly in an embodiment;
[0023] Figure 3 This is a schematic diagram of a pipeline diagram for illustrating the inlet and outlet positions of a buffer in an embodiment;
[0024] Figure 4 This is a schematic diagram of the structure of the preheating device used in the embodiment;
[0025] Figure 5 The diagram is a schematic diagram of an embodiment for illustrating the conveying method of the present invention.
[0026] Figure markings: 1. Precursor source bottle; 11. Steel cylinder; 12. Bottom heating belt; 13. Side heating belt; 2. Source bottle valve group; 21. First diaphragm valve; 22. Second diaphragm valve; 23. Third diaphragm valve; 24. Heating component; 25. Inlet connector; 26. Outlet connector; 3. Precursor pre-gasification pipeline; 31. Filter; 32. Fourth diaphragm valve; 33. Fifth diaphragm valve; 34. First pressure gauge; 35. Exhaust pipeline; 36. Sixth diaphragm valve; 4. Buffer; 41. Second pressure gauge; 5. Inert gas pipeline; 51. Second mass flow meter; 52. Gas heating device; 6. First preheating device; 61. Air flow channel; 62. Heating wire; 63. Reflection plate; 64. Baffle; 7. First mass flow meter; 8. Second preheating device; 9. Reaction chamber. DETAILED DESCRIPTION
[0027] The following description is merely a preferred embodiment of the present invention, and the scope of protection is not limited to this embodiment. All technical solutions based on the principles of the present invention should be within the scope of protection of the present invention. It should also be noted that improvements and modifications that do not depart from the principles of the present invention, which are within the scope of protection of the present invention, are within the scope of protection of the present invention.
[0028] like Figure 1 As shown, a solid precursor delivery system includes a precursor source bottle 1, a source bottle valve group 2, a precursor pre-gasification pipeline 3, a buffer 4, an inert gas pipeline 5, a first preheating device 6, a first mass flowmeter 7, a second preheating device 8 and a reaction chamber 9, the source bottle valve group 2 is installed at the inlet and outlet ends of the precursor source bottle 1, the precursor pre-gasification pipeline 3 is connected to the outlet end of the source bottle valve group 2, and the precursor pre-gasification pipeline 3 transports the sublimated precursor to the buffer 4 for storage; the buffer 4 is provided with two air inlet ends, the precursor pre-gasification pipeline 3 and the inert gas pipeline 5 are respectively connected to the two air inlet ends of the buffer 4, and the buffer 4 stores a mixed gas of the gaseous precursor sublimated from the precursor source bottle 1 and the inert gas from the inert gas pipeline 5.
[0029] The above-mentioned system structure design effectively solves the problem of insufficient sublimation of solid precursors. In actual applications, testing has shown that the sublimation rate of solid precursors can be increased by 30%, greatly reducing the risk of pipeline blockage caused by insufficient sublimation. At the same time, the purity of the gaseous precursor entering the reaction chamber 9 is improved, effectively reducing the probability of contamination of the process chamber by incompletely vaporized precursor particles, thereby improving the yield rate of thin film deposition and significantly improving production efficiency and product quality.
[0030] Buffer 4 is connected to reaction chamber 9 via a pipeline. A first preheating device 6, a first mass flowmeter 7, and a second preheating device 8 are all mounted on the pipeline. Inert gas acts as a carrier gas and dilution gas to transport the gaseous precursor into reaction chamber 9. Along the flow direction of the process gas, the first preheating device 6 is located at the front end of the first mass flowmeter 7, and the second preheating device 8 is located at the rear end of the first mass flowmeter 7. The second preheating device 8 is located at the inlet of reaction chamber 9. The first preheating device 6 is used to heat the process gas entering the first mass flowmeter 7, and the second preheating device 8 is used to process the gas entering reaction chamber 9.
[0031] Through such a layout design, the first preheating device 6 can fully heat the process gas about to enter the first mass flowmeter 7, ensuring that there are no solid particles in the gas flowing through the first mass flowmeter 7. Compared with the traditional transportation method, the incidence of mass flowmeter failure caused by particle blockage is effectively reduced by about 40%, greatly extending the service life of the first mass flowmeter 7, and can improve the flow control accuracy by 35%, providing more accurate parameter guarantee for the subsequent thin film deposition process.
[0032] The second preheating device 8 processes the gas about to enter the reaction chamber 9 again, which can reduce the content of incompletely vaporized precursor particles in the gas entering the reaction chamber 9 by 80%, significantly reducing the contamination of the reaction chamber 9 by particles, and increasing the yield rate of thin film deposition from the original 75% to 90%, greatly improving production efficiency and product quality.
[0033] like Figure 2As shown, the precursor source bottle 1 includes a steel cylinder 11, a side heating belt 13 installed on the outer periphery of the steel cylinder 11, and a bottom heating belt 12 installed at the bottom of the steel cylinder 11; a temperature measuring point is set on the outside of the steel cylinder 11 to monitor the temperature of the steel cylinder 11. The heating power of the bottom heating belt 12 and the side heating belt 13 is independently controlled through temperature feedback to make the steel cylinder 11 reach a preset temperature. The temperature range of the precursor source of the present invention is 120°C-150°C. This design brings many significant benefits. In actual application, precise temperature control can effectively ensure that the solid precursor is fully sublimated at an appropriate temperature. Compared with traditional methods, the precursor sublimation rate is increased by about 25%, greatly reducing the problems of pipeline blockage and reaction chamber contamination caused by insufficient sublimation. Moreover, the independent control of the heating power of the bottom heating belt and the side heating belt can better adapt to the sublimation requirements of different precursors, enhance the applicability and stability of the system, provide reliable temperature protection for the entire solid precursor delivery process, and effectively improve the quality and efficiency of the thin film deposition process.
[0034] The source bottle valve group 2 includes a first diaphragm valve 21, a second diaphragm valve 22, a third diaphragm valve 23, a heating component 24, an inlet connector 25 and an outlet connector 26. The first diaphragm valve 21 and the third diaphragm valve 23 are both connected to the precursor source bottle 1 through a pipeline. The second diaphragm valve 22 is connected to the first diaphragm valve 21 and the third diaphragm valve 23 through a pipeline. The inlet connector 25 and the outlet connector 26 are respectively installed on the pipelines on both sides of the second diaphragm valve 22. The inlet connector 25 is connected to an inert gas pipe. An electromagnetic control valve is installed on the inlet connector 25. The inlet connector 25 can be selectively connected to an inert gas or blocked. After research, the inventor found that the introduction of inert gas into the cylinder 11 during the process will cause dust from the solid precursor powder and cause a particle effect. Therefore, in the present invention, the electromagnetic control valve is closed to block the inlet connector 25. The heating element 24 is disposed between the first diaphragm valve 21, the second diaphragm valve 22, and the third diaphragm valve 23. The heating element 24 is used to heat the first diaphragm valve 21, the second diaphragm valve 22, the third diaphragm valve 23, and the connected pipelines. The heating element 24 can be a wrapped heating tape or a heating rod to heat the assembled source bottle valve assembly 2. The outlet connector 26 is connected to the precursor pre-gasification pipeline 3.
[0035] The precursor source bottle 1 can be one or more different steel cylinders 11. Solid precursors of different materials are set between different steel cylinders 11. The solid precursors are all connected to the buffer 4. Different precursor source bottles 1 can be selected and replaced; different precursor source bottles 1 are isolated by valves.
[0036] like Figure 3As shown, a heating component 24 is provided on each precursor pre-gasification pipeline 3 to heat the entire pipeline to avoid condensation. The precursor pre-gasification pipeline 3 includes a filter 31, a fourth diaphragm valve 32, a fifth diaphragm valve 33 and a first pressure gauge 34; the filter 31 is installed at the inlet end of the precursor pre-gasification pipeline 3. When the particles in the precursor source bottle 1 are larger than the filter diameter of the filter 31, they will not be able to pass through the filter 31 to enter the pipeline, thereby achieving a filtering effect. The first pressure gauge 34 is installed between the fourth diaphragm valve 32 and the fifth diaphragm valve 33. The first pressure gauge 34 detects the saturated vapor pressure from the precursor source bottle 1 and determines the temperature control temperature of the cylinder 11 based on the value of the saturated vapor pressure. Because as the temperature in the cylinder 11 increases, the saturated vapor pressure of the corresponding precursor will also increase. Therefore, it is necessary to monitor the saturated vapor pressure to set the set temperature of the cylinder 11 and maintain sufficient gas-phase precursor output. An exhaust line 35 is also provided between the filter 31 and the fourth diaphragm valve 32. A sixth diaphragm valve 36 is provided on the exhaust line 35. The exhaust line 35 is a bypass branch. The exhaust line 35 is connected to the vacuum pump end. After the sixth diaphragm valve 36 is opened, the precursor does not enter the cavity and is directly discharged from the exhaust line 35. This operation is used to purge the pipeline. Specifically, the heating component 24 effectively prevents the condensation problem caused by the temperature drop in the pipeline, reduces the risk of condensate blocking the pipeline, and improves the stability of the conveying system. The setting of the filter 31 blocks large particles of impurities from entering the pipeline, reduces the risk of damage to subsequent equipment, and ensures the purity of the conveying gas. The temperature of the cylinder 11 is controlled by detecting the saturated vapor pressure through the first pressure gauge 34, and the output of the gas-phase precursor is accurately adjusted to ensure the stable demand for the precursor in the thin film deposition process. The design of the exhaust pipe 35 and the sixth diaphragm valve 36 allows the pipe to be purged conveniently to remove residual impurities when necessary, further improving the reliability and cleanliness of the entire conveying system and providing a strong guarantee for the final high-quality thin film deposition process.
[0037] The buffer 4 contains the sublimated precursor and the inert gas from the inert gas pipeline 5 and keeps them in a gaseous state. Heating devices are provided around the buffer 4 to keep it heated. Preferably, the side wall temperature of the buffer 4 is set in the range of 130°C-170°C; the buffer 4 is provided with a second pressure gauge 41, which monitors the pressure in the buffer 4 and keeps the pressure in the buffer 4 stable to achieve the stability of the precursor supply.
[0038] The inert gas pipeline 5 includes a second mass flow meter 51 and a gas heating device 52. The second mass flow meter 51 is arranged in front of the gas heating device 52. The second mass flow meter 51 controls the gas flow entering the buffer 4. The gas heating device 52 heats the gas passing through the gas heating device 52 so that the temperature of the gas flowing out of the gas heating device 52 reaches the set temperature.
[0039] like Figure 4 As shown, the first preheating device 6 and the second preheating device 8 have the same structure, and only the installation position is different. The preheating device includes an air flow channel 61, a heating wire 62 and a reflector 63. The cavity of the air flow channel 61 is made of light-transmissive quartz material. Staggered baffles 64 are provided in the air flow channel 61. The baffles 64 block the flow direction of the air flow, thereby extending the retention time of the air flow in the air flow channel 61, thereby fully heating. Similarly, the baffles 64 are made of transparent quartz and are welded to the air flow channel 61; the heating wires 62 are provided on both sides of the air flow channel 61, and the reflector is provided. On the outside of the heating filament 62, the heating filament 62 generates heat radiation that is transferred to the process gas in the airflow channel 61. A reflector 63 is placed on the heating filament 62. Since the heat generated by the heating filament 62 is diffused in all directions, in order to avoid heat diffusion along unnecessary places and resulting in loss, the reflector 63 reflects the heat into the airflow channel 61. If there are unsublimated solid precursor particles in the airflow channel 61, the heat generated by the heating filament 62 will radiate to the particles, causing the particles to heat up and sublime. Therefore, the function of the preheating device is to fully sublimate the particles flowing therethrough. The airflow channel 61 is also provided with a temperature sensor to control the temperature in the airflow channel 61.
[0040] The first preheating device 6 fully sublimates the precursor to ensure that the process gas entering the first mass flow meter 7 is particle-free. On the one hand, it can improve the service life of the first mass flow meter 7. On the other hand, it makes the gas flowing through it particle-free, which can make the flow adjustment of the mass flow meter more accurate and facilitate the parameter control of thin film deposition. The second preheating device 8 fully vaporizes the precursor therein. Due to the measurement of the mass flow meter, the mass flow meter will also take away some heat, causing condensation and producing particles, so as to ensure that no particles enter the reaction chamber 9. The second preheating device 8 fully heats the process gas at the rear end of the first mass flow meter 7 to ensure that the gas entering the reaction chamber 9 is particle-free. The outlet of the second preheating device 8 is set close to the inlet of the reaction chamber 9 to reduce elbows and long-distance pipes and reduce the occurrence of cold spots. The length and inflection point in the figure are only for reference and do not represent the actual structure.
[0041] See Figure 5 As shown, a solid-state precursor delivery method:
[0042] S1 Precursor Sublimation: Precursor source bottle 1 and source bottle valve assembly 2 heat the precursor, causing the solid precursor to sublime. The sublimated vapor precursor is filtered through filter 31 before entering buffer 4. Specifically, the coordinated heating method of precursor source bottle 1 and source bottle valve assembly 2 can increase the sublimation efficiency of the solid precursor by 25% compared to traditional methods, effectively solving the problem of insufficient solid precursor sublimation. The provision of filter 31 further ensures the purity of the vapor precursor entering buffer 4, reducing the probability of subsequent equipment failure due to impurity particles.
[0043] S2 Precursor Storage: Buffer 4 caches gaseous precursors and heated inert gases, and maintains constant pressure and temperature to ensure a large supply of process gas to the furnace tube equipment. Specifically, the function of buffer 4 to maintain constant pressure and temperature enables the furnace tube equipment to obtain a stable large supply of process gas during long-term operation, thereby ensuring the continuity of the production process and reducing film quality defects caused by unstable gas supply.
[0044] S3 Precursor metering: The process gas is preheated by the first preheating device 6 to ensure that there are no particles, and then the flow rate is controlled by the first mass flow meter 7. Specifically, the pretreatment of the process gas by the first preheating device 6 effectively avoids damage to the first mass flow meter 7 by particles, extends the service life of the flow meter, and ensures the accuracy of flow control, making the gas flow control during the thin film deposition process more accurate, thereby improving the uniformity and consistency of thin film deposition.
[0045] S4 Precursor Entry: After passing through the second preheating device 8 to ensure it is free of particles, the process gas enters the reaction chamber 9 for the thin film deposition reaction. Specifically, the second preheating device 8 re-processes the process gas, almost completely eliminating particles from entering the reaction chamber 9. This reduces the probability of contamination from incompletely vaporized precursor particles, significantly improving the yield rate and quality stability of thin film deposition, and providing a strong guarantee for the production of high-quality thin films.
Claims
1. A solid precursor delivery system, comprising a precursor source bottle (1), a source bottle valve group (2), a precursor pre-gasification pipeline (3), a buffer (4), an inert gas pipeline (5), a first preheating device (6), a first mass flow meter (7), a second preheating device (8) and a reaction chamber (9), characterized in that: The source bottle valve group (2) is installed on the inlet and outlet ends of the precursor source bottle (1), the precursor pre-gasification pipeline (3) is connected to the outlet end of the source bottle valve group (2), the buffer (4) is provided with two air inlet ends, the precursor pre-gasification pipeline (3) and the inert gas pipeline (5) are respectively connected to the two air inlet ends of the buffer (4), the buffer (4) is connected to the reaction chamber (9) through a pipeline, the first preheating device (6), the first mass flow meter (7), and the second preheating device (8) are all installed on the pipeline, the first preheating device (6) is located at the front end of the first mass flow meter (7), the second preheating device (8) is located at the rear end of the first mass flow meter (7), and the second preheating device (8) is located at the rear end of the first mass flow meter (7). Located at the inlet end of the reaction chamber (9), the first preheating device (6) and the second preheating device (8) have the same structure; the first preheating device (6) includes an air flow channel (61), a heating wire (62) and a reflecting plate (63); the cavity of the air flow channel (61) is made of light-transmissive quartz material; staggered baffles (64) are arranged in the air flow channel (61); the baffles (64) are welded on the air flow channel (61); the heating wire (62) is arranged on both sides of the air flow channel (61); the reflecting plate (63) is arranged on the outside of the heating wire (62); the heating wire (62) generates heat radiation and transmits it to the process gas in the air flow channel (61); and a temperature sensor is also arranged on the air flow channel (61).
2. A solid precursor delivery system according to claim 1, characterized in that: The precursor source bottle (1) comprises a steel cylinder (11), a side heating belt (13) and a bottom heating belt (12), wherein the side heating belt (13) is installed on the outside of the steel cylinder (11), and the bottom heating belt (12) is installed on the bottom of the steel cylinder (11). A temperature measuring point is also provided on the outside of the steel cylinder (11).
3. A solid precursor delivery system according to claim 2, characterized in that: The source bottle valve group (2) includes a first diaphragm valve (21), a second diaphragm valve (22), a third diaphragm valve (23), a heating component (24), an inlet connector (25) and an outlet connector (26). The first diaphragm valve (21) and the third diaphragm valve (23) are both connected to the precursor source bottle (1) through a pipeline. The second diaphragm valve (22) is connected to the first diaphragm valve (21) and the third diaphragm valve (23) through a pipeline. The inlet connector (25) and the outlet connector (26) are respectively installed on the pipelines on both sides of the second diaphragm valve (22). The inlet connector (25) is externally connected to an inert gas pipe, an electromagnetic control valve is installed on the inlet connector (25), the heating component (24) is arranged between the first diaphragm valve (21), the second diaphragm valve (22), and the third diaphragm valve (23), the heating component (24) is used to heat the first diaphragm valve (21), the second diaphragm valve (22), the third diaphragm valve (23) and the connected pipelines, the heating component (24) can be a winding heating belt or a heating rod structure, and the outlet connector (26) is connected to the precursor pre-gasification pipeline (3).
4. A solid precursor delivery system according to claim 1, characterized in that: The precursor pre-gasification pipeline (3) is provided with a heating component (24), and the precursor pre-gasification pipeline (3) includes a filter (31), a fourth diaphragm valve (32), a fifth diaphragm valve (33) and a first pressure gauge (34). The filter (31) is installed at the inlet end of the precursor pre-gasification pipeline (3), and the first pressure gauge (34) is installed between the fourth diaphragm valve (32) and the fifth diaphragm valve (33). The first pressure gauge (34) is used to detect the saturated vapor pressure from the precursor source bottle (1). An exhaust pipeline (35) is also provided between the filter (31) and the fourth diaphragm valve (32), and a sixth diaphragm valve (36) is installed on the exhaust pipeline (35). The exhaust pipeline (35) is a bypass branch.
5. A solid precursor delivery system according to claim 4, characterized in that: The fifth diaphragm valve (33) is connected to the buffer (4) through a pipeline, and a second pressure gauge (41) is installed on the buffer (4).
6. The solid precursor delivery system according to claim 1, characterized in that: The inert gas pipeline (5) includes a second mass flow meter (51) and a gas heating device (52). The second mass flow meter (51) is arranged in front of the gas heating device (52). The gas heating device (52) is connected to the buffer (4) through a pipeline. The second mass flow meter (51) is used to control the gas flow entering the buffer (4).
7. A method for delivering a solid precursor according to any one of claims 1 to 6, characterized in that: Delivery methods include: S1 Precursor sublimation: The precursor source bottle (1) and the source bottle valve assembly (2) heat the precursor to sublime the solid precursor, and the sublimated gaseous precursor is filtered through the filter (31) and then enters the buffer (4); S2 Precursor Storage: The buffer (4) stores gaseous precursors and heated inert gas and maintains constant pressure and temperature to ensure a large-dose process gas supply to the furnace equipment; S3 Precursor metering: The process gas is preheated by a first preheating device (6) to ensure that there are no particles, and then the flow rate is controlled by a first mass flow meter (7); S4 Precursor enters the chamber: After the process gas passes through the second preheating device (8) to ensure that there are no particles, it enters the reaction chamber (9) for thin film deposition reaction.
Citation Information
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