High-flow-rate gas generator and supply method suitable for chemical vapor deposition equipment

Abstract

This invention discloses a high-flow-rate gas generator and supply method suitable for chemical vapor deposition equipment, belonging to the field of gas semiconductor manufacturing technology. This invention uses a butterfly valve instead of a traditional flow meter to supply flow, avoiding the disadvantages of high resistance and low flow rate associated with flow meters. Furthermore, the generator integrates vibration and heating devices, using temperature and vibration coupling control, combined with closed-loop pressure control, to ensure the high-flow-rate gas generator can maintain a constant target gas pressure, thus ensuring a stable gas supply flow rate. Moreover, this invention achieves high-precision control by using a mature PID algorithm to rapidly reach the target flow rate through closed-loop pressure control. This invention achieves a balance between flow rate, accuracy, and stability.

Description

Technical Field

[0001] This invention relates to a high-flow-rate gas and supply method suitable for chemical vapor deposition equipment, belonging to the field of gas semiconductor manufacturing technology. Background Technology

[0002] Chemical vapor deposition (CVD) is a process used to prepare thin film materials in semiconductors and optoelectronic devices. Atomic layer deposition (ALD) is essentially a CVD process with higher precision in controlling film thickness and quality. It achieves precise control over film thickness and composition by alternately introducing different chemical vapor precursors on the substrate surface and depositing materials layer by layer on the substrate through chemical reactions. Its core lies in the self-limiting surface chemical reaction mechanism, where only one layer of atoms is deposited in each reaction, thus obtaining very uniform and dense films.

[0003] In both CVD and ALD processes, raw material supply is a crucial component. The stability, accuracy, and flow rate of the raw material supply directly determine the quality of the manufactured materials. With the continuous development of semiconductor materials, their applications have permeated various industries, leading to increasingly stringent requirements for the quality of deposited thin films. However, raw material supply, as one of the key factors affecting the quality of deposited thin films, has received insufficient attention. For example, the application of single-walled carbon nanotubes in battery slurries requires a high-flow-rate, highly stable, and highly precise gaseous carbon source supply to achieve high-quality growth of single-walled carbon nanotubes. Currently, the carbon source supply method used is the traditional flow meter method.

[0004] While traditional flow meter-based flow control can achieve high-precision control, it cannot supply large volumes of gas due to its own pipeline resistance (high-precision flow meters typically have thinner pipelines, resulting in their own pipeline resistance), thus failing to meet the needs of industrial-grade semiconductor material manufacturing. Other methods that can supply large volumes cannot achieve high stability and high-precision control. Therefore, existing gas flow supply methods cannot achieve a balance between flow rate, accuracy, and stability. Summary of the Invention

[0005] To further ensure the deposition effect, this invention provides a high-flow-rate gas generator and supply method suitable for chemical vapor deposition equipment, providing a high-flow-rate, highly stable, and highly precise gas supply for thin film deposition or atomic-level material growth.

[0006] A high-flow-rate gas supply method suitable for chemical vapor deposition equipment is disclosed. The method is based on a high-flow-rate gas generator, which includes a source bottle, a heating device, an atomizer, a pressure gauge, and a controller. The source bottle stores a gas source in a liquid state. The heating device and atomizer convert the gas source in the source bottle from a liquid state to a gaseous state. The controller adjusts the power of the heating device and atomizer according to the required flow rate to regulate the gas pressure inside the source bottle. Optionally, in the high-flow-rate gas generator, the heating device is located outside the source bottle, and the atomizer is located inside the source bottle. A three-way valve connects the source bottle opening to the pressure gauge. An angle valve connects the pressure gauge to the three-way valve, and another passage of the three-way valve is connected to a gas supply pipeline via a butterfly valve. The gas supply pipeline is connected to the vapor deposition chamber. The heating device, atomizer, and pressure gauge are all connected to the controller. The method includes:

[0007] Step 1: For a gas source that exists in a liquid state inside the source bottle, calibrate the relationship between pressure and flow rate inside the source bottle;

[0008] Step 2: Determine the target pressure value inside the source bottle based on the required flow rate, and use a PID algorithm to control the power of the heating device and atomizer to stabilize the pressure inside the source bottle at the target pressure value.

[0009] Optionally, step 1 includes:

[0010] Step 1.1: Store the liquid gas source in the source bottle, and adjust the power of the heating device and atomizer to stabilize the gas pressure inside the source bottle. The gas pressure inside the vapor deposition chamber is evacuated to a vacuum. The butterfly valve is then opened to supply gas to the vapor deposition chamber at a certain flow rate (N). After a certain time, the pressure inside the vapor deposition chamber is measured and recorded as N. ;

[0011] Step 1.2, calibrate the mass flow meter using flow rate as the metric. 标定 The calibration gas is also supplied for N time, and the pressure inside the vapor deposition chamber is... ;

[0012] Step 1.3: Calculate the stable gas pressure inside the source bottle using the following flow conversion formula. The actual flow rate corresponding to the gas flow rate supplied to the vapor deposition chamber for N time at a gas flow rate of kPa. :

[0013]

[0014] in, 标定 The gas flow rate is for calibration purposes and is a known quantity. 气体源The mass flow rate conversion factor is the mass flow rate of the gas source stored in the source bottle in liquid form. 标定 To determine the mass flow rate conversion factor for the calibration gas;

[0015] Step 1.4: Repeat steps 1.1 to 1.3 above to obtain a stable gas pressure inside the source bottle. The actual flow rate corresponding to the gas flow rate supplied to the vapor deposition chamber for N time at a gas flow rate of kPa. , ≠ ;

[0016] Step 1.5, based on the gas pressure inside the source bottle obtained in Steps 1.3 and 1.4 , Corresponding actual traffic , The parameters in the fitting formula for determining the relationship between the gas pressure P and the flow rate Q inside the source bottle are... and :

[0017]

[0018] in, Q represents the gas pressure inside the source bottle. The corresponding gas flow rate at that time.

[0019] Optionally, step 2, which uses a PID algorithm to control the power of the heating device and the atomizer to stabilize the pressure inside the source bottle at the target pressure value, further includes: determining the relationship between the temperature provided by the heating device and the vibration power of the atomizer coupled with the liquid-vapor conversion efficiency.

[0020] Define the current power of the heating device as: 加热 = 当前 2 汽化 ,in 当前 Indicates the current generator temperature. 汽化 Indicates the vaporization temperature of the liquid inside the source bottle;

[0021] Define the power of the atomizer as 雾化 The current power of the overall generator is recorded as: 加热 雾化 ,in , These are the power weighting coefficients for the heating device and the atomizer, respectively, adjusted by controlling the overall generator power. They will receive corresponding pressure.

[0022] Optional, , The value is determined using the following method:

[0023] The source bottle is heated to a certain temperature using a heating device. , > 汽化 Adjust the atomizer power to half of its maximum power, denoted as . 雾化1 After the gas pressure inside the source bottle stabilizes, observe the pressure gauge reading. ;

[0024] Keeping the atomizer power constant, adjust the heating device to heat the source bottle to the specified temperature. , ≤2 汽化 The pressure gauge showed an air pressure of ;

[0025] Adjust the heating temperature back to normal. Adjust the atomizer power to 雾化2 , 雾化2 雾化1 The pressure gauge showed a pressure of ;

[0026] Then correspondingly:

[0027]

[0028] The derivation yields , :

[0029]

[0030]

[0031] The heating device is a heating jacket with a temperature display function; adjusting its temperature will automatically adjust its power.

[0032] Optionally, the calibration gas in step 1.2 is Ar / H2 gas.

[0033] Optionally, the The value ranges from 1 kPa to 3 kPa.

[0034] Optionally, the gas source existing in liquid form includes ethanol, methanol, and phenol.

[0035] A second objective of this invention is to provide a high-flow-rate gas generator suitable for chemical vapor deposition equipment. The high-flow-rate gas generator includes: a source bottle, a heating device, an atomizer, a pressure gauge, and a controller. The source bottle is used to store a gas source that exists in a liquid state. The heating device and the atomizer are used to convert the gas source in the source bottle from a liquid state to a gas state. The controller is used to adjust the power of the heating device and the atomizer according to the required flow rate to adjust the gas pressure in the source bottle.

[0036] Optionally, in the high-flow-rate gas generator, the heating device is located outside the source bottle, the atomizer is located inside the source bottle, the source bottle opening is connected to the pressure gauge via a three-way valve, the pressure gauge is connected to the three-way valve via an angle valve, the other passage of the three-way valve is connected to the gas supply pipeline via a butterfly valve, and the gas supply pipeline is connected to the vapor deposition chamber; the heating device, atomizer, and pressure gauge are all connected to the controller.

[0037] Optionally, the source bottle material includes stainless steel, glass, ceramic, and Teflon.

[0038] The beneficial effects of this invention are:

[0039] 1. High flow rate: This invention uses a butterfly valve instead of a traditional flow meter to supply flow, avoiding the disadvantages of high resistance and low flow rate associated with flow meters. Furthermore, the generator integrates vibration and heating devices, maximizing the generation of the gas source.

[0040] 2. High Stability: While ensuring a large flow rate, this invention can achieve a stable supply of a large flow rate. This invention uses coupled temperature and vibration control, combined with closed-loop pressure control, to enable the large-flow-rate gas generator to maintain a constant target gas pressure, thus ensuring a stable gas supply flow rate.

[0041] 3. High precision: This invention proposes a gas generation control method that couples temperature and vibration power to control the liquid-gas conversion efficiency. Through coupled control, higher precision gas pressure control is achieved, and through closed-loop control of gas pressure, a mature PID algorithm enables the gas pressure, i.e. the flow rate, to quickly reach the target flow rate, thus achieving high precision control. Attached Figure Description

[0042] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0043] Figure 1This is a schematic diagram of the high-flow-rate gas generator suitable for chemical vapor deposition equipment provided by the present invention, wherein 1-source bottle, 2-heating device, 3-atomizer, 4-three-way valve, 5-pressure gauge, 6-angle valve, 7-butterfly valve, and 8-gas supply pipeline.

[0044] Figure 2 This is a comparison chart showing the growth of single-walled carbon nanotubes with different flow rates of gas sources.

[0045] Figure 3 This is a comparison chart of gas flow supply for ethanol flow control using conventional flow meter methods and using the high-flow gas generator provided by this invention.

[0046] Figure 4 This is a gas flow supply diagram for ethanol flow control using the high-flow-rate gas generator provided in this application.

[0047] Figure 5 Raman spectra of single-walled carbon nanotubes grown using existing horiba flowmeters and the high-flow-rate gas generator provided in this invention are shown for comparison. Detailed Implementation

[0048] To make the objectives, technical solutions, and advantages of the present invention clearer, the embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

[0049] The conventional flow control methods are introduced below:

[0050] Existing ethanol flow supply methods: Ethanol is used as a carbon source for atomic layer thin film deposition. The existing supply method is to control the supply flow by using a flow tank with a flow meter. The flow is provided by the evaporation of ethanol itself, and the flow control is achieved by setting the flow meter parameters. In practical applications, this control method has two major drawbacks. First, ethanol has limited self-evaporation capacity, and after a period of use, the flow rate often decreases and fails to reach the set flow rate (related research shows that ethanol concentration affects the evaporation mode and rate of droplets on superhydrophobic surfaces. At low ethanol concentrations (≤20wt%), the droplet evaporation rate is slower and tends towards the constant contact angle (CCA) mode, while at high ethanol concentrations (40wt%~60wt%), the droplet evaporation rate is faster and tends towards the constant contact radius (CCR) mode. As ethanol evaporates, the concentration gradually decreases, which may cause the evaporation mode to change from the CCR mode to the CCA mode, thus reducing the evaporation rate). Second, the flow meter itself generates significant resistance in the pipeline. Even if the ethanol evaporation rate is increased by heating, the pipeline resistance of the flow meter itself still cannot provide a large flow rate, meaning it cannot simultaneously meet the requirements of high flow rate and high accuracy. Furthermore, the gas source flow rate will have a certain impact on the deposition film effect; please refer to [reference needed]. Figure 2 , Figure 2 The three images from left to right are scanning electron microscope (SEM) images of the growth of single-walled carbon nanotubes at gas flow rates of 100 sccm, 500 sccm, and 800 sccm, respectively. Under the condition that other factors remain unchanged, as the gas flow rate increases, the number of carbon nanotubes growing can be clearly observed to increase significantly under the same SEM scale.

[0051] As described above regarding existing carbon source supply methods, current gas source supply methods cannot provide large flow rates. Therefore, this application abandons the conventional flow meter control scheme and innovatively proposes a pressure control scheme instead of flow control. Furthermore, it proposes a method for calibrating the relationship between pressure and flow rate, and through atomization and heating coupling control, makes gas pressure control more stable and precise. This achieves a large flow rate, high stability, and high precision gas flow supply.

[0052] The high-flow-rate supply solution provided by this invention is also applicable to the supply of other liquid sources such as methanol and phenol.

[0053] Example 1

[0054] This embodiment provides a high-flow-rate gas generator suitable for chemical vapor deposition equipment. See [link to documentation]. Figure 1 The high-flow-rate gas generator includes a source bottle 1, a heating device 2 is installed outside the source bottle 1, an atomizer 3 is installed inside the source bottle 1, a pressure gauge 5 is connected to the bottle opening of the source bottle 1 through a three-way valve 4, an angle valve 6 is connected between the pressure gauge 5 and the three-way valve 4, and another passage of the three-way valve 4 is connected to the gas supply pipeline 8 through a butterfly valve 7; the gas supply pipeline 8 is connected to the chamber for depositing thin films.

[0055] This high-flow-rate gas generator is suitable for gas sources existing in liquid form, such as ethanol, methanol, and phenol. The control process of this high-flow-rate gas generator is described below using a tubular furnace as an example of a deposition equipment. The high-flow-rate gas generator provides the ethanol carbon source. The gas supply line 8 of the high-flow-rate gas generator is connected to the quartz tube chamber inside the tubular furnace (considering industry conventions, the pressure inside the tubular furnace will refer to the pressure inside the quartz tube chamber). The gas supply line 8 can be a corrugated pipe, and the heating device 2 can be a heating jacket. The high-flow-rate gas supply for the chemical vapor deposition process, based on this high-flow-rate gas generator, includes the following steps:

[0056] Step 1: Calibrate the relationship between flow rate and pressure;

[0057] Step 1.1: Store the gas source, which exists in liquid form, in source bottle 1, and adjust the power of heating device 2 and atomizer 3 to stabilize the gas pressure inside source bottle 1. The gas pressure inside the tubular furnace was evacuated to a vacuum. After opening butterfly valve 7 and supplying the tubular furnace with a certain gas flow rate for a certain period of time, the pressure inside the tubular furnace was measured and recorded as kPa. . The value range is typically from 1 kPa to 3 kPa. Gas sources existing in liquid form include ethanol, methanol, phenol, etc.

[0058] Step 1.2, calibrate the mass flow meter using flow rate as the metric. 标定 The calibration gas is also supplied to the tubular furnace for N time, after which the pressure inside the furnace is... ;

[0059] In this embodiment, the calibration gas is an Ar / H2 gas, with H2 accounting for 3% by volume. For ease of calculation, it can be calibrated using a mass flow meter to supply Ar / H2 gas at a flow rate of 1000 sccm for N time, after which the pressure inside the tubular furnace will be... .

[0060] Step 1.3: Calculate the stable gas pressure inside the source bottle using the following flow conversion formula. The actual flow rate corresponding to the gas flow rate N time supplied to the tubular furnace at a gas flow rate of kPa is... :

[0061]

[0062] in, 标定 The gas flow rate is for calibration purposes and is a known quantity. 气体源 The mass flow rate conversion factor is the mass flow rate of the gas source stored in the source bottle in liquid form. 标定 This is the mass flow rate conversion factor for the calibration gas.

[0063] The mass flow rate conversion factor of a substance can usually be obtained by consulting relevant technical manuals or calculated using the conversion factor calculation formula; the basic conversion factor calculation formula is as follows:

[0064]

[0065] in, Let be the density of the gas under standard conditions. The specific heat at constant pressure of a gas. It is the gas molecule composition coefficient, which is related to the components that make up the gas molecules.

[0066] If a mixed gas is used for calibration, the conversion factor is calculated using the following formula:

[0067]

[0068] in, , , , Let be the density of each gas in the gas mixture under standard conditions. , , , This represents the specific heat at constant pressure of each gas in the gas mixture. , , , The coefficients representing the composition of gas molecules in the gas mixture; , , , This refers to the flow rate of each gas in the gas mixture (which can be determined based on the proportion of each gas and the total flow rate). This represents the total flow rate of the mixed gas. For this embodiment, where ethanol is used as the carbon source and Ar / H2 as the calibration gas, the flow rate conversion formula is:

[0069]

[0070] in, Here, is the Ar / H2 mass flow rate conversion factor, and C is the ethanol mass flow rate conversion factor. For ease of calculation, in this embodiment... The value is 1000 sccm, but other values ​​can be selected in practical applications.

[0071] In practical applications, the gas calibrated in step 1.2 above can also be other gases, with corresponding mass flow conversion coefficients. This refers to the mass flow rate conversion factor for other gases. Typically, a gas with a known mass flow rate conversion factor can be used as the calibration gas.

[0072] Step 1.4: Repeat steps 1.1 to 1.3 above to obtain a stable gas pressure inside the source bottle. The actual flow rate corresponding to the gas flow rate N time supplied to the tubular furnace at a gas flow rate of kPa is... , .

[0073] Step 1.5, based on the gas pressure inside the source bottle obtained in Steps 1.3 and 1.4 , Corresponding actual traffic , The parameters in the fitting formula for determining the relationship between the gas pressure P and the flow rate Q inside the source bottle are... and :

[0074]

[0075] in, Q represents the gas pressure inside the source bottle. The corresponding gas flow rate at that time.

[0076] Step 2: Control the pressure;

[0077] Based on the flow rate and pressure relationship obtained in the first step above, controlling the pressure controls the flow rate. This generator's second major advantage is its ability to achieve stable and precise flow rate control, which in turn enables stable and precise pressure control. The method is as follows:

[0078] This invention uses closed-loop control, employing a pressure gauge to monitor the gas pressure inside the source cylinder in real time. The pressure inside the source bottle is controlled by adjusting the atomizer and controlling the generator temperature. When the target pressure is greater than the current pressure, the PID controller reduces the atomizer power and generator temperature accordingly; conversely, when the target pressure is less than the current pressure, the PID controller increases the atomizer power and generator temperature accordingly. This closed-loop control process can be implemented using existing PID control theory, adjusting the atomizer power and heating device power to control the air pressure inside the source bottle. Maintain at the predetermined value.

[0079] The specific control parameters of the PID controller are optimized by relevant technical personnel through experiments and adjustments based on the actual dynamic characteristics and control objectives. The specific adjustment process is not described in this embodiment.

[0080] This invention also proposes a formula for controlling the liquid-vapor conversion efficiency by coupling temperature and vibration power. In this invention, the heating device is a heating jacket with a temperature display function, and the corresponding target temperature can be directly set. The heating device adjusts its power to reach the corresponding target temperature. Therefore, in this invention, temperature is directly used as one of the control variables.

[0081] Temperature and atomization control result in different liquid-to-vapor conversion efficiencies; therefore, effective and rapid temperature control requires reasonable control of both temperature and atomizer power. Assume the current generator temperature is... 当前 The vaporization temperature of the liquid inside the source bottle is 汽化 Then the current power of the heating device can be approximated as:

[0082]

[0083] Assuming the current atomizer power is 雾化 Then the current power of the overall generator can be approximated as:

[0084]

[0085]

[0086] in , These are the power weighting coefficients for the heating element and the atomizer, respectively. The overall generator power is adjusted by... You can get the corresponding pressure.

[0087] During thin film deposition, after the gas generator is connected to the corresponding system (in the context of thin film deposition, the corresponding system here refers to a tube furnace), the source bottle is heated to the specified temperature using a heating device. ( > 汽化 Adjust the atomizer power to half of its maximum power, denoted as . 雾化1 After the gas pressure in the gas generator (i.e., the gas pressure inside the source bottle) stabilizes, observe the pressure gauge reading. Keeping the atomizer power constant, adjust the heating device to heat the source bottle to the specified temperature. ( ≤2 汽化 The pressure gauge showed an air pressure of [value missing]. Adjust the heating temperature back to the original temperature. Adjust the atomizer power to 雾化2 The pressure gauge showed a pressure of Then, correspondingly:

[0088]

[0089] Right now

[0090]

[0091]

[0092] , It is only suitable for temperatures and powers with large flow output.

[0093] Example 2

[0094] This embodiment provides a specific example of thin film deposition: taking the preparation of single-walled carbon nanotubes as an example, the high-flow-rate gas generator provided in Example 1 is used to supply the gas source to achieve large-area growth of single-walled carbon nanotubes, and the gas source is ethanol.

[0095] In this embodiment, an argon-hydrogen mixture containing 3% hydrogen is used as the calibration gas, and its mass flow conversion factor is: 1.40, the mass flow rate conversion factor for ethanol is =0.39. When an argon-hydrogen mixture with N = 1000 sccm per minute is introduced, the pressure inside the furnace is... =20.1 kPa. The pressure of the control generator is... =10 kPa, after ethanol gas is introduced for 1 minute, the pressure inside the furnace is =14.2 kPa, then according to the formula, the ethanol flow rate corresponding to a pressure of 20 kPa is:

[0096]

[0097] Using the same method, the flow rate was measured to be 3524 sccm when the generator pressure was 30 kPa. The fitted relationship between pressure and flow rate is as follows:

[0098]

[0099] The unit for flow rate is sccm, and the unit for pressure is kPa.

[0100] The corresponding efficiency of liquid-gas conversion was calculated using the formula for temperature and vibration power coupling control provided in Example 1. =0.62, =0.38. When the pressure needs to be adjusted from 10 kPa to 15 kPa, the PLC will adjust the required power in real time using a PID algorithm. Assuming the current required power is 60%, the atomizer power needs to be adjusted to 70.3%, the heating mantle power to 43.1%, and the heating mantle temperature to 67.5℃.

[0101] Figure 3 The graph compares the gas supply for ethanol flow control using a conventional flow meter and the high-flow-rate gas generator provided by this invention. It can be seen that the pressure value is higher when using the high-flow-rate gas generator provided by this invention for ethanol flow control, meaning that the high-flow-rate gas generator provided by this invention can provide a large flow of ethanol gas. Figure 4 The process of adjusting the gas pressure inside the bottle from 8 kPa to 15 kPa when using the high-flow gas generator provided by the present invention to provide a gas source shows that the pressure can be adjusted to 15 kPa after about 70 seconds, corresponding to a flow rate of 2042 sccm, and the error can be stabilized within ±1%, that is, the present invention can provide a stable flow rate.

[0102] To further highlight the superior performance of the high-flow-rate gas generator provided in this application in chemical vapor deposition scenarios, this embodiment also presents a comparison of the results of providing a carbon source for the growth process of single-walled carbon nanotubes using an existing advanced flow controller (Horiba flow meter) capable of providing a flow rate of 2000 sccm and the high-flow-rate gas generator provided in this invention. Figure 5 The Raman spectra of the corresponding grown single-walled carbon nanotubes show that the Raman spectrum of the single-walled carbon nanotubes supplied with carbon source by the high-flow-rate gas generator provided by this invention has a G / D ratio (i.e., the ratio of G peak intensity to D peak intensity) of 30, while the G / D ratio of the single-walled carbon nanotubes supplied with carbon source by the existing horiba flow meter is only 11. A higher G / D ratio usually means that the material has better crystallinity and fewer lattice defects. In other words, using the high-flow-rate gas generator provided by this invention to supply carbon source can result in better quality of the grown single-walled carbon nanotubes.

[0103] Some steps in the embodiments of the present invention can be implemented using software, and the corresponding software program can be stored in a readable storage medium, such as an optical disc or a hard disk.

[0104] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A high-flow-rate gas supply method suitable for chemical vapor deposition equipment, the method being implemented based on a high-flow-rate gas generator, characterized in that, The high-flow-rate gas generator includes: a source bottle, a heating device, an atomizer, a pressure gauge, and a controller; wherein the source bottle is used to store a gas source existing in a liquid state, the heating device and the atomizer are used to convert the gas source in the source bottle from a liquid state to a gas state, and the controller is used to adjust the power of the heating device and the atomizer according to the required flow rate to adjust the gas pressure in the source bottle; In the high-flow-rate gas generator, the heating device is located outside the source bottle, and the atomizer is located inside the source bottle. A three-way valve connects the source bottle opening to the pressure gauge, and an angle valve connects the pressure gauge to the three-way valve. The other passage of the three-way valve is connected to a gas supply pipeline via a butterfly valve, and the gas supply pipeline is connected to a vapor deposition chamber. The heating device, atomizer, and pressure gauge are all connected to the controller. The method includes: Step 1: For a gas source that exists in a liquid state inside the source bottle, calibrate the relationship between pressure and flow rate inside the source bottle; Step 2: Determine the target pressure value inside the source bottle based on the required flow rate, and use a PID algorithm to control the power of the heating device and atomizer to stabilize the pressure inside the source bottle at the target pressure value. Step 1 includes: Step 1.1: Store the liquid gas source in the source bottle, and adjust the power of the heating device and atomizer to stabilize the gas pressure inside the source bottle. The gas pressure inside the vapor deposition chamber is evacuated to a vacuum. The butterfly valve is then opened to supply gas to the vapor deposition chamber at a certain flow rate (N). After a certain time, the pressure inside the vapor deposition chamber is measured and recorded as N. ; Step 1.2, calibrate the mass flow meter using flow rate as the metric. 标定 The calibration gas is also supplied to the vapor deposition chamber for N time, after which the pressure inside the chamber is... ; Step 1.3: Calculate the stable gas pressure inside the source bottle using the following flow conversion formula. The actual flow rate corresponding to the gas flow rate supplied to the vapor deposition chamber for N time at a gas flow rate of kPa. : in, 标定 The gas flow rate is for calibration purposes and is a known quantity. 气体源 The mass flow rate conversion factor is the mass flow rate of the gas source stored in the source bottle in liquid form. 标定 To determine the mass flow rate conversion factor for the calibration gas; Step 1.4: Repeat steps 1.1 to 1.3 above to obtain a stable gas pressure inside the source bottle. The actual flow rate Q2 corresponding to the gas flow rate N time supplied to the vapor deposition chamber at kPa is given. ≠ ; Step 1.5, based on the gas pressure inside the source bottle obtained in Steps 1.3 and 1.4 , Corresponding actual traffic , The parameters in the fitting formula for determining the relationship between the gas pressure P and the flow rate Q inside the source bottle are... and : in, Q represents the gas pressure inside the source bottle. The corresponding gas flow rate at that time; Step 2, which uses a PID algorithm to control the power of the heating device and the atomizer to stabilize the pressure inside the source bottle at the target pressure value, also includes: determining the relationship between the coupled temperature provided by the heating device and the vibration power of the atomizer and the liquid-vapor conversion efficiency. Define the current power of the heating device as: 加热 = 当前 2 汽化 ,in 当前 Indicates the current generator temperature. 汽化 Indicates the vaporization temperature of the liquid inside the source bottle; Define the power of the atomizer as 雾化 The current power of the overall generator is recorded as: 加热 雾化 ,in , These are the power weighting coefficients for the heating device and the atomizer, respectively, adjusted by controlling the overall generator power. Receive the corresponding pressure; The power weighting coefficient of the heating device and the atomizer , The value is determined using the following method: The source bottle is heated to a certain temperature using a heating device. , > 汽化 Adjust the atomizer power to half of its maximum power, denoted as . 雾化1 After the gas pressure inside the source bottle stabilizes, observe the pressure gauge reading. ; Keeping the atomizer power constant, adjust the heating device to heat the source bottle to the specified temperature. , ≤2 汽化 The pressure gauge showed an air pressure of ; Adjust the heating temperature back to normal. Adjust the atomizer power to 雾化2 , 雾化2 雾化1 The pressure gauge showed a pressure of ; but , They are respectively: The heating device is a heating jacket with a temperature display function; adjusting its temperature will automatically adjust its power.

2. The high-flow-rate gas supply method according to claim 1, characterized in that, In step 1.2, the calibration gas used is Ar / H2 gas.

3. The high-flow-rate gas supply method according to claim 2, characterized in that, The The value ranges from 1 kPa to 3 kPa.

4. The high-flow-rate gas supply method according to claim 3, characterized in that, The gas sources existing in liquid form include ethanol, methanol, and phenol.

5. A high-flow-rate gas generator suitable for chemical vapor deposition equipment, characterized in that, The high-flow-rate gas generator includes: a source bottle, a heating device, an atomizer, a pressure gauge, and a controller; wherein the source bottle is used to store a gas source existing in a liquid state, the heating device and the atomizer are used to convert the gas source in the source bottle from a liquid state to a gas state, and the controller is used to execute the method according to any one of claims 1-4 to adjust the power of the heating device and the atomizer according to the required flow rate to adjust the gas pressure in the source bottle; In the high-flow-rate gas generator, the heating device is located outside the source bottle, the atomizer is located inside the source bottle, the source bottle opening is connected to the pressure gauge via a three-way valve, the pressure gauge is connected to the three-way valve via an angle valve, the other passage of the three-way valve is connected to the gas supply pipeline via a butterfly valve, and the gas supply pipeline is connected to the gas phase deposition chamber; the heating device, atomizer, and pressure gauge are all connected to the controller.

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