Substrate processing apparatus, liquid raw material replenishment system, method of manufacturing semiconductor device, substrate processing method, and recording medium

Abstract

A technology is provided comprising: a vaporization container for vaporizing a liquid feedstock inside; a liquid feedstock replenishment line, one end of which is connected to the vaporization container and the other end of which is connected to a liquid feedstock supply source; a first valve disposed on the liquid feedstock replenishment line; a second valve disposed on the liquid feedstock replenishment line upstream of the first valve; a liquid feedstock storage section formed between the first valve and the second valve; and a control section for controlling the opening and closing of the first valve and the second valve, such that by filling the liquid feedstock storage section with liquid feedstock by opening the second valve while the first valve is closed, and then closing the second valve and opening the first valve to discharge the liquid feedstock filled in the liquid feedstock storage section into the vaporization container, a filling and discharging process is provided to supply liquid feedstock to the vaporization container.

Description

Technical Field

[0001] This disclosure relates to a substrate processing apparatus, a liquid material replenishment system, a method for manufacturing a semiconductor device, a substrate processing method, and a recording medium. Background Technology

[0002] Patent Document 1 discloses a liquid feedstock replenishment system for replenishing liquid feedstock to the vaporization container of a substrate processing apparatus.

[0003] Existing technical documents

[0004] Patent documents

[0005] Patent Document 1: WO2018 / 056346 Summary of the Invention

[0006] The problem that the invention aims to solve

[0007] However, when replenishing the vaporization container with liquid feedstock pressurized from the supply system, it is sometimes difficult to accurately control the amount of liquid feedstock supplied to the vaporization container.

[0008] The subject of this disclosure is to control the supply amount in a way that accurately supplies a specified amount of liquid raw material into the vaporization container when replenishing the liquid raw material into the vaporization container.

[0009] Methods for solving problems

[0010] According to this disclosure, a technology is provided comprising: a vaporization container for vaporizing a liquid raw material inside; a liquid raw material replenishment line, one end of which is connected to the vaporization container and the other end of which is connected to a supply source of the liquid raw material; a first valve disposed on the liquid raw material replenishment line; a second valve disposed on the liquid raw material replenishment line upstream of the first valve; a liquid raw material storage section formed between the first valve and the second valve; and a control section for controlling the opening and closing of the first valve and the second valve, such that after filling the liquid raw material storage section with the liquid raw material by opening the second valve while the first valve is closed, closing the second valve and opening the first valve, thereby discharging the liquid raw material filled in the liquid raw material storage section into the vaporization container through a filling discharge process, thereby supplying the liquid raw material into the vaporization container.

[0011] Invention Effects

[0012] According to this disclosure, when replenishing liquid raw materials into the vaporization container, the supply amount can be controlled in such a way that a specified amount of liquid raw materials is accurately supplied into the vaporization container. Attached Figure Description

[0013] Figure 1This is a structural diagram showing the storage tank and the like included in the substrate processing apparatus of the present disclosure.

[0014] Figure 2 This is a cross-sectional view showing the processing chamber and the like in the substrate processing apparatus of the present disclosure.

[0015] Figure 3 This is a schematic structural diagram illustrating a substrate processing apparatus according to an embodiment of the present disclosure.

[0016] Figure 4 This is a block diagram illustrating the controller included in the substrate processing apparatus according to embodiments of the present disclosure.

[0017] Figure 5 This is a diagram showing the film deposition sequence when performing film deposition on a wafer using the substrate processing apparatus according to embodiments of the present disclosure.

[0018] Figure 6 This is a flowchart of the liquid raw material replenishment process according to an embodiment of this disclosure.

[0019] Figure 7A It means in Figure 6 A diagram showing the filling state of the liquid feedstock before the opening valve 758 in S14 of the liquid feedstock replenishment process.

[0020] Figure 7B It means in Figure 6 A diagram showing the filling state of the liquid raw material after opening valve 758 in S14 and before opening valve 759 in S18 during the liquid raw material replenishment process.

[0021] Figure 7C It means in Figure 6 A diagram showing the filling state of the liquid raw material after opening valve 759 in S12 of the liquid raw material replenishment process.

[0022] Figure 8 This is a flowchart of liquid raw material replenishment processing in other embodiments of this disclosure.

[0023] Figure 9 This is a diagram showing a modified example of the liquid raw material storage section according to an embodiment of the present disclosure. Detailed Implementation

[0024] The inventors have conducted an in-depth study on the relationship between the amount of liquid raw material stored in the storage tank and the in-plane uniformity of the film formed on the substrate by the raw material gas generated by vaporizing the liquid raw material. As a result, the inventors found that the concentration of impurities contained in the vaporized raw material gas varies depending on the amount (balance) of liquid raw material stored in the storage tank. If the amount of liquid raw material stored in the storage tank decreases, the in-plane uniformity of the film formed on the substrate increases.

[0025] Therefore, the aim is to reduce the amount of liquid feedstock stored in the storage tank. However, this requires that the replenishment of liquid feedstock to the storage tank be carried out in small quantities and with high precision. Therefore, the use of a liquid mass flow controller to control the replenishment amount is also considered. However, in order to accurately control the replenishment amount using a liquid mass flow controller, the differential pressure between the replenishment source and the replenishment destination must be stable, which is difficult to apply to replenishing storage tanks where the internal pressure changes during replenishment.

[0026] The preferred embodiments of this disclosure will be described below.

[0027] (Overall structure) based on Figures 1-5 An example of a substrate processing apparatus, liquid raw material replenishment system, semiconductor device manufacturing method, and process according to embodiments of the present disclosure will be described. Furthermore, in the figures, arrow H indicates the vertical direction of the apparatus, arrow W indicates the width direction of the apparatus (horizontal direction), and arrow D indicates the depth direction of the apparatus (horizontal direction). Additionally, the figures used in the following description are schematic, and the dimensional relationships and ratios of the elements shown may not necessarily correspond to reality. Furthermore, the dimensional relationships and ratios of elements may not be consistent between different figures.

[0028] like Figure 3 As shown, it has a liquid raw material replenishment system 780 (refer to). Figure 1 The substrate processing apparatus 10 includes a processing furnace 202 for processing a wafer 200, which serves as a substrate. The processing furnace 202 has a cylindrical heater 207 extending in the vertical direction of the apparatus, which is supported on a heater base (not shown) that serves as a holding plate. The heater 207 heats the processing chamber 201, which will be described later, to a predetermined temperature.

[0029] And, as Figure 2 , Figure 3 As shown, a cylindrical processing tube 203, concentric with the heater 207, serves as a processing unit, located inside the heater 207. A processing chamber 201 for processing multiple wafers 200 is formed inside the processing tube 203. Specifically, multiple wafers (e.g., 25 to 200) are loaded vertically onto a wafer boat 217, which serves as a substrate support, and these wafers are disposed inside the processing chamber 201. A cylindrical heat insulation cylinder 218 is located at the lower part of the wafer boat 217. With this structure, heat from the heater 207 is difficult to transfer to the sealing cap 219, which will be described later.

[0030] In addition, such as Figure 3As shown, a cylindrical manifold (inlet flange) 209, concentric with the processing pipe 203, is disposed below the processing pipe 203. The upper end of the manifold 209 is opposite to the lower end of the processing pipe 203, and the manifold 209 supports the processing pipe 203 via an O-ring 220, which serves as a sealing member.

[0031] Furthermore, in the processing chamber 201, nozzles 410 and 420 extending in the vertical direction are arranged between the wall of the processing tube 203 and the plurality of wafers 200 loaded by the crystal boat 217. Moreover, in the nozzles 410 and 420, a plurality of gas supply holes 410a and 420a are formed in a region opposite to the wafers 200 in the horizontal direction. Thus, the gas ejected from the gas supply holes 410a and 420a flows toward the wafers 200.

[0032] Furthermore, the lower ends of nozzles 410 and 420 are bent, penetrating the sidewall of manifold 209, and the lower ends of nozzles 410 and 420 protrude outward from manifold 209. Gas supply pipes 310 and 320, serving as gas supply lines, are respectively connected to the lower ends of nozzles 410 and 420. Thus, various gases are supplied to processing chamber 201.

[0033] In gas supply pipes 310 and 320, mass flow controllers (MFCs) 312 and 322, serving as flow controllers (flow control units), and valves 314 and 324, serving as on / off valves, are sequentially installed from the upstream side of the gas flow direction (hereinafter referred to as the "gas flow direction") in gas supply pipes 310 and 320. Furthermore, in gas supply pipes 310 and 320, the portions downstream of valves 314 and 324 in the gas flow direction are respectively connected to the ends of gas supply pipes 510 and 520, which serve as gas supply lines for supplying inactive gases. In gas supply pipes 510 and 520, MFCs 512 and 522, serving as flow controllers (flow control units), and valves 514 and 524, serving as on / off valves, are sequentially installed from the upstream side of the gas flow direction in gas supply pipes 510 and 520.

[0034] The raw material gas, which is used as the processing gas, is supplied from the gas supply pipe 310 to the processing chamber 201 via the MFC 312, valve 314, and nozzle 410. Thus, the supply unit 308 that supplies the raw material gas to the processing chamber 201 is configured to include the gas supply pipe 310, MFC 312, valve 314, and nozzle 410.

[0035] The raw material gas supply system consists of gas supply pipe 310, MFC 312, and valve 314. Alternatively, nozzle 410 can be included in the raw material gas supply system. The raw material gas supply system can also be referred to as a raw material supply system.

[0036] In contrast, a reaction gas, which serves as a processing gas, is supplied from the gas supply pipe 320 to the processing chamber 201 via the MFC 322, valve 324, and nozzle 420.

[0037] When the reactant gas (reactant) is supplied from the gas supply pipe 320, the reactant gas supply system (reactant supply system) mainly consists of the gas supply pipe 320, MFC 322, and valve 324. It is also possible to include the nozzle 420 in the reactant gas supply system. When the reactant gas flows from the nozzle 420, the nozzle 420 can also be referred to as a reactant gas nozzle.

[0038] Furthermore, inactive gas is supplied to the processing chamber 201 from the gas supply pipes 510 and 520 via MFCs 512 and 522, valves 514 and 524, and nozzles 410 and 420.

[0039] The inactive gas supply system is mainly composed of gas supply pipes 510, 520, MFC 512, 522 and valves 514, 325.

[0040] On the other hand, one end of an exhaust pipe 231, which serves as an exhaust flow path for venting the atmosphere of the processing chamber 201, is connected to the wall of the manifold 209. A pressure sensor 245, which serves as a pressure detector (pressure detection unit) for detecting the pressure of the processing chamber 201, and an APC (Auto Pressure Controller) valve 243, which serves as an exhaust valve (pressure adjustment unit), are installed on the exhaust pipe 231. A vacuum pump 246, which serves as a vacuum exhaust device, is installed at the end of the exhaust pipe 231.

[0041] The APC valve 243 is configured such that by opening and closing the valve while the vacuum pump 246 is operating, vacuum exhaust from the processing chamber 201 can be performed and stopped. Furthermore, by adjusting the valve opening based on pressure information detected by the pressure sensor 245 while the vacuum pump 246 is operating, the pressure in the processing chamber 201 can be adjusted. The exhaust system mainly consists of the exhaust pipe 231, the APC valve 243, and the pressure sensor 245. It is also possible to include the vacuum pump 246 in the exhaust system.

[0042] A sealing cover 219, serving as a furnace opening cover, is provided below the manifold 209 to airtightly seal the lower opening of the manifold 209. The sealing cover 219 is configured to abut against the lower end of the manifold 209 from the lower side in the vertical direction. An O-ring 220, serving as a sealing member, is provided on the upper surface of the sealing cover 219 and abuts against the lower end of the manifold 209. On the opposite side of the processing chamber 201 relative to the sealing cover 219, a rotation mechanism 267 is provided to rotate the wafer boat 217 (described later). The rotation shaft 255 of the rotation mechanism 267 passes through the sealing cover 219 and is connected to the wafer boat 217. The rotation mechanism 267 is configured to rotate the wafer 200 by rotating the wafer boat 217.

[0043] The sealing cap 219 is configured to move vertically upwards and downwards via a boat lift 115, which is vertically mounted outside the processing tube 203. The boat lift 115 is configured to move the boat 217 in and out of the processing chamber 201 by raising and lowering the sealing cap 219. The boat lift 115 is a conveying device (conveyor) for moving the boat 217, i.e., the wafer 200, in and out of the processing chamber 201. Additionally, a shutter 219s, serving as a furnace opening cover, is provided below the manifold 209, capable of airtightly sealing the lower opening of the manifold 209 during the descent of the sealing cap 219 using the boat lift 115. An O-ring 220c, serving as a sealing member, is provided on the upper surface of the shutter 219s, abutting against the lower end of the manifold 209. The opening and closing actions (lifting, rotating, etc.) of the gate 219s are controlled by the gate opening and closing mechanism 115s.

[0044] In addition, such as Figure 2 As shown, a temperature sensor 263, serving as a temperature detector, is installed in the processing chamber 201. The energizing of the heater 207 is adjusted based on the temperature information detected by the temperature sensor 263, thereby achieving the desired temperature distribution in the processing chamber 201. The temperature sensor 263, like the nozzles 410 and 420, is installed along the inner wall of the processing tube 203.

[0045] Next, the control unit 121, which is a control unit, of the substrate processing apparatus 10 will be described. For example... Figure 4 As shown, the control unit 121 is configured as a computer having a CPU (Central Processing Unit) 121a, RAM (Random Access Memory) 121b, a storage device 121c, and an I / O port 121d. The RAM 121b, storage device 121c, and I / O port 121d are configured to exchange data with the CPU 121a via an internal bus 121e. The control unit 121 is connected to an input / output device 122, such as a touch panel.

[0046] The storage device 121c is composed of, for example, flash memory, HDD (Hard Disk Drive), etc. The storage device 121c stores control programs for controlling the operation of the board processing device, various programs such as the liquid material replenishment program (described later), and data for executing each program in a readable manner.

[0047] RAM121b is configured as a storage area (working area) to temporarily hold programs, data, etc. read by CPU121a.

[0048] I / O port 121d is connected to the MFC512, 522, 312, 322, valves 514, 524, 314, 324, pressure sensor 245, APC valve 243, vacuum pump 246, temperature sensor 263, heater 207, rotating mechanism 267, crystal boat elevator 115, gate opening and closing mechanism 115s, ultrasonic sensor 650, MFC706, valves 758, 759, etc. (described later).

[0049] CPU 121a is configured to read and execute control programs from storage device 121c, and to read data from storage device 121c based on inputs such as operation commands from input / output device 122.

[0050] CPU 121a is configured to control, based on the read data, various gas flow adjustment actions performed by MFCs 512, 522, 312, and 322; opening and closing actions of valves 514, 524, 314, and 324; opening and closing actions of APC valve 243 and pressure adjustment actions of APC valve 243 based on pressure sensor 245; starting and stopping vacuum pump 246; temperature adjustment actions of heater 207 based on temperature sensor 263; rotation and rotation speed adjustment actions of crystal boat 217 based on rotation mechanism 267; lifting and lowering actions of crystal boat 217 performed by crystal boat elevator 115; and opening and closing actions of gate 219s performed by gate opening and closing mechanism 115s. Furthermore, CPU 121a is configured to control the opening and closing of valve 758 (as a second valve) and valve 759 (as a first valve) according to the execution of a liquid raw material replenishment procedure (liquid raw material replenishment processing). In addition, the control unit 121 can be configured as a control unit that controls the opening and closing of valves 758 and 759 of the liquid raw material replenishment system. Alternatively, other control units that can be configured to control ultrasonic sensor 650, MFC706, valves 758 and 759 can be provided separately from the control unit 121.

[0051] The control unit 121 can be configured by installing a program stored in an external storage device (e.g., magnetic tape, floppy disk, hard disk, CD, DVD, MO, USB memory, memory card, etc.) 123 into a computer.

[0052] Storage device 121c and external storage device 123 constitute a computer-readable recording medium. Hereinafter, they will also be referred to simply as recording medium. When the term "recording medium" is used in this specification, sometimes only storage device 121c is included, sometimes only external storage device 123 is included, or sometimes both are included. Furthermore, the provision of a program to a computer may also be performed without using external storage device 123, but rather using communication means such as the Internet or a dedicated line.

[0053] Furthermore, the control of the ultrasonic sensor 650, MFC706, valves 758 and 759 by the control unit 121 will be explained together with their functions described later.

[0054] (Main structural components)

[0055] [Storage Tank] Next, the storage tank 610 for storing liquid raw materials that have been vaporized into raw material gas will be described. The liquid raw materials are vaporized in the storage tank 610, which serves as a vaporization container.

[0056] Storage tank 610 may be formed, for example, in a rectangular or cylindrical shape. Furthermore, as... Figure 1 As shown, the storage space 612 formed inside the storage tank 610 is formed by a bottom 620, a wall 630 rising from the periphery of the bottom 620, and a top 640 that seals off the storage space 612 surrounded by the wall 630 from the top, forming a sealed space from the outside. Furthermore, this storage space 612 is set to a predetermined pressure. The lower end portion of the gas supply pipe 310 is provided through and disposed within the storage space 612.

[0057] The bottom 620 has an upward-facing bottom surface 622, and a recess 624 is formed on the central side of the bottom surface 622 in both the width and depth directions of the device. The recess 624 extends in the vertical direction and has a rectangular cross-section.

[0058] Furthermore, in this embodiment, the lower limit setting for the liquid raw material is set high (large) relative to the lower limit value that the liquid raw material can be stored in the storage space 612 (see illustration). Additionally, in this embodiment, the upper limit setting for the liquid raw material is set low (small) relative to the upper limit value that the liquid raw material can be stored in the storage space 612 (see illustration).

[0059] An ultrasonic sensor 650, serving as a liquid level sensor, is disposed in the storage space 612 and extends vertically, with its upper end mounted on the top 640. The cross-sectional shape of the ultrasonic sensor 650 is rectangular, smaller than the cross-sectional shape of the recess 624. Furthermore, the lower portion of the ultrasonic sensor 650 is disposed in the recess 624, and a sensor element 652 is mounted at the lower end of the ultrasonic sensor 650.

[0060] In this structure, the ultrasonic waves generated by the sensor element 652 are reflected by the surface of the liquid raw material. The wave-receiving part (not shown) of the ultrasonic sensor 650 receives the reflected waves, thereby continuously detecting the liquid level of the liquid raw material stored in the storage tank 610. In this way, the ultrasonic sensor 650 functions as a continuous sensor (also known as a continuous sensor, continuous level sensor, or continuous liquid level sensor).

[0061] [Gasification Section] The gasification section 700 is a device that vaporizes liquid raw materials stored in storage tank 610 into raw material gas by bubbling, and has a gas supply pipe 704 for supplying carrier gas and a mass flow controller (MFC) 706.

[0062] A gas supply pipe 704 extends through the top 640, and one end of the gas supply pipe 704 is disposed within the liquid raw material stored in the storage tank 610. In addition, an MFC 706 is disposed in the portion of the gas supply pipe 704 that is disposed outside the storage tank 610.

[0063] In this structure, a carrier gas with its flow rate adjusted using an MFC706 is supplied from one end of a gas supply pipe 704 to the liquid raw material stored in a storage tank 610. The carrier gas acts on the liquid raw material, causing it to vaporize. The vaporized raw material gas is then pressurized through the pressure P0 within the storage tank 610 and pumped into the gas supply pipe 310.

[0064] Furthermore, in the bubbling method, the supply amount of carrier gas to the storage tank 610 (bubbler) can be controlled, but the actual vaporization amount cannot be determined. Therefore, in this embodiment, the ultrasonic sensor 650 is used to detect the decrease in liquid raw material, thereby determining the vaporization amount.

[0065] [Supply Unit] The supply unit 750, as a liquid raw material supply system, is a device that replenishes the liquid raw material pressurized from the supply tank 760 to the storage tank 610. It includes a liquid supply pipe 754 as a liquid raw material supply pipeline for supplying liquid raw material flow, an on / off valve 759 as a first valve, and an on / off valve 758 as a second valve. Alternatively, the supply tank 760, which serves as the liquid raw material supply source, may also be included in the supply unit 750.

[0066] A liquid supply pipe 754 extends through the top 640, and a nozzle 754N, serving as a liquid raw material supply nozzle, is formed at one end. The nozzle 754N is disposed in the storage space 612, and the nozzle outlet 754A is positioned above the liquid level of the liquid raw material stored in the storage tank 610 (the upper limit of storage, see reference). Figure 1 The nozzle 754A is positioned slightly above the liquid surface of the raw material. This allows the liquid material to be discharged from the liquid supply pipe 754 into the storage space 612. In other words, during the filling and discharging process described later, by opening the valve 759, the liquid material can be discharged from the liquid material storage section 756 into the storage space 612 using the pressure difference between the liquid material storage section 756 and the storage space 612.

[0067] A downstream end 755 is formed in the continuous portion of the liquid supply pipe 754 from the nozzle 754N, arranged vertically in the axial direction. Valves 758 and 759 are provided at the downstream end 75. Valves 758 and 759 are located in the portion of the liquid supply pipe 754 that is disposed outside the storage tank 610. Valves 758 and 759 are located vertically above the storage tank 610. Furthermore, valve 758 is provided separately from valve 759 at a position upstream (upper) of valve 759, and a liquid raw material storage section 756 is formed in the portion of the liquid supply pipe 754 between valves 758 and 759, serving as a space for storing liquid raw materials. The liquid raw material storage section 756 is located vertically above the storage tank 610.

[0068] Furthermore, in this embodiment, the downstream end 755 is arranged vertically, but the downstream end 755 may also be arranged at an angle with the nozzle 754N side facing downwards. Additionally, both valves 758 and 759 are provided at the downstream end 55, but valve 758 may also be provided upstream of the downstream end 755. As in this embodiment, by arranging valves 758 and 759 vertically, the liquid material stored between valves 758 and 759 can be effectively discharged using gravity.

[0069] The replenishment tank 760 is disposed outside the storage tank 610 and connected to the other end of the liquid supply pipe 754. A pressure delivery pipe 761 is connected to the upper part of the replenishment tank 760. Pressure delivery gas is supplied to the replenishment tank 760 from the pressure delivery pipe 761, and the liquid raw material stored in the replenishment tank 760 is pressured into the liquid supply pipe 754 by the pressure delivery pressure P1 in the replenishment tank 760.

[0070] Furthermore, the pressure P1 in the replenishment tank 760 is greater than the pressure P0 in the storage tank 610, preferably more than 10 times the pressure P0. By setting it to more than 10 times, a sufficient amount of liquid material can be filled into the liquid storage section 756. If it is less than 10 times, due to the atmosphere at pressure P0 present in the liquid storage section 756 before filling it with liquid material, it may be impossible to fill the liquid storage section 756 with a sufficient amount of liquid material. In addition, a larger pressure difference is preferred in order to fill the liquid storage section 756 with as much liquid material as possible, but the valves on the piping and the pressure resistance limit of the piping also need to be considered.

[0071] For example, the pressure P0 inside the storage tank 601 is 100 to 10000 Pa, and the pressure P1 from the replenishment tank 760 is 0.1 to 10 MPa, etc.

[0072] When replenishing liquid material from replenishment tank 760 to storage tank 610 via liquid supply pipe 754, valve 758 is opened while valve 759 is closed, thereby filling liquid material into liquid storage section 756. Afterwards, valve 758 is closed and valve 759 is opened, thereby discharging liquid material from liquid storage section 756 into storage tank 610. In other words, replenishment (filling and discharging process) is performed by temporarily storing liquid material in liquid storage section 756 and discharging the stored liquid material into storage tank 610. Furthermore, valves 758 and 759 are closed when no liquid material is being replenished.

[0073] If we define the capacity of the liquid raw material storage section 756 as capacity X0, the amount of liquid raw material filling the liquid raw material storage section 756 as fillable amount X1, and the amount of liquid raw material discharged from the liquid raw material storage section 756 through the open valve 759 as discharge amount X2, then the relationship becomes X0 ≥ X1 ≥ X2. In the storage tank 610, the liquid raw material is vaporized. When the valve 759 is opened, gas enters the liquid raw material storage section 756. When the valve 759 is closed and the valve 758 is opened in this state, the gas is forced into the liquid raw material storage section 756 while being compressed by the liquid raw material supplied from the liquid supply pipe 754. Therefore, when gas enters the liquid raw material storage section 756, X0 > X1. Furthermore, if the entire amount of liquid raw material filling the liquid raw material storage section 756 is not discharged, X1 > X2. Furthermore, by reducing the pressure inside the storage tank 610, the amount of gas entering the liquid raw material storage section 756 when the valve 759 is opened can be minimized. Here, the pressure reduction state refers to a pressure lower than atmospheric pressure, preferably pressure P0.

[0074] For example, the capacity X0 is 20cc or less, preferably 10cc or less. From the viewpoint of improving supply control, it is preferable to have the smallest possible volume, but from the viewpoint of shortening the replenishment processing time (increasing productivity), it is preferable that the capacity X0 is, for example, 1cc or more.

[0075] X2 is preferably less than or equal to the amount of liquid raw material (processing consumption C) required for the film-forming process described later, which is performed a predetermined number of times (1 batch), and more preferably less than 1 / 2 of the processing consumption C. That is, it is preferable to supply liquid raw material from the liquid raw material storage unit 756 multiple times to an amount equal to or greater than the processing consumption C.

[0076] Furthermore, the fillable amount X1 and discharge amount X2 can be preset in the device by performing actions in advance to measure the fill / discharge amount, store the average value, etc.

[0077] (Function) Next, a method for manufacturing a semiconductor device using the substrate processing apparatus 10 will be described. Furthermore, the operation of each component constituting the substrate processing apparatus 10 is controlled by the control unit 121.

[0078] First, use Figure 5 An example of the sequence for forming a film on a wafer 200 using the substrate processing apparatus 10 will be described. In this embodiment, the processing chamber 201, which houses multiple wafers 200, is heated to a predetermined temperature. Furthermore, the following processes are performed in the processing chamber 201 a predetermined number of times (n times): a raw material gas supply process in which a raw material gas containing a predetermined element is supplied from the supply orifice 410a of the nozzle 410, and a reaction gas supply process in which a reaction gas is supplied from the supply orifice 420a of the nozzle 420. As a result, a film containing the predetermined element is formed on the wafer 200. The predetermined number of times (n times) is one batch process in the film formation process and is preset. In this embodiment, this predetermined number of times is referred to as the "set number N".

[0079] The manufacturing method of semiconductor devices will be described in detail below.

[0080] [Loading / Placing] First, multiple wafers 200 are loaded (wafer charge) onto the wafer carrier 217. The gate 219s is moved by the gate opening / closing mechanism 115s, opening the lower end opening of the manifold 209 (gate opening). And, as... Figure 3 As shown, a crystal boat 217 loaded with multiple wafers 200 is lifted by a crystal boat elevator 115 and moved (crystal boat loading) into the processing chamber 201. In this state, the sealing cap 219 seals the lower end of the manifold 209 via an O-ring 220b.

[0081] [Pressure / Temperature Adjustment] Next, vacuum degassing is performed using vacuum pump 246 to bring the processing chamber 201 to the desired pressure (vacuum level). At this time, the pressure in the processing chamber 201 is measured by pressure sensor 245, and based on this measured pressure information, feedback control (pressure adjustment) is applied to APC valve 243. Vacuum pump 246 remains continuously operational at least until the processing of wafer 200 is complete.

[0082] Additionally, the processing chamber 201 is heated by heater 207 to bring it to the desired temperature. Heating of the processing chamber 201 by heater 207 continues at least until the processing of the wafer 200 is completed.

[0083] Furthermore, the crystal boat 217 and the wafer 200 are rotated by the rotation mechanism 267. The rotation of the crystal boat 217 and the wafer 200 based on the rotation mechanism 267 continues at least until the processing of the wafer 200 is completed.

[0084] [Adjustment of liquid raw material quantity (an example of a storage process)] Next, with Figure 1 The liquid raw material stored in the storage tank 610 is shown to be at an initial liquid level L0, which is a predetermined filling level, and the liquid raw material is stored in the storage tank 610. Here, in this embodiment, the initial liquid level L0 refers to the liquid level when the minimum amount of liquid raw material required for the ultrasonic sensor 650 to detect the liquid level and the total amount of liquid raw material required for the film-forming process described later (set number N) are stored in the storage tank 610.

[0085] The minimum amount of liquid material required for the ultrasonic sensor 650 to detect the liquid level refers to the amount when the liquid level is at the lower limit of the storage tank 610.

[0086] Furthermore, the amount of liquid raw material required for the predetermined number of film-forming processes (set number N) refers to the amount required to form a film on wafer 200 by sequentially performing the raw material gas supply process, residual gas removal process, reaction gas supply process, and residual gas removal process (described later) a predetermined number of times (more than once). This amount of liquid raw material is referred to as "processing consumption C".

[0087] Furthermore, in this embodiment, the amount of liquid raw material required for the film-forming process of a predetermined number of times (set number N) is detected by an ultrasonic sensor 650 based on the actual amount of liquid consumed. However, it can also be preset to a predetermined supply amount C1 based on the average amount used in the same batch of processing. In this case, the capacity X0 of the liquid raw material storage unit 756 is preferably equal to or less than the predetermined supply amount C1, and the fillable amount X1 of the liquid raw material storage unit 756 and the discharge amount X2 discharged from the liquid raw material storage unit 756 are preferably equal to or less than the predetermined supply amount C1.

[0088] The following section provides a detailed explanation of how to supplement and adjust the amount of liquid raw materials.

[0089] Control unit 121 via Figure 6 The liquid feedstock replenishment process shown involves adding liquid feedstock to storage tank 610. First, in step S10, the liquid feedstock level L is detected by ultrasonic sensor 650. In step S12, it is determined whether the liquid feedstock level has reached the initial level L0. If the liquid feedstock level has reached the initial level L0, the process ends.

[0090] If the liquid level of the raw material has not reached the initial level L0, in step S14, valve 758 is opened. Before valve 758 is opened, as follows: Figure 7A As shown, the liquid feedstock is filled to a position upstream of valve 758 in the liquid supply pipe 754. At this time, valve 759 is closed. Figure 7B As shown, by opening valve 758, liquid raw material is filled into liquid storage section 756 using the pressure from replenishment tank 760 (filling process). In step S16, the process waits until the liquid raw material is filled into liquid storage section 756, and after filling, it proceeds to step S18. Whether the filling of liquid raw material is complete can be determined by the elapsed time from the opening of valve 758.

[0091] In step S18, valve 758 is closed, and in step S20, valve 759 is opened. During this time, between steps S18 and S20, both valves 758 and 759 remain closed for a predetermined time. By setting the timing for maintaining the two valves closed for this predetermined time, even if there is a discrepancy in the opening and closing timing between the two valves, it is possible to prevent both valves from becoming open. When both valves are in the open state, the connection between the replenishment tank 760 and the storage tank 610 is established. In this case, a large amount of raw material flows into the storage tank 610, making it difficult to control the amount of liquid raw material supplied to the storage tank 610. As described above, it is preferable to control the opening and closing timing of both valves in a manner that both are closed before one of valves 758 and 759 is opened.

[0092] By opening valve 759, such as Figure 7C As shown, liquid raw material is discharged from the liquid storage section 756 and supplied to the storage tank 610 through the opening of the nozzle 754N (discharge process). The amount of liquid raw material supplied to the storage tank 610 through this operation is called the discharge amount X2. In step S22, the system waits until the liquid raw material is discharged from the liquid storage section 756. After discharge, the process proceeds to step S24. Whether the discharge of the liquid raw material is complete can be determined by the elapsed time from the opening of the valve 759. In step S24, the valve 758 is closed, and the process returns to step S10, repeating the filling and discharge process. The filling and discharge process is repeated until the liquid level L of the liquid raw material detected by the ultrasonic sensor 650 reaches the initial liquid level L0.

[0093] Furthermore, between steps S24 and S14, and similarly between steps S18 and S20, both valves 758 and 759 remain closed.

[0094] [Film Formation Process (An Example of Substrate Processing)]

[0095] [Gasification Process] The liquid raw materials stored in storage tank 610 are vaporized into raw material gas.

[0096] Specifically, the amount of raw material gas required for the raw material gas supply process (described later) is pre-stored in the control unit 121. The control unit 121 controls the MFC 706 of the vaporization unit 700 to supply an inactive gas as a carrier gas to the liquid raw material stored in the storage tank 610. As a result, the liquid raw material is vaporized into raw material gas.

[0097] As inert gases, rare gases such as nitrogen (N2), argon (Ar), helium (He), neon (Ne), and xenon (Xe) can be used. More than one of these gases can be used as an inert gas. This also applies to the steps described later.

[0098] [Raw material gas supply process (an example of a processing process)] Next, open... Figure 3 The valve 314 shown allows the raw material gas to flow into the gas supply pipe 310. One or more types of gases obtained by vaporizing a liquid raw material in a vaporization container can be used as the raw material gas.

[0099] For example, as a raw material gas, a gas containing specified elements such as silicon (Si) as a semiconductor element and titanium (Ti), zirconium (Zr), hafnium (Hf), tantalum (Ta), aluminum (Al), molybdenum (Mo), and tungsten (W) as metallic elements can be used; that is, a gas that is in a liquid state at room temperature and pressure (i.e., a gas as a liquid raw material). By vaporizing these liquid raw materials in a vaporization container, a raw material gas can be obtained.

[0100] For example, various Si-containing raw materials such as tetrabutyldimethylaminosilane (Si[N(CH3)2]4, abbreviated as 4DMAS) gas, tributyldimethylaminosilane (Si[N(CH3)2]3H, abbreviated as 3DMAS) gas, bis(diethylaminosilane) (Si[N(C2H5)2]2H2, abbreviated as BDEAS), and bis(tert-butylaminosilane) (SiH2[NH(C4H9)]2, abbreviated as BTBAS) gas can be used. The following gases are used as raw materials: aminosilane, silicon monochloride (SiH3Cl, MCS), dichlorosilane (SiH2Cl2, DCS), trichlorosilane (SiHCl3, TCS), tetrachlorosilane (SiCl4, STC), hexachlorosilane (Si2Cl6, HCDS), octachlorotrisilane (Si3Cl8, OCTS), and 1,2-bis(trichlorosilyl)ethane. ((SiCl3)2C2H4, abbreviated as BTCSE) gas, bis(trichlorosilyl)methane ((SiCl3)2CH2, abbreviated as BTCSM) gas, 1,1,2,2-tetrachloro-1,2-dimethylsilane ((CH3)2Si2Cl4, abbreviated as TCDMDS) gas, 1,2-dichloro-1,1,2,2-tetramethylsilane ((CH3)4Si2Cl2, abbreviated as DCTMDS) gas, 1 - Monochloro-1,1,2,2,2-pentamethyldisilane ((CH3)5Si2Cl, abbreviated as MCPMDS) gas, trifluorosilane (SiHF3, abbreviated as TFS) gas, tetrafluorosilane (SiF4, abbreviated as STF) gas, tribromosilane (SiHBr3, abbreviated as TBS) gas, tetrabromosilane (SiBr4, abbreviated as STB) gas and other halosilane feedstock gases, trisilane (Si3H8) gas, tetrasilane (Si4H 10 ) gas, pentasilane (Si5H) 12 ) gas, hexasilane (Si6H) 14 Inorganic silane raw material gases such as 1,4-disilbutane (Si2C2H) 10 Organosilanes and other gaseous raw materials, as well as liquid raw materials.

[0101] In addition, liquid feedstocks such as tetra(dimethylamino)titanium (Ti[N(CH3)2]4, abbreviated as TDMAT) gas and titanium tetrachloride (TiCl4) gas as Ti-containing feedstocks, tetra(ethylmethylamino)hafnium (Hf[N(C2H5)(CH3)]4, abbreviated as TEMAH) gas and hafnium tetrachloride (HfCl4) gas as Hf-containing feedstocks, tetra(ethylmethylamino)zirconium (Zr[N(C2H5)(CH3)]4, abbreviated as TEMAZ) gas as Zr-containing feedstocks, trimethylaluminum (Al(CH3)3, abbreviated as TMA) gas as Al-containing feedstocks, and tetraethoxytantalum (Ta(OC2H5)5), triethylmethylaminotert-butyliminotantalum (Ta[NC(CH3)3][N(C2H5)CH3]3), pentaethoxytantalum (Ta(OC2H5)5) gas as Ta-containing feedstocks can be used.

[0102] In particular, compared to impurities contained in liquid feedstocks, using liquid feedstocks with low vapor pressure makes it easier to achieve the impurity reduction effect based on the technology of this disclosure, and is therefore more preferable.

[0103] The feed gas is regulated by MFC312 and supplied to the processing chamber 201 from the supply port 410a of nozzle 410. Simultaneously, valve 514 is opened, allowing carrier gas to flow within gas supply pipe 510. The carrier gas, regulated by MFC512, is supplied to the processing chamber 201 along with the feed gas from the supply port 410a of nozzle 410 and exhausted from exhaust pipe 231.

[0104] Furthermore, to prevent the raw material gas from entering the nozzle 420 (to prevent backflow), valve 524 is opened to allow the carrier gas to flow into the gas supply pipe 520. The carrier gas is supplied to the processing chamber 201 via the gas supply pipe 520 and the nozzle 420, and is exhausted from the exhaust pipe 231.

[0105] At this time, adjust the APC valve 243 appropriately to bring the pressure in the processing chamber 201 to, for example, a pressure within the range of 1 to 1000 Pa. Furthermore, in this specification, the range of values, for example, 1 to 1000 Pa, refers to a pressure of 1 Pa or more and 1000 Pa or less. That is, the range of values ​​includes 1 Pa and 1000 Pa. The same applies to other numerical ranges described in this specification.

[0106] The supply flow rate of the raw material gas controlled by MFC312 is, for example, 10 to 2000 sccm, preferably 50 to 1000 sccm, and more preferably in the range of 100 to 500 sccm.

[0107] The time for supplying raw material gas to wafer 200 is, for example, within the range of 1 to 60 seconds.

[0108] Heater 207 heats the wafer 200 to a temperature range of, for example, 400 to 600°C.

[0109] When a raw material gas is supplied to the processing chamber 201 under the aforementioned conditions, a layer containing a specified element contained in the raw material gas is formed on the outermost surface of the wafer 200.

[0110] [Residual Gas Removal Process (Example of a Processing Step)] After the containing layer of the specified element is formed, valve 314 is closed to stop the supply of raw material gas. At this time, APC valve 243 remains open, and vacuum pump 246 is used to vent the processing chamber 201 under vacuum, removing any unreacted raw material gas remaining in the processing chamber 201 or that contributes to the formation of the containing layer of the specified element. Valves 514 and 524 maintain the supply of carrier gas to the processing chamber 201 while remaining open. The carrier gas acts as a purge gas, which improves the effectiveness of removing any unreacted raw material gas remaining in the processing chamber 201 or that contributes to the formation of the containing layer of the specified element.

[0111] [Reaction Gas Supply Process (Example of a Processing Process)] After removing residual gas from processing chamber 201, valve 324 is opened to allow reaction gas to flow within gas supply pipe 320. As the reaction gas, for example, an oxygen-containing gas (oxidizing gas, oxidant) containing oxygen (O) is used as the reaction gas (reactant) to react with a specified element contained in the raw material gas. Examples of oxygen-containing gases that can be used include oxygen (O2) gas, ozone (O3) gas, plasma-excited O2 gas (O2*), O2 gas + hydrogen (H2) gas, water vapor (H2O gas), hydrogen peroxide (H2O2) gas, nitrous oxide (N2O) gas, nitric oxide (NO) gas, nitrogen dioxide (NO2) gas, carbon monoxide (CO) gas, carbon dioxide (CO2) gas, etc. One or more of these can be used as the reaction gas.

[0112] The reaction gas is flow-regulated by MFC322 and supplied to the wafer 200 in the processing chamber 201 through the supply port 420a of nozzle 420, and exhausted through exhaust pipe 231. That is, the wafer 200 is exposed to the reaction gas.

[0113] At this time, valve 524 is opened, allowing the carrier gas to flow within the gas supply pipe 520. The carrier gas, with its flow rate adjusted by MFC 522, is supplied to the processing chamber 201 along with the reactant gas and exhausted from the exhaust pipe 231. To prevent the reactant gas from entering the nozzle 410 (preventing backflow), valve 514 is opened, allowing the carrier gas to flow into the gas supply pipe 510. The carrier gas is supplied to the processing chamber 201 via the gas supply pipe 510 and nozzle 410 and exhausted from the exhaust pipe 231.

[0114] At this time, the APC valve 243 is adjusted appropriately to bring the pressure in the processing chamber 201 to, for example, a range of 1 to 1000 Pa. The supply flow rate of the reaction gas, controlled by the MFC 322, is, for example, 5 to 40 slm, preferably 5 to 30 slm, and more preferably 10 to 20 slm. The time for supplying the reaction gas to the wafer 200 is, for example, a range of 1 to 60 seconds. Other processing conditions are the same as those described in the raw material gas supply process.

[0115] At this time, the gas flowing in the processing chamber 201 is only a reactive gas and an inactive gas. When oxygen-containing gas is supplied to the processing chamber 201 as a reactive gas under the aforementioned conditions, the reactive gas reacts with at least a portion of the element-containing layer formed on the wafer 200 during the raw material gas supply process, oxidizing the element-containing layer to form an oxide layer containing the element and O. That is, the element-containing layer is modified into an oxide layer containing the element.

[0116] [Residual Gas Removal Process (Example of a Processing Process)] After the oxide layer is formed, valve 324 is closed to stop the supply of reaction gas. Furthermore, through the same processing steps as the residual gas removal process after the raw material gas supply process, unreacted or reaction gases and reaction byproducts remaining in the processing chamber 201 that contribute to the formation of the oxide layer are removed from the processing chamber 201.

[0117] The gasification process, raw material gas supply process, residual gas removal process, reaction gas supply process, and residual gas removal process described above are performed in a cycle, repeated more than once, according to a predetermined number of times. In this way, by performing batch processing (multiple processes are performed multiple times), an oxide film obtained by stacking an oxide layer on wafer 200 is formed.

[0118] Furthermore, batch processing refers to a process in which a predetermined number of cycles are performed, including a gasification process, a raw material gas supply process, a residual gas removal process, a reaction gas supply process, and a residual gas removal process, to form a film of a specified thickness on wafer 200. Moreover, a film of a specified thickness is formed on wafer 200 in one batch.

[0119] The specified thickness is, for example, 10–150 nm, preferably 40–100 nm, and more preferably 60–80 nm.

[0120] [Supplementary Step] Thus, by batch processing the wafer 200, a film of a specified thickness is formed on the wafer 200. Furthermore, the liquid raw material stored in the storage tank 610 consumes the processing consumption C, therefore, the liquid raw material level in the storage tank 610 is lower than the initial liquid level L0.

[0121] Therefore, control unit 121 executes Figure 6 The liquid feedstock replenishment process shown involves replenishing the liquid feedstock by ensuring that its level L reaches the initial level L0 (replenishment step). This replenishment is performed in each batch of processing. Specifically, replenishment continues until the level L, which has decreased by the processing consumption C, reaches the initial level L0. Therefore, the fill-and-discharge process in the liquid feedstock replenishment is repeatedly executed until the amount of liquid feedstock supplied is equal to or exceeds the processing consumption C. However, if the liquid feedstock level L is higher than the initial level L0 before the start of batch processing, in subsequent replenishment steps, at the point in time where the fill-and-discharge process is executed until the amount of liquid feedstock supplied is one cycle less than the processing consumption C, the level L may sometimes reach the initial level L0.

[0122] [Exhaust / Pressure Adjustment] After forming a film of a specified thickness on wafer 200 and completing the residual gas removal process, open... Figure 3 Valves 514 and 524, as shown, supply carrier gas to the processing chamber 201 through gas supply pipes 310 and 320, respectively, and exhaust gas through exhaust pipe 231. The carrier gas acts as a purging gas, removing residual gases and byproducts from the processing chamber 201 (post-purging). Afterward, the atmosphere in the processing chamber 201 is replaced with the carrier gas, and the pressure inside the processing chamber 201 returns to normal atmospheric pressure.

[0123] After [moving out / removing], the sealing cover 219 is lowered by the crystal boat elevator 115, the lower end of the manifold 209 opens, and the processed wafer 200 is moved out from the lower end of the manifold 209 to the outside of the processing tube 203 while supported by the crystal boat 217 (crystal boat unloading).

[0124] After being removed, the gate 219s moves, and the lower opening of the manifold 209 is sealed by the gate 219s via the O-ring 220c (gate closed). After the processed wafer 200 is moved outside the processing tube 203, it is removed from the wafer boat 217 (wafer discharge).

[0125] As explained above, after the wafer 200 with a film of a specified thickness is removed after each processing (step), and when films are formed on other wafers 200, the processes of "loading / transferring," "pressure / temperature adjustment," "film formation treatment," "venting / pressure adjustment," and "removal / removal" are performed again, except for the aforementioned "adjustment of liquid raw material quantity." That is, the batch processing of wafers 200 is performed again.

[0126] Through the above-described film formation process, an oxide film containing specified elements contained in the raw material gas can be formed on the wafer 200. For example, the above-described raw material gas can be used to form oxide films such as titanium oxide (TiO film), zirconium oxide (ZrO film), hafnium oxide (HfO film), tantalum oxide (TaO film), aluminum oxide (AlO film), molybdenum oxide (MoO film), and tungsten oxide (WO film). Furthermore, for example, by using a nitrogen-containing gas (nitriding gas, nitriding agent) instead of an oxygen-containing gas as the reaction gas, nitride films such as titanium nitride (TiN film), zirconium nitride (ZrN film), hafnium nitride (HfN film), tantalum nitride (TaN film), aluminum nitride (AlN film), molybdenum nitride (MoN film), and tungsten nitride (WN film) can also be formed.

[0127] [Other] After that, known patterning, dicing, wire bonding, molding, and trimming processes are performed on the wafer 200 with the film formed to manufacture a semiconductor device.

[0128] (Summary) As explained above, by controlling the replenishment unit 750 as described above, the liquid raw material pressurized from the replenishment tank 760 is supplied to the storage tank 610, thereby enabling the supply amount to be controlled in such a way that a predetermined amount of liquid raw material is accurately supplied to the storage tank 610.

[0129] Specifically, in the above embodiment, by controlling the opening and closing of valves 758 and 759, liquid temporarily stored in the liquid storage section 756 is discharged into the storage tank 610, thereby replenishing the liquid raw material. In particular, when the amount of liquid raw material replenished is small, if the liquid raw material is supplied by only one valve opening and closing, the supply amount will deviate due to pressure fluctuations in the liquid supply pipe 754 and the accuracy of timing control of the opening and closing of the single valve. However, with the supply method of this embodiment, even a small amount of liquid raw material can be accurately supplied at a constant amount.

[0130] Furthermore, while an MFC (Mass Flow Controller) is considered for accurately supplying small amounts of liquid, fluctuations in pressure within the storage tank 610 and the delivery pressure from the replenishment tank 760 cause pressure variations within the liquid supply pipe 754, making accurate operation difficult. Additionally, this increases costs. In this embodiment, even with pressure variations within the liquid supply pipe 754, an accurate quantity of liquid feedstock can be supplied, which is also advantageous in terms of cost.

[0131] Furthermore, during each batch processing of wafer 200, liquid raw material is replenished to storage tank 610 using replenishment unit 750 (refilling per batch). This ensures that the amount of liquid raw material stored in storage tank 610 remains within a predetermined range. In other words, by replenishing the liquid raw material in a reduced amount, the amount of liquid raw material stored in storage tank 610 during the film deposition process on wafer 200 becomes constant (the liquid level becomes constant). Therefore, by suppressing deviations in the concentration of impurities contained in the raw material gas, deviations in the in-plane uniformity of the film formed on wafer 200 can be suppressed.

[0132] Furthermore, in the above embodiment, the initial liquid level L0 is set to the level at which the total amount of liquid raw material required for the ultrasonic sensor 650 to detect the liquid level, plus the amount of liquid raw material required for a predetermined number of film-forming processes (requiring the formation of an oxide film on the wafer 200), is stored in the storage tank 610. In other words, the liquid level is maintained at the lowest permissible position so that the absolute amount of impurities contained in the liquid raw material stored in the storage tank 610 is as low as possible. Moreover, even if the amount of liquid raw material used in a batch changes, the liquid raw material is replenished (refilled) in a reduced amount, and the replenished liquid level always remains a constant height. Therefore, compared to the case where the initial liquid level L0 is, for example, at the upper limit setting of the storage tank 610, the concentration of impurities contained in the raw material gas is reduced, thus improving in-plane uniformity.

[0133] Furthermore, while this disclosure has been described in detail with reference to specific embodiments, it is not limited to the embodiments described herein. It will be apparent to those skilled in the art that various other embodiments can be implemented within the scope of this disclosure. For example, in the above embodiments, liquid raw materials are vaporized into raw material gas by bubbling, but baking or direct vaporization methods can also be used to vaporize liquid raw materials into raw material gas.

[0134] Furthermore, in the above embodiment, the liquid material replenishment process is repeatedly performed until the liquid material level L detected by the ultrasonic sensor 650 reaches the initial liquid level L0. However, the liquid material replenishment process can also be performed without detecting the liquid level L. In this case, the amount of liquid material required for this batch processing is preset as the supply specified amount C1. Considering the amount of liquid material supplied by performing one cycle of liquid material replenishment process (discharge amount X2), the predetermined number of times the liquid material replenishment process needs to be repeated to supply the supply specified amount C1 is calculated in advance. Furthermore, according to... Figure 8 The process shown involves performing a liquid feedstock replenishment process. In this process, the required amount of liquid feedstock for batch processing is replenished by performing the replenishment process a predetermined number of times.

[0135] In this liquid material replenishment process, in step S14, valve 758 is opened. With valve 758 open, liquid material is filled into the liquid storage section 756. In step S16, the process remains idle until liquid material is filled into the liquid storage section 756. After filling, in step S18, valve 758 is closed, and in step S20, valve 759 is opened. With valve 759 open, liquid material is discharged from the liquid storage section 756 and supplied to the storage tank 610 through the opening of nozzle 754N. The amount of liquid material supplied to the storage tank 610 through this action is called the discharge amount X2. In step S22, the process remains idle until liquid material is discharged from the liquid storage section 756. After discharge, in step S24, valve 758 is closed. Then, in step S26, it is determined whether the process of steps S14 to S24 has been executed a predetermined number of times. If the determination in step S26 is negative, the process returns to step S14 and repeats; if the determination is positive, the process ends. In this way, by pre-setting the supply quantity C1, even if the liquid level sensor such as the ultrasonic sensor 650 malfunctions, the liquid raw material can be accurately replenished.

[0136] In addition, in this embodiment, a liquid raw material storage section 756 for storing liquid raw materials is formed through the liquid supply pipe 754 between valves 758 and 759. However, a liquid raw material storage section 756A with a larger capacity than the liquid supply pipe 754 can also be formed between valves 758 and 759 (see reference). Figure 9 The liquid raw material storage section 756A can be constructed, for example, by piping with a larger diameter than other parts, or it can be constructed by a buffer tank.

[0137] In addition, in the above embodiment, an example of vaporizing liquid raw material in storage tank 610 by bubbling was described, but a heater for heating the liquid raw material stored in storage tank 610 can also be provided to vaporize the liquid raw material by heating it.

[0138] Industrial availability

[0139] According to this disclosure, when replenishing liquid raw materials into the vaporization container, the supply amount can be controlled in such a way that a specified amount of liquid raw materials is accurately supplied into the vaporization container.

[0140] Symbol Explanation

[0141] 10. Substrate processing apparatus

[0142] 121 Control Department

[0143] 201 Processing Room

[0144] 310 Gas supply pipe

[0145] 610 Storage Tank (Vaporization Container)

[0146] 754N Nozzle (Liquid Feed Supply Nozzle)

[0147] 754A nozzle

[0148] 756 Liquid Raw Material Storage Department

[0149] 759 valve (first valve)

[0150] 758 valve (second valve)

[0151] 760 replenishment tank (canister).

Claims

1. A substrate processing apparatus, characterized in that, have: A vaporization container that vaporizes liquid feedstock inside; A liquid feedstock supply line is connected at one end to a nozzle formed inside the vaporization container and at the other end to a liquid feedstock supply source. The first valve is disposed in the liquid raw material replenishment pipeline, which is continuous with the nozzle and whose axial direction is vertical; The second valve is located upstream of and above the first valve on the liquid raw material supply line. A liquid raw material storage section is formed between the first valve and the second valve; and The control unit is configured to control the opening and closing of the first valve and the second valve, so that after filling the liquid raw material storage unit with the liquid raw material by opening the second valve while the first valve is closed, the second valve is closed and the first valve is opened to discharge the liquid raw material filled in the liquid raw material storage unit into the vaporization container, thereby supplying the liquid raw material into the vaporization container.

2. The substrate processing apparatus according to claim 1, characterized in that, The substrate processing apparatus includes: Processing chamber, which processes the substrate; and A processing gas supply piping connects the processing chamber to the vaporization container, and introduces the processing gas obtained by vaporizing the liquid raw material in the vaporization container into the processing chamber. The control unit is configured to control the first valve and the second valve so that the filling and discharging process is performed whenever the substrate is processed with the processing gas for a predetermined number of times in the processing chamber.

3. The substrate processing apparatus according to claim 2, characterized in that, The control unit is configured to control the first valve and the second valve to repeatedly perform the filling and discharging process until the amount of liquid raw material supplied to the vaporization container becomes the processing consumption amount consumed by performing the processing gas on the substrate a set number of times.

4. The substrate processing apparatus according to claim 2, characterized in that, The amount of liquid raw material discharged into the vaporization container in one filling and discharging process is less than or equal to the processing consumption amount consumed by performing the processing gas on the substrate a set number of times.

5. The substrate processing apparatus according to claim 2, characterized in that, The volume of the liquid raw material storage section is less than or equal to the processing consumption amount consumed by performing the processing gas on the substrate a set number of times.

6. The substrate processing apparatus according to claim 1, characterized in that, The volume of the liquid raw material storage section is greater than the amount of liquid raw material discharged into the vaporization container during one filling and discharging process.

7. The substrate processing apparatus according to any one of claims 1 to 6, characterized in that, The pressure at which the liquid feedstock is delivered from the supply source to the liquid feedstock replenishment pipeline is greater than the pressure inside the vaporization container.

8. The substrate processing apparatus according to claim 7, characterized in that, The delivery pressure is more than 10 times the pressure inside the vaporization container.

9. The substrate processing apparatus according to any one of claims 1 to 6, characterized in that, The substrate processing apparatus further includes a liquid level sensor for measuring the liquid level of the liquid raw material within the vaporization container. The control unit is configured to control the first valve and the second valve to perform the filling and discharging process a predetermined number of times until the liquid level of the liquid raw material, as measured by the liquid level sensor, reaches a preset filling level.

10. The substrate processing apparatus according to claim 9, characterized in that, The control unit is configured to control the first valve and the second valve so as to stop the filling and discharge process when the liquid level of the liquid raw material, as determined by the liquid level sensor, reaches the filling level.

11. The substrate processing apparatus according to any one of claims 1 to 6, characterized in that, The control unit is configured to control the first valve and the second valve to perform the filling and discharging process a predetermined number of times until the amount of liquid raw material supplied to the vaporization container reaches a predetermined supply amount.

12. The substrate processing apparatus according to claim 11, characterized in that, The volume of the liquid raw material storage section is less than the specified supply amount.

13. The substrate processing apparatus according to any one of claims 1 to 6, characterized in that, A liquid feed nozzle is provided inside the gasification container, with its upstream end connected to the liquid feed supply pipeline. The liquid feed nozzle is configured such that its outlet is located above the liquid surface of the liquid feed stored in the vaporization container.

14. The substrate processing apparatus according to any one of claims 1 to 6, characterized in that, The first valve and the second valve are positioned vertically above the vaporization container.

15. The substrate processing apparatus according to any one of claims 1 to 6, characterized in that, The control unit is configured to control the first valve and the second valve during the filling and discharging process, such that both valves are closed before one is opened.

16. The substrate processing apparatus according to any one of claims 1 to 6, characterized in that, The volume of the liquid raw material storage section is smaller than the volume of the gasification container.

17. A liquid feedstock replenishment system, characterized in that, have: A liquid feedstock supply line has one end connected to a nozzle formed inside a vaporization container that vaporizes the liquid feedstock, and the other end connected to a supply source of the liquid feedstock. The first valve is disposed in the liquid raw material replenishment pipeline, which is continuous with the nozzle and whose axial direction is vertical; The second valve is located upstream of and above the first valve on the liquid raw material supply line. A liquid raw material storage section is formed between the first valve and the second valve; and The control unit is configured to control the opening and closing of the first valve and the second valve, so that after filling the liquid raw material storage unit with the liquid raw material by opening the second valve while the first valve is closed, the second valve is closed and the first valve is opened to discharge the liquid raw material filled in the liquid raw material storage unit into the vaporization container, thereby supplying the liquid raw material into the vaporization container.

18. A method for manufacturing a semiconductor device, characterized in that, Liquid raw materials are supplied to the vaporization container through filling and discharging processes in a substrate processing apparatus. The substrate processing apparatus includes: The vaporization container vaporizes the liquid raw material inside; A liquid feedstock supply line is connected at one end to a nozzle formed inside the vaporization container and at the other end to a liquid feedstock supply source. The first valve is disposed in the liquid raw material replenishment pipeline, which is continuous with the nozzle and whose axial direction is vertical; The second valve is located upstream of and above the first valve on the liquid raw material supply line. as well as A liquid raw material storage section is formed between the first valve and the second valve. The filling process involves opening the second valve while the first valve is closed to fill the liquid raw material storage section with the liquid raw material. The discharge process, following the filling process, involves closing the second valve and opening the first valve to discharge the liquid raw material filling the liquid raw material storage section into the vaporization container.

19. A substrate processing method, characterized in that, Liquid raw material is supplied to the vaporization container through a filling and discharging process in a substrate processing apparatus. The substrate processing apparatus includes: The vaporization container vaporizes the liquid raw material inside; A liquid feedstock supply line is connected at one end to a nozzle formed inside the vaporization container and at the other end to a liquid feedstock supply source. The first valve is disposed in the liquid raw material replenishment pipeline, which is continuous with the nozzle and whose axial direction is vertical; The second valve is located upstream of and above the first valve on the liquid raw material supply line. as well as A liquid raw material storage section is formed between the first valve and the second valve. The filling process involves opening the second valve while the first valve is closed to fill the liquid raw material storage section with the liquid raw material. The discharge process, following the filling process, involves closing the second valve and opening the first valve to discharge the liquid raw material filling the liquid raw material storage section into the vaporization container.

20. A computer-readable recording medium containing a program, characterized in that, The program, via a computer, causes the substrate processing apparatus to perform a process of supplying liquid raw materials into the vaporization container by carrying out filling and discharging processes within the substrate processing apparatus. The substrate processing apparatus includes: A liquid feedstock supply line is connected at one end to a nozzle formed inside the vaporization container and at the other end to a liquid feedstock supply source. The first valve is disposed in the liquid raw material replenishment pipeline, which is continuous with the nozzle and whose axial direction is vertical; The second valve is located upstream of and above the first valve on the liquid raw material supply line. as well as A liquid raw material storage section is formed between the first valve and the second valve. The filling process involves opening the second valve while the first valve is closed to fill the liquid raw material storage section with the liquid raw material. The discharge process, after the filling process, involves closing the second valve and opening the first valve to discharge the liquid raw material filled in the liquid raw material storage section into the vaporization container.

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