Classifications

• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P50/00—Etching of wafers, substrates or parts of devices
  • H10P50/60—Wet etching
  • H10P50/64—Wet etching of semiconductor materials
  • H10P50/642—Chemical etching
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
  • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
  • H10P14/34—Deposited materials, e.g. layers
  • H10P14/3451—Structure
  • H10P14/3452—Microstructure
  • H10P14/3454—Amorphous
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
  • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
  • H10P14/34—Deposited materials, e.g. layers
  • H10P14/3451—Structure
  • H10P14/3452—Microstructure
  • H10P14/3456—Polycrystalline
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P50/00—Etching of wafers, substrates or parts of devices
  • H10P50/20—Dry etching; Plasma etching; Reactive-ion etching
  • H10P50/24—Dry etching; Plasma etching; Reactive-ion etching of semiconductor materials
  • H10P50/242—Dry etching; Plasma etching; Reactive-ion etching of semiconductor materials of Group IV materials
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P72/00—Handling or holding of wafers, substrates or devices during manufacture or treatment thereof
  • H10P72/04—Apparatus for manufacture or treatment
  • H10P72/0402—Apparatus for fluid treatment
  • H10P72/0418—Apparatus for fluid treatment for etching
  • H10P72/0421—Apparatus for fluid treatment for etching for drying etching

Definitions

• This disclosure relates to a processing method, a processing device, a method for manufacturing a semiconductor device, and a program.
• a process may be performed in which a crystal layer dividing film is formed on the surface of a metal-containing film or abnormal growth nuclei are removed from the surface of the metal-containing film to form multiple layers of the metal-containing film on a substrate (see, for example, Patent Document 1).
• This disclosure provides technology that can improve the roughness of a film surface (hereinafter referred to as surface roughness).
• This disclosure makes it possible to improve the surface roughness of the film.
• FIG. 1 is a schematic vertical cross-sectional view of a vertical processing furnace of a substrate processing apparatus according to one embodiment of the present disclosure.
• FIG. 2 is a schematic cross-sectional view taken along line AA in FIG.
• FIG. 3 is a schematic configuration diagram of a controller of a substrate processing apparatus according to one embodiment of the present disclosure, and is a block diagram showing a control system of the controller.
• FIG. 4 is a diagram illustrating a process flow according to one embodiment of the present disclosure.
• FIG. 5 is a flow diagram showing the first cleaning process in the process flow of FIG. Fig. 6(A) is a diagram for explaining the state of the inner surface of the reaction tube before the cleaning process is performed, and Fig.
• FIG. 6(B) is a diagram for explaining the state of the inner surface of the reaction tube after the cleaning process is performed from the state shown in Fig. 6(A).
• Fig. 7(A) is a diagram for explaining the state of the surface inside the reaction tube before the cleaning treatment
• Fig. 7(B) is a diagram for explaining the state of the surface inside the reaction tube when the treatment treatment is performed from the state shown in Fig. 7(A)
• Fig. 7(C) is a diagram for explaining the state of the surface inside the reaction tube when the cleaning treatment is performed from the state shown in Fig. 7(B).
• FIG. 8 is a flow diagram showing a first cleaning process in the second aspect of the present disclosure.
• FIG. 9 is a flow diagram showing a first cleaning process in the third aspect of the present disclosure.
• the processing furnace 202 has a heater 207 as a temperature adjustment unit (heating unit).
• the heater 207 is cylindrical and is installed vertically by being supported by a holding plate.
• the heater 207 also functions as an activation mechanism (excitation unit) that activates (excites) gas by heat.
• a reaction tube 203 is disposed concentrically with the heater 207 inside the heater 207.
• the reaction tube 203 is made of a heat-resistant material such as quartz (SiO 2 ) or silicon carbide (SiC) and is formed in a cylindrical shape with a closed upper end and an open lower end.
• a manifold 209 is disposed concentrically with the reaction tube 203 below the reaction tube 203.
• the manifold 209 is made of a metal material such as stainless steel (SUS) and is formed in a cylindrical shape with an open upper end and a closed lower end. The upper end of the manifold 209 is engaged with the lower end of the reaction tube 203 and is configured to support the reaction tube 203.
• An O-ring 220a is provided between the manifold 209 and the reaction tube 203 as a seal member.
• the reaction tube 203 is installed vertically like the heater 207.
• the reaction tube 203 and the manifold 209 mainly constitute a processing vessel (reaction vessel).
• a processing chamber 201 is formed in a cylindrical hollow portion of the processing vessel.
• the processing chamber 201 is configured to be capable of accommodating a wafer 200 as a substrate.
• Nozzles 249a to 249c serving as first to third supply units are provided in the processing chamber 201 so as to penetrate the sidewall of the manifold 209, respectively.
• the nozzles 249a to 249c are also referred to as first to third nozzles, respectively.
• the nozzles 249a to 249c are made of a heat-resistant material such as SiO2 or SiC.
• Gas supply pipes 232a to 232c are connected to the nozzles 249a to 249c, respectively.
• Gas supply pipes 232a to 232c are provided with mass flow controllers (MFCs) 241a to 241c, which are flow rate controllers (flow rate control parts), and valves 243a to 243c, which are on-off valves, in order from the upstream side of the gas flow.
• MFCs mass flow controllers
• Gas supply pipes 232d and 232f are connected to gas supply pipe 232a downstream of valve 243a.
• Gas supply pipe 232e is connected to gas supply pipe 232b downstream of valve 243b.
• Gas supply pipe 232g is connected to gas supply pipe 232c downstream of valve 243c.
• Gas supply pipes 232d to 232g are provided with MFCs 241d to 241g and valves 243d to 243g in order from the upstream side of the gas flow.
• the nozzles 249a to 249c are provided in a circular space between the inner wall of the reaction tube 203 and the wafers 200 in a plan view, from the lower part to the upper part of the inner wall of the reaction tube 203, so as to rise upward in the arrangement direction of the wafers 200. That is, the nozzles 249a to 249c are provided in an area horizontally surrounding the wafer arrangement area on the side of the wafer arrangement area in which the wafers 200 are arranged, so as to follow the wafer arrangement area. In a plan view, the nozzle 249b is arranged so as to face the exhaust port 233 (described later) in a straight line across the center of the wafer 200 that is loaded into the processing chamber 201.
• the nozzles 249a and 249c are arranged so as to sandwich the straight line L passing through the nozzle 249b and the center of the exhaust port 233 from both sides along the inner wall of the reaction tube 203 (the outer periphery of the wafers 200).
• Gas supply holes 250a to 250c for supplying gas are provided on the side surfaces of the nozzles 249a to 249c, respectively.
• Each of the gas supply holes 250a to 250c opens so as to face (face) the exhaust port 233 in a plan view, and is capable of supplying gas toward the wafer 200.
• a plurality of gas supply holes 250a to 250c are provided from the bottom to the top of the reaction tube 203.
• the first process gas is supplied from the gas supply pipe 232a into the process chamber 201 via the MFC 241a, the valve 243a, and the nozzle 249a.
• a raw material gas or the like can be used as the first process gas.
• a metal-containing gas which is a gas containing a metal element, a silicon (Si)-containing gas, or the like can be used.
• the second process gas is supplied from the gas supply pipe 232b into the process chamber 201 via the MFC 241b, the valve 243b, and the nozzle 249b.
• the second process gas may be, for example, a reactive gas.
• the reactive gas may be, for example, a nitriding gas.
• the third process gas is supplied from the gas supply pipe 232c into the process chamber 201 via the MFC 241c, the valve 243c, and the nozzle 249c.
• a reducing gas or a treatment gas (also called a modifying gas) as the second gas can be used.
• a gas containing Si and hydrogen (H) can be used.
• a cleaning gas as a first gas is supplied from the gas supply pipe 232d through the MFC 241d, the valve 243d, the gas supply pipe 232a, and the nozzle 249a into the processing chamber 201.
• a halogen-containing gas such as a halogen-based gas can be used.
• Inert gas is supplied from gas supply pipes 232e to 232g into the processing chamber 201 via MFCs 241e to 241g, valves 243e to 243g, gas supply pipes 232e to 232g, and nozzles 249a to 249c.
• the inert gas acts as a purge gas, carrier gas, dilution gas, etc.
• the first process gas supply system (also called raw material gas supply system) is mainly composed of the gas supply pipe 232a, the MFC 241a, and the valve 243a.
• the second process gas supply system (also called reactive gas supply system) is mainly composed of the gas supply pipe 232b, the MFC 241b, and the valve 243b.
• the third process gas supply system (also called reduction gas supply system, second gas supply system, treatment gas supply system, or modified gas supply system) is mainly composed of the gas supply pipe 232c, the MFC 241c, and the valve 243c.
• the cleaning gas supply system (also called first gas supply system) is mainly composed of the gas supply pipe 232d, the MFC 241d, and the valve 243d.
• the inert gas supply system is mainly composed of the gas supply pipes 232e to 232g, the MFCs 241e to 241g, and the valves 243e to 243g.
• any or all of the various supply systems described above may be configured as an integrated supply system 248 in which valves 243a to 243g and MFCs 241a to 241g are integrated.
• the integrated supply system 248 is connected to each of the gas supply pipes 232a to 232g, and is configured so that the supply operation of various substances (various gases) into the gas supply pipes 232a to 232g, i.e., the opening and closing operation of the valves 243a to 243g and the flow rate adjustment operation by the MFCs 241a to 241g, are controlled by a controller 121, which will be described later.
• the integrated supply system 248 is configured as an integrated or separate integrated unit, and can be attached and detached to and from the gas supply pipes 232a to 232g, etc., in units of integrated units, and is configured so that maintenance, replacement, expansion, etc. of the integrated supply system 248 can be performed in units of integrated units.
• An exhaust port 233 for exhausting the atmosphere in the processing chamber 201 is provided at the bottom of the side wall of the reaction tube 203. As shown in FIG. 2, the exhaust port 233 is provided at a position facing the nozzles 249a to 249c (gas supply holes 250a to 250c) across the wafer 200 in a plan view. The exhaust port 233 may be provided along the side wall of the reaction tube 203 from the bottom to the top, that is, along the wafer arrangement area. An exhaust pipe 231 is connected to the exhaust port 233.
• a vacuum pump 246 as a vacuum exhaust device is connected to the exhaust pipe 231 via a pressure sensor 245 as a pressure detector (pressure detection unit) that detects the pressure in the processing chamber 201 and an APC (Auto Pressure Controller) valve 244 as a pressure regulator (pressure adjustment unit).
• the APC valve 244 is configured to be able to evacuate and stop the evacuation of the processing chamber 201 by opening and closing the valve while the vacuum pump 246 is operating, and further, to be able to adjust the pressure inside the processing chamber 201 by adjusting the valve opening based on pressure information detected by the pressure sensor 245 while the vacuum pump 246 is operating.
• An exhaust system is mainly configured by the exhaust pipe 231, the APC valve 244, and the pressure sensor 245.
• the vacuum pump 246 may be included in the exhaust system.
• a seal cap 219 is provided as a furnace port cover body capable of airtightly closing the lower end opening of the manifold 209.
• the seal cap 219 is made of a metal material such as SUS and is formed in a disk shape.
• An O-ring 220b is provided on the upper surface of the seal cap 219 as a sealing member that abuts against the lower end of the manifold 209.
• a rotation mechanism 267 is installed to rotate the boat 217 described later.
• the rotation shaft 255 of the rotation mechanism 267 is connected to the boat 217 through the seal cap 219.
• the rotation mechanism 267 is configured to rotate the wafers 200 by rotating the boat 217.
• the seal cap 219 is configured to be raised and lowered vertically by a boat elevator 115 as a lifting mechanism installed outside the reaction tube 203.
• the boat elevator 115 is configured as a transport device (transport mechanism) that transports the wafers 200 in and out of the processing chamber 201 by raising and lowering the seal cap 219.
• a shutter 219s is provided as a furnace port cover that can airtightly close the lower end opening of the manifold 209 when the seal cap 219 is lowered and the boat 217 is removed from the processing chamber 201.
• the shutter 219s is made of a metal material such as SUS and is formed in a disk shape.
• An O-ring 220c is provided on the upper surface of the shutter 219s as a sealing member that abuts against the lower end of the manifold 209.
• the opening and closing operation of the shutter 219s (lifting and lowering operation, rotating operation, etc.) is controlled by a shutter opening and closing mechanism 115s.
• the boat 217 as a substrate support is configured to support a plurality of wafers 200, for example 25 to 200, in multiple stages in a horizontal position and aligned vertically with their centers aligned, i.e., arranged at intervals.
• the boat 217 is made of a heat-resistant material such as SiO2 or SiC.
• heat insulating plates 218 made of a heat-resistant material such as SiO2 or SiC are supported in multiple stages.
• a temperature sensor 263 is installed inside the reaction tube 203 as a temperature detector. By adjusting the power supply to the heater 207 based on the temperature information detected by the temperature sensor 263, the temperature inside the processing chamber 201 is distributed as desired.
• the temperature sensor 263 is installed along the inner wall of the reaction tube 203.
• the controller 121 which is a control unit (control means), is configured as a computer equipped with a CPU (Central Processing Unit) 121a, a RAM (Random Access Memory) 121b, a storage device 121c, and an I/O port 121d.
• the RAM 121b, the storage device 121c, and the I/O port 121d are configured to be able to exchange data with the CPU 121a via an internal bus 121e.
• An input/output device 122 configured as, for example, a touch panel, is connected to the controller 121.
• an external storage device 123 can be connected to the controller 121.
• the storage device 121c is composed of, for example, a flash memory, a HDD (Hard Disk Drive), an SSD (Solid State Drive), etc.
• a control program for controlling the operation of the substrate processing apparatus, a process recipe describing the procedures and conditions of the substrate processing described later, etc. are recorded and stored in a readable manner.
• the process recipe is a combination of procedures in the substrate processing described later, which are executed by the controller 121 in the substrate processing apparatus to obtain a predetermined result, and functions as a program.
• the process recipe and the control program are collectively referred to simply as a program.
• the process recipe is also simply referred to as a recipe.
• the word program when used, it may include only the recipe alone, only the control program alone, or both.
• the RAM 121b is configured as a memory area (work area) in which the programs and data read by the CPU 121a are temporarily stored.
• the I/O port 121d is connected to the above-mentioned MFCs 241a to 241g, valves 243a to 243g, pressure sensor 245, APC valve 244, vacuum pump 246, temperature sensor 263, heater 207, rotation mechanism 267, boat elevator 115, shutter opening/closing mechanism 115s, etc.
• the CPU 121a is configured to read and execute a control program from the storage device 121c, and to read a recipe from the storage device 121c in response to input of an operation command from the input/output device 122, etc.
• the CPU 121a is configured to control the flow rate adjustment of various substances (various gases) by the MFCs 241a to 241g, the opening and closing of the valves 243a to 243g, the opening and closing of the APC valve 244 and the pressure adjustment by the APC valve 244 based on the pressure sensor 245, the start and stop of the vacuum pump 246, the temperature adjustment of the heater 207 based on the temperature sensor 263, the rotation and rotation speed adjustment of the boat 217 by the rotation mechanism 267, the raising and lowering of the boat 217 by the boat elevator 115, the opening and closing of the shutter 219s by the shutter opening and closing mechanism 115s, etc.
• the controller 121 can be configured by installing the above-mentioned program recorded and stored in the external storage device 123 into a computer.
• the external storage device 123 includes, for example, a magnetic disk such as an HDD, an optical disk such as a CD, a magneto-optical disk such as an MO, and a semiconductor memory such as a USB memory or an SSD.
• the storage device 121c and the external storage device 123 are configured as computer-readable recording media. Hereinafter, these are collectively referred to as recording media.
• recording medium When the term recording medium is used in this specification, it may include only the storage device 121c alone, only the external storage device 123 alone, or both.
• the program may be provided to the computer using a communication means such as the Internet or a dedicated line, without using the external storage device 123.
• Step S10> a pre-coating process for forming a pre-coating film in a processing vessel prior to a film-forming process will be described. Note that the pre-coating film is also simply called a film.
• a precoating process is performed (also referred to as precoating) to form a precoat film on the inside of the processing vessel, that is, on the surfaces of the members inside the processing vessel, such as the inner wall of the reaction tube 203, the outer surfaces of the nozzles 249a to 249c, the inner surfaces of the nozzles 249a to 249c, the inner surface of the manifold 209, the surface of the boat 217, and the upper surface of the seal cap 219.
• the precoating process may be performed with the boat 217 carried out.
• a first process gas is supplied into the process chamber 201.
• the valve 243a is opened to allow the first process gas to flow into the gas supply pipe 232a.
• the flow rate of the first process gas is adjusted by the MFC 241a, and the first process gas is supplied into the process chamber 201 through the nozzle 249a and exhausted from the exhaust port 233.
• the valve 243f is simultaneously opened to allow an inert gas to flow into the gas supply pipe 232a.
• the valves 243e and 243g may be opened to allow an inert gas to flow into the gas supply pipes 232b and 232c.
• a metal-containing gas can be used as the first processing gas.
• a transition metal-containing gas can be used as the metal-containing gas.
• a titanium (Ti), tungsten (W), molybdenum (Mo), or tantalum (Ta)-containing gas can be used as the transition metal-containing gas.
• a titanium tetrachloride (TiCl 4 ) gas can be used as the Ti-containing gas.
• an aluminum (Al), gallium (Ga), or indium (In)-containing gas can be used as the metal-containing gas.
• a Si-containing gas can be used as the first processing gas in addition to the metal-containing gas. One or more of these can be used as the first processing gas.
• N2 nitrogen
• a rare gas such as argon (Ar) gas, helium (He) gas, neon (Ne) gas, xenon (Xe) gas, etc.
• Ar argon
• He helium
• Xe xenon
• one or more of these gases can be used. This also applies to each step described later.
• valve 243a is closed to stop the supply of the first process gas into the process chamber 201. Then, the process chamber 201 is evacuated to remove gas remaining in the process chamber 201 (purging). At this time, the valves 243e, 243f, and 243g are opened to supply an inert gas into the process chamber 201.
• the inert gas acts as a purge gas.
• a second process gas is supplied into the process chamber 201.
• the valve 243b is opened to allow the second process gas to flow into the gas supply pipe 232b.
• the flow rate of the second process gas is adjusted by the MFC 241b, and the second process gas is supplied into the process chamber 201 through the nozzle 249b and exhausted from the exhaust port 233.
• the valve 243e is simultaneously opened to allow an inert gas to flow into the gas supply pipe 232b.
• the valves 243f and 243g may be opened to allow an inert gas to flow into the gas supply pipes 232a and 232c.
• a second process gas is supplied into the process container.
• a nitriding gas or the like is used as the second process gas.
• a hydrogen nitride gas such as ammonia (NH 3 ) gas, diazane (N 2 H 2 ) gas, hydrazine (N 2 H 4 ) gas, or N 3 H 8 gas can be used as the nitriding gas.
• NH 3 ammonia
• N 2 H 2 diazane
• N 2 H 4 hydrazine
• N 3 H 8 gas hydrazine
• a film of a predetermined composition and a predetermined thickness can be formed on the member inside the processing vessel.
• a titanium nitride (TiN) film is formed.
• a third process gas is supplied into the process chamber 201.
• the valve 243c is opened to allow the third process gas to flow into the gas supply pipe 232c.
• the flow rate of the third process gas is adjusted by the MFC 241c, and the third process gas is supplied into the process chamber 201 through the nozzle 249c and exhausted from the exhaust port 233.
• the valve 243g is simultaneously opened to allow an inert gas to flow into the gas supply pipe 232c.
• the valves 243f and 243e may be opened to allow an inert gas to flow into the gas supply pipes 232a and 232b.
• the third process gas may be, for example, a gas containing Si and H.
• the Si and H-containing gas may be, for example, a silane-based gas such as monosilane (SiH 4 ) gas, disilane (Si 2 H 6 ) gas, or trisilane (Si 3 H 8 ) gas. One or more of these may be used as the third process gas.
• a cycle including the above-mentioned S15 to S17 i.e., a cycle in which S15 to S17 are performed non-simultaneously, is performed a predetermined number of times (Y times, where Y is an integer of 1 or 2 or more), to form a pre-coat film of a predetermined thickness on the members inside the processing vessel.
• a predetermined number of times Y times, where Y is an integer of 1 or 2 or more
• TiSiN titanium silicon nitride
• the above series of operations completes the precoat process.
• adhesion to the inner walls of the processing vessel is improved, making it less likely for the film to peel off from the inner walls.
• the surface roughness of the initial precoat film can be reduced.
• the above-mentioned pre-coating process also makes it possible to prevent the film thickness drop phenomenon from occurring during film formation.
• the above-mentioned pre-coating process also makes it possible to prepare the environment and conditions inside the processing vessel before the next film formation process.
• the supply order and timing of the first process gas, second process gas, and third process gas in the above-mentioned precoat process are not limited to the above-mentioned order and timing.
• step S20> a description will be given of a film forming process in which the wafers 200 are carried into the processing furnace 202 and a film is formed on the wafers 200. That is, in this process, a film forming process is performed in which the wafers 200 are processed in a processing chamber.
• wafer used in this specification can mean the wafer itself, or a laminate of the wafer and a specified layer or film formed on its surface.
• surface of a wafer used in this specification can mean the surface of the wafer itself, or the surface of a specified layer, etc. formed on the wafer.
• the processing chamber 201 i.e., the space in which the wafer 200 exists, is evacuated by the vacuum pump 246 so that the pressure (vacuum level) is the desired. At this time, the pressure inside the processing chamber 201 is measured by the pressure sensor 245, and the APC valve 244 is feedback-controlled (pressure adjustment) based on the measured pressure information.
• the processing chamber 201 is also heated by the heater 207 so that the inside of the processing chamber 201 is at the desired temperature. At this time, the amount of electricity supplied to the heater 207 is feedback-controlled (temperature adjustment) based on the temperature information detected by the temperature sensor 263 so that the inside of the processing chamber 201 has the desired temperature distribution.
• the rotation mechanism 267 also starts rotating the wafer 200. The evacuation inside the processing chamber 201 and the heating and rotation of the wafer 200 continue at least until the processing of the wafer 200 is completed.
• a first process gas is supplied to the wafer 200 in the process chamber 201.
• the valve 243a is opened to allow the first process gas to flow into the gas supply pipe 232a.
• the flow rate of the first process gas is adjusted by the MFC 241a, and the first process gas is supplied into the process chamber 201 through the nozzle 249a and exhausted from the exhaust port 233.
• the valve 243f is simultaneously opened to allow an inert gas to flow into the gas supply pipe 232a.
• the valves 243e and 243g may be opened to allow an inert gas to flow into the gas supply pipes 232b and 232c.
• the first processing gas described above is supplied to the wafer 200.
• a second process gas is supplied to the wafer 200 in the process chamber 201.
• the valve 243b is opened to allow the second process gas to flow into the gas supply pipe 232b.
• the flow rate of the second process gas is adjusted by the MFC 241b, and the second process gas is supplied into the process chamber 201 through the nozzle 249b and exhausted from the exhaust port 233.
• the valve 243e is simultaneously opened to allow an inert gas to flow into the gas supply pipe 232b.
• the valves 243f and 243g may be opened to allow an inert gas to flow into the gas supply pipes 232a and 232c.
• the second process gas described above is supplied to the wafer 200.
• a film with a predetermined composition and a predetermined thickness can be formed on the wafer 200.
• the film T1 formed here is a polycrystalline film.
• the film T1 formed here may be, for example, a metal-containing film, which is a film containing a metal element.
• the metal-containing film may be, for example, a transition metal-containing film, which is a film containing a Group 3 to 11 element, which is a transition metal element.
• the transition metal-containing film may be, for example, a Ti, W, Mo, or Ta-containing film.
• the transition metal-containing film may be, for example, a transition metal nitride film.
• the transition metal nitride film may be, for example, a tantalum nitride (TaN) film, a tungsten nitride (WN) film, a molybdenum nitride (MoN) film, or a titanium nitride (TiN) film.
• the film T1 may be, for example, a simple film or a nitride film of Al, Si, Ga, In, or the like.
• an inert gas is supplied as a purge gas from each of the nozzles 249a to 249c into the processing chamber 201, and exhausted from the exhaust port 233. This purges the processing chamber 201, and gas and reaction by-products remaining in the processing chamber 201 are removed from the processing chamber 201 (after-purge). Thereafter, the atmosphere in the processing chamber 201 is replaced with the inert gas (inert gas replacement), and the pressure in the processing chamber 201 is returned to normal pressure (atmospheric pressure return).
• a film T1 is formed inside the processing vessel, that is, on the surfaces of the components inside the processing vessel, such as the inner wall of the reaction tube 203, the outer surfaces of the nozzles 249a to 249c, the inner surface of the nozzles 249a to 249c, the inner surface of the manifold 209, the surface of the boat 217, and the upper surface of the seal cap 219, and accumulates as deposits. If the amount of deposits, that is, the accumulated film thickness of the film T1, becomes too thick, peeling of the deposited film may occur, and the amount of particles generated may increase.
• a cleaning process may be performed to remove all the deposited film deposited inside the processing vessel before peeling of the deposited film occurs, and a precoat film may be formed inside the processing vessel from which all the deposited film has been removed.
• the productivity may decrease because of the long time required for the cleaning process and for forming the precoat film.
• a first cleaning process is performed to clean (also called etching) the surface of the film T1 formed in the processing vessel each time the film formation process S20 is performed, i.e., each time the substrate is processed, a second cleaning process is performed to remove the deposited film in the processing vessel when the accumulated film thickness in the processing vessel reaches a predetermined value or more.
• the accumulated film thickness is the thickness of the film formed by the film formation process, and when the first cleaning process is performed, it is calculated by subtracting the amount etched by the first cleaning process.
• the accumulated film thickness is calculated by pre-storing, for example, the film thickness formed on the wafer 200 by one film formation process and the amount etched by the first cleaning process, and each time the film formation process and the first cleaning process are performed, the number of processes for each process is counted, and the accumulated film thickness formed in the processing vessel is estimated.
• the accumulated film thickness may be an actual measurement value.
• the accumulated film thickness may be calculated based on at least one of the processing time, the flow rate of the gas used in the film formation process and the first cleaning process, and the pressure in the processing chamber 201.
• step S30> it is determined whether the cumulative film thickness is equal to or greater than a predetermined value. If the cumulative film thickness is smaller than the predetermined value, a first cleaning step S40, which will be described later, is performed. If the cumulative film thickness is equal to or greater than the predetermined value, a second cleaning step S50, which will be described later, is performed.
• a first cleaning process (also called an etching process) capable of removing (also called etching) at least a part of the film T1 formed in the process container is performed.
• the first cleaning process can also be called simple cleaning or light cleaning that is performed in a short time after each film formation process.
• the shutter 219s is moved by the shutter opening/closing mechanism 115s to open the lower end opening of the manifold 209 (shutter open).
• the empty boat 217 i.e., the boat 217 not loaded with the wafers 200
• the boat elevator 115 is lifted by the boat elevator 115 and loaded into the processing chamber 201.
• the seal cap 219 seals the lower end of the manifold 209 via the O-ring 220b.
• the first cleaning process may be performed in a state where the boat 217 is unloaded.
• the processing chamber 201 is evacuated by the vacuum pump 246 so that the interior of the processing chamber 201 is at the desired pressure.
• the interior of the processing chamber 201 is heated by the heater 207 so that the interior of the processing chamber 201 is at the desired temperature.
• Rotation of the boat 217 by the rotation mechanism 267 is started. Operation of the vacuum pump 246, heating of the interior of the processing chamber 201, and rotation of the boat 217 continue at least until this process is completed. Note that the boat 217 does not have to be rotated.
• the processing temperature in this process is 400 to 500°C, which is the same as the processing temperature in the film formation process S20 described above.
• the processing pressure in this process is lower than the processing pressure in the film formation process S20.
• the processing temperature refers to the temperature of the wafer 200 or the temperature inside the processing chamber 201
• the processing pressure refers to the pressure inside the processing chamber 201
• the processing time refers to the time the processing continues.
• next treatment process S41, cleaning process S42, and purging S43 are performed a predetermined number of times (m times, where m is an integer of 1 or 2 or more), thereby completing the first cleaning process.
• a film T1 is deposited on the surface of the reaction tube 203, etc. Since the film T1 deposited here is a polycrystalline film with columnar crystals, when a cleaning process is performed by supplying a cleaning gas to the film T1 in this state, the cleaning gas may enter the grain boundaries, as shown in FIG. 6B, and the film T1 may be scraped (etched) from the grain boundaries. This may cause the surface of the film T1 to become uneven, and the surface roughness of the film T1 may become large. If the surface roughness of the film T1 is large, the surface area inside the processing vessel may become large, and the consumption of the processing gas inside the processing vessel may differ. This may cause the supply amount of the processing gas to the wafer 200 to differ, and the film thickness formed on the wafer 200 may become uneven. In addition, the film may partially peel off from inside the processing vessel, generating particles.
• a treatment process is performed before the cleaning process.
• a second film, film T2 is formed on a surface including grain boundaries of film T1, which is a polycrystalline film formed in a processing vessel.
• the surface including grain boundaries of film T1 is modified by the treatment gas, and film T2 is formed on the surface including grain boundaries of film T1. In this way, it is possible to prevent the grain boundaries of film T1 from being exposed to the cleaning gas.
• a film T2 is formed on the surface including the grain boundaries of the film T1 deposited on the surface of the reaction tube 203, etc., as shown in FIG. 7(B). That is, the film T2 is formed so as to fill the grain boundaries of the film T1.
• the film T1 is etched from above by the first cleaning process described later, improving the surface roughness of the film, and the amount of processing gas consumed by the wafer 200 when processing the wafer 200 can be made uniform for each wafer.
• “for each wafer” includes either or both of "for each wafer when multiple wafers are processed in one process” and "for each wafer when substrate processing (also called batch processing) is performed.”
• a third process gas is supplied into the process chamber 201.
• the valve 243c is opened to allow the third process gas to flow into the gas supply pipe 232c.
• the flow rate of the third process gas is adjusted by the MFC 241c, and the third process gas is supplied into the process chamber 201 through the nozzle 249c and exhausted from the exhaust port 233.
• the valve 243g is simultaneously opened to allow an inert gas to flow into the gas supply pipe 232c.
• the valves 243f and 243e may be opened to allow an inert gas to flow into the gas supply pipes 232a and 232b.
• a third processing gas is supplied as a treatment gas into the processing container.
• the treatment gas in this step may be supplied continuously or in portions.
• the treatment gas may be a gas capable of forming a film by itself or a gas capable of changing the surface state of a target film.
• the treatment gas may be, for example, a Si-containing gas.
• the Si-containing gas may be, for example, a silane- based gas such as SiH4 gas, Si2H6 gas, or Si3H8 gas.
• an oxidizing gas, a metal-containing gas, or the like may be used.
• the oxidizing gas may be, for example, oxygen ( O2 ) gas, ozone ( O3 ) gas, water vapor ( H2O ) gas, hydrogen peroxide ( H2O2 ) gas, a mixed gas of hydrogen ( H2 ) and O2 , nitrous oxide ( N2O ) gas, nitric oxide (NO) gas, nitrogen dioxide ( NO2 ) gas, or the like. At least one of these can be used as the oxidation gas.
• the treatment gas can be used as the treatment gas.
• a gas that can fill the grain boundaries of the film to be cleaned is preferable.
• a gas that can form a film on the grain boundaries is preferable.
• Gases capable of forming a film on the grain boundaries in this way include the Si-containing gas and metal-containing gas of the present disclosure.
• a gas that seals the halogen element in the film in the processing vessel is preferred, and a gas that does not contain a halogen element is used.
• a silane-based gas or an oxidizing gas for example, a silane-based gas or an oxidizing gas.
• the treatment gas is supplied to the film T1 in a state where the treatment gas is decomposed.
• the state where the treatment gas is decomposed includes, for example, supplying the treatment gas at a temperature equal to or higher than the decomposition temperature of the treatment gas.
• the state where the treatment gas is decomposed is, for example, a state where the film T1 is composed of a catalyst for the treatment gas. That is, the film T1 is preferably a film that serves as a catalyst for the treatment gas.
• the temperature adjustment time can be shortened during each of the substrate processing, cleaning processing, etching processing, and treatment processing (also called modification processing). This allows the throughput in the manufacturing process of semiconductor devices to be improved.
• the film T2 formed here is a film with lower crystallinity than the film T1, such as an amorphous film. This allows the crystal grain boundaries of the film T1, which is a polycrystalline film, to be filled with the film T2.
• the etching rate of the film T2 when a cleaning gas is supplied (second etching rate) is equal to or less than the etching rate of the film T1 when a cleaning gas is supplied (first etching rate).
• the etching rate of the film T2 when a cleaning gas is supplied is smaller than the etching rate of the film T1 when a cleaning gas is supplied.
• the thickness of the film T2 formed here is thinner than the thickness of the film T1. As a result, the film T1 is etched from above by the first cleaning process described below, improving the surface roughness of the film.
• a film containing elements of groups 13 to 16 is formed.
• a film containing elements of groups 13 to 16 for example, a film containing Si, boron (B), oxygen (O), or phosphorus (P) can be used.
• a silicon nitride (SiN) film, a silicon oxide (SiO) film, a TiSiN film, a B film, a boron nitride (BN) film, a P film, or a TiPN film can be used.
• the decomposition temperature of the SiH4 gas is, for example, 350 to 400° C.
• the SiH4 gas is easily decomposed on the TiN film, and the TiN film is a film that serves as a catalyst for SiH4 .
• a cleaning gas is supplied into the processing chamber 201.
• the valve 243d is opened to allow the cleaning gas to flow into the gas supply pipe 232a.
• the cleaning gas is adjusted in flow rate by the MFC 241d, is supplied into the processing chamber 201 via the nozzle 249a, and is exhausted from the exhaust pipe 231.
• the valve 243f is simultaneously opened to allow an inert gas to flow into the gas supply pipe 232a.
• the valves 243e and 243g may be opened to allow the inert gas to flow into the gas supply pipes 232b and 232c.
• the cleaning gas may be, for example, a halogen-based gas.
• halogen-based gas include nitrogen trifluoride (NF3 ) gas, fluorine ( F2 ) gas, chlorine ( Cl2 ) gas, hydrogen fluoride (HF) gas, chlorine trifluoride ( ClF3 ) gas, hydrogen chloride (HCl) gas, boron trichloride ( BCl3 ) gas, and bromine ( Br2 ) gas.
• NF3 nitrogen trifluoride
• F2 fluorine
• Cl2 chlorine
• HF hydrogen fluoride
• ClF3 chlorine trifluoride
• HHCl hydrogen chloride
• BCl3 boron trichloride
• Br2 bromine
• the cleaning gas is supplied to the film T1 having the film T2 formed on its surface including the grain boundaries, and at least a portion of the film T1 is removed.
• valve 243d is closed to stop the supply of cleaning gas into the processing chamber 201.
• the film T1 in the processing vessel is etched to a predetermined thickness by performing a cycle including the above-described S41 to S43, i.e., a cycle in which S41 to S43 are performed non-simultaneously, a predetermined number of times (m times, where m is an integer of 1 or 2 or more).
• the processing conditions for the first cleaning (etching) process are as follows: Cleaning gas supply flow rate: 0.1 to 10 slm Inert gas supply flow rate (each gas supply pipe): 0 to 10 slm Supply time of each gas: 5 to 300 seconds, preferably 100 to 200 seconds Treatment temperature: 200° C. or higher but lower than 900° C., preferably 300 to 800° C., more preferably 350 to 600° C. Treatment pressure: 150 to 400 Pa, preferably 200 to 300 Pa.
• 0 slm means that the gas is not supplied. This also applies to other descriptions in this disclosure.
• abnormal growth nuclei grow along with the crystal growth of TiN.
• the abnormal growth nuclei formed on the surface of the TiN film in the processing vessel are removed (etched).
• the surface of the TiN film formed in the processing vessel is etched and flattened.
• Step S50> an empty boat 217 is loaded into the processing chamber 201, and a second cleaning process is performed to remove the deposition film and pre-coat film deposited on the inner wall of the processing vessel and the like for a longer time than the first cleaning process described above. That is, the cycle of steps S41 to S43 described above is performed a predetermined number of times (m times, where m is an integer of 1 or 2 or more), and when the cumulative film thickness in the processing vessel reaches a predetermined value or more, the second cleaning process is performed. This removes the film deposited in the processing vessel.
• the processing chamber 201 is evacuated by the vacuum pump 246 so that the interior of the processing chamber 201 reaches the desired pressure.
• the interior of the processing chamber 201 is also heated by the heater 207 so that the interior of the processing chamber 201 reaches the desired temperature.
• Rotation of the boat 217 by the rotation mechanism 267 is also started. Operation of the vacuum pump 246, heating of the interior of the processing chamber 201, and rotation of the boat 217 continue at least until this process is completed. Note that the boat 217 does not have to be rotated.
• the above-mentioned cleaning gas is supplied into the processing chamber 201.
• the valve 243d is opened to allow the cleaning gas to flow into the gas supply pipe 232a.
• the cleaning gas is adjusted in flow rate by the MFC 241d, is supplied into the processing chamber 201 through the nozzle 249a, and is exhausted from the exhaust pipe 231.
• the valve 243f may be opened at the same time to allow an inert gas to flow into the gas supply pipe 232a.
• the valves 243e and 243g may be opened to allow an inert gas to flow into the gas supply pipes 232b and 232c.
• the valve 243d is closed to stop the supply of cleaning gas into the processing chamber 201.
• the cleaning gas is supplied into the processing vessel in which the film to be cleaned is formed for a longer period of time than the supply period of the cleaning gas during the first cleaning process.
• the processing chamber 201 is purged (purging) by a processing procedure similar to that of the purge S12 described above. Thereafter, the atmosphere in the processing chamber 201 is replaced with an inert gas (inert gas replacement).
• the precoating process S10 is performed to form a precoat film inside the processing vessel described above.
• the inside of the processing vessel is precoated.
• a second cleaning process is performed.
• the deposition film and precoat film deposited in the processing vessel are etched. In other words, by performing the second cleaning process, even the precoat film formed in the processing vessel is etched.
• the first cleaning process is performed in a short time, and if the cumulative film thickness inside the processing vessel after substrate processing is equal to or greater than the predetermined value, the second cleaning process is performed. This makes it possible to perform cleaning efficiently in a short time compared to the case where the first cleaning process described above is not performed.
• the first cleaning process is performed by carrying out the cleaning process S411, the purging process S412, and the treatment process S413 a predetermined number of times (m times, where m is an integer of 1 or 2 or more). That is, the order of the processes is different from that of the first cleaning process described above.
• the cleaning process S411, the purging process S412, and the treatment process S413 are performed in the same manner as the cleaning process S42, the purging process S43, and the treatment process S41 described above.
• the cleaning process is performed after the treatment process, so as in the above embodiment, the deterioration of the surface roughness of the film T1 can be improved.
• the treatment process S413 is further performed at the end of the first cleaning process, so that the components contained in the cleaning gas can be prevented from remaining in the reaction tube 203.
• the components contained in the cleaning gas can be prevented from being adsorbed onto the wafer 200.
• the treatment process S44 is carried out after the treatment process S41, cleaning process S42 and purging process S43 in the above-described embodiment are carried out a predetermined number of times (m times, where m is an integer of 1 or 2 or more). That is, the treatment process S44 is carried out after the process shown in Fig. 5 is carried out.
• the treatment process S44 is carried out in the same manner as the above-described treatment process S41. That is, the treatment process is carried out before and after the cleaning process.
• the deterioration of the surface roughness of the film T1 can be improved.
• the components contained in the cleaning gas can be further prevented from remaining in the reaction tube 203.
• the components contained in the cleaning gas can be prevented from being adsorbed onto the wafer 200 in the next film formation process S20.
• the present disclosure is not limited thereto, and can also be suitably applied to the case where the film T1 formed on the wafer 200 is etched. That is, the present disclosure can also be suitably applied to the case where the film T2 is formed on the surface including the grain boundaries of the film T1 formed on the wafer 200, and the film T1 formed on the wafer 200 is etched. In this embodiment, the surface roughness of the film formed on the surface of the wafer 200 can also be reduced. This can improve the uniformity of the film formed on the surface of the wafer 200, and the characteristics of the semiconductor device can be improved.
• the substrate to which this embodiment is applied either or both of the product substrate and the dummy substrate can be used.
• the product substrate is a substrate used as a semiconductor device.
• the surface roughness of the film forming one structure of the semiconductor device can be improved.
• the dummy substrate is a substrate used when processing the product substrate.
• the dummy substrate is, for example, a monitor substrate used for inspection, or a fill dummy substrate used to make the gas consumption uniform.
• the amount of gas consumed in the dummy substrate can be made uniform for each substrate processing. This makes it possible to make the amount of consumption of the processing gas supplied to each product substrate uniform.
• the recipes used for each process are prepared individually according to the process content and stored in the storage device 121c via an electric communication line or the external storage device 123. Then, when starting each process, it is preferable that the CPU 121a appropriately selects an appropriate recipe according to the process content from among the multiple recipes recorded and stored in the storage device 121c. This makes it possible to reproducibly form films of various film types, composition ratios, film qualities, and thicknesses using a single substrate processing device. It also reduces the burden on the operator and makes it possible to quickly start each process while avoiding operating errors.
• the above-mentioned recipes do not necessarily have to be created from scratch, but may be prepared, for example, by modifying an existing recipe that has already been installed in the substrate processing apparatus.
• the modified recipe may be installed in the substrate processing apparatus via an electric communication line or a recording medium on which the recipe is recorded.
• an existing recipe that has already been installed in the substrate processing apparatus may be directly modified by operating the input/output device 122 provided in the existing substrate processing apparatus.
• an example of forming a film using a batch-type substrate processing apparatus that processes multiple substrates at a time has been described.
• the present disclosure is not limited to the above embodiment, and can be suitably applied, for example, to a case where a film is formed using a single-wafer substrate processing apparatus that processes one or several substrates at a time.
• an example of forming a film using a substrate processing apparatus having a hot-wall type processing furnace has been described.
• the present disclosure is not limited to the above embodiment, and can be suitably applied, for example, to a case where a film is formed using a substrate processing apparatus having a cold-wall type processing furnace.
• each process can be performed using the same process procedures and conditions as those in the above-mentioned and other embodiments, and the same effects as those in the above-mentioned and other embodiments can be obtained.
• processing procedures and processing conditions in this case can be, for example, the same as the processing procedures and processing conditions in the above-mentioned aspects and other aspects.

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• 2023
  • 2023-06-29 JP JP2025529147A patent/JPWO2025004295A1/ja active Pending
  • 2023-06-29 CN CN202380094083.2A patent/CN120712638A/zh active Pending
  • 2023-06-29 KR KR1020257032431A patent/KR20260028662A/ko active Pending
  • 2023-06-29 WO PCT/JP2023/024287 patent/WO2025004295A1/ja not_active Ceased
• 2024
  • 2024-06-07 TW TW113121143A patent/TW202507044A/zh unknown
• 2025
  • 2025-09-25 US US19/340,286 patent/US20260026280A1/en active Pending

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