WO2019097901A1 - 基板処理方法および基板処理装置 - Google Patents

基板処理方法および基板処理装置 Download PDF

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Publication number
WO2019097901A1
WO2019097901A1 PCT/JP2018/037581 JP2018037581W WO2019097901A1 WO 2019097901 A1 WO2019097901 A1 WO 2019097901A1 JP 2018037581 W JP2018037581 W JP 2018037581W WO 2019097901 A1 WO2019097901 A1 WO 2019097901A1
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Prior art keywords
phosphoric acid
tank
aqueous solution
supply
substrate
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PCT/JP2018/037581
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English (en)
French (fr)
Japanese (ja)
Inventor
修 堀口
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Screen Holdings Co Ltd
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Screen Holdings Co Ltd
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Priority to CN201880073324.4A priority Critical patent/CN111344839B/zh
Priority to KR1020207013563A priority patent/KR102483802B1/ko
Publication of WO2019097901A1 publication Critical patent/WO2019097901A1/ja
Anticipated expiration legal-status Critical
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    • 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
    • H10P50/28—Dry etching; Plasma etching; Reactive-ion etching of insulating materials
    • H10P50/282—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials
    • H10P50/283—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials by chemical means
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • 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
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H10P14/69—Inorganic materials
    • H10P14/692—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses
    • H10P14/6921—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses containing silicon
    • H10P14/69215—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses containing silicon the material being a silicon oxide, e.g. SiO2
    • 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
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H10P14/69—Inorganic materials
    • H10P14/694—Inorganic materials composed of nitrides
    • H10P14/6943—Inorganic materials composed of nitrides containing silicon
    • H10P14/69433—Inorganic materials composed of nitrides containing silicon the material being a silicon nitride not containing oxygen, e.g. SixNy or SixByNz
    • 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
    • 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
    • H10P72/0422—Apparatus for fluid treatment for etching for wet etching
    • H10P72/0424—Apparatus for fluid treatment for etching for wet etching using mainly spraying means, e.g. nozzles
    • 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
    • H10P72/06—Apparatus for monitoring, sorting, marking, testing or measuring
    • H10P72/0604—Process monitoring, e.g. flow or thickness monitoring

Definitions

  • the present invention relates to a method and apparatus for processing a substrate.
  • Substrates to be processed include, for example, substrates for FPD (Flat Panel Display) such as semiconductor wafers, liquid crystal display devices and organic EL (electroluminescence) display devices, substrates for optical disks, substrates for magnetic disks, and magneto-optical disks.
  • substrates for FPD Fluorescence Panel Display
  • Patent Document 1 discloses a substrate processing apparatus and a substrate processing method for selectively etching a silicon nitride film by supplying a phosphoric acid aqueous solution containing silicon to a substrate on which a silicon oxide film and a silicon nitride film are formed. .
  • a substrate processing apparatus and a substrate processing method for selectively etching a silicon nitride film by supplying a phosphoric acid aqueous solution containing silicon to a substrate on which a silicon oxide film and a silicon nitride film are formed. .
  • a phosphoric acid aqueous solution By containing silicon in the phosphoric acid aqueous solution, etching of the silicon oxide film is suppressed, thereby achieving highly selective silicon nitride film etching.
  • the substrate processing apparatus described in Patent Document 1 includes a spin chuck that holds and rotates a substrate, first to third tanks that respectively store a phosphoric acid aqueous solution, and a new liquid supply device.
  • the phosphoric acid aqueous solution is supplied from the first tank to the treatment liquid nozzle, and the phosphoric acid aqueous solution discharged from the treatment liquid nozzle is supplied to the substrate held by the spin chuck.
  • the phosphoric acid aqueous solution is supplied from the second tank to the first tank.
  • the spent phosphoric acid aqueous solution after being supplied to the substrate is collected in the third tank.
  • the phosphoric acid concentration in the recovered aqueous phosphoric acid solution is detected by a phosphoric acid concentration meter.
  • a phosphoric acid concentration adjusting operation is performed on the third tank by supplying phosphoric acid, DIW (deionized water) or nitrogen gas.
  • the silicon concentration in the recovered aqueous phosphoric acid solution is detected by the silicon densitometer.
  • the new solution supply device replenishes the third tank with the phosphoric acid aqueous solution, thereby adjusting the silicon concentration of the phosphoric acid aqueous solution in the third recovery tank to the reference silicon concentration.
  • the new liquid supply device prepares a new liquid (an unused phosphoric acid aqueous solution) whose silicon concentration is variably set according to the detection result of the silicon densitometer, and supplies the new liquid to the third tank Do.
  • a new liquid an unused phosphoric acid aqueous solution
  • the liquid path is switched so as to switch the roles of the second tank and the third tank, and the same operation is repeated.
  • the new solution supply device variably sets the silicon concentration of the new solution to be replenished in accordance with the silicon concentration in the recovered phosphoric acid aqueous solution. Therefore, it is necessary to prepare new solutions with different concentrations each time replenishment is performed.
  • the new solution supply device has a silicon densitometer, and while detecting the silicon concentration with this silicon densitometer, a phosphoric acid aqueous solution (stock solution) and a silicon concentrate are introduced and mixed. The introduction of a new solution disturbs the mixture, and accordingly the measurement results of the silicon densitometer are also disturbed. It takes time to prepare a new solution because it takes a corresponding time for the concentration of silicon in the mixture to become uniform and stable.
  • the liquid recovery to the third tank is stopped, the silicon concentration is measured, and the silicon concentration of the new solution is set accordingly, and then the new solution is prepared. Therefore, the new solution may be prepared in advance. Can not. Therefore, even if it is sufficient to supply a new solution at a reference concentration, a waiting time for new solution preparation occurs. If liquid replenishment to the first tank is delayed due to this waiting time, the productivity of substrate processing is affected.
  • an embodiment of the present invention is a substrate processing method and a substrate processing apparatus capable of stabilizing the concentration of silicon in an aqueous solution of phosphoric acid supplied to a substrate with an inexpensive configuration without impairing the productivity of substrate processing.
  • One embodiment of the present invention provides a substrate processing method of selectively etching the silicon nitride film by supplying a phosphoric acid aqueous solution containing silicon to a substrate where a silicon oxide film and a silicon nitride film are exposed at the surface.
  • the method according to one embodiment of the present invention comprises the steps of: storing a phosphoric acid aqueous solution containing silicon in a specified silicon concentration range in a tank; and supplying a phosphoric acid aqueous solution in the tank to a nozzle; Supplying silicon to process the substrate, recovering the phosphoric acid aqueous solution supplied to the substrate from the nozzle and used for processing the substrate to the tank, and silicon in the tank at a first concentration.
  • the silicon nitride film exposed on the surface of the substrate is selectively etched by treating the substrate with an aqueous solution of phosphoric acid.
  • an aqueous solution of phosphoric acid By controlling the concentration of silicon contained in the phosphoric acid aqueous solution to a specified silicon concentration range, it is possible to suppress the etching of the silicon oxide film exposed on the surface of the substrate, thereby enhancing the selectivity of the silicon nitride film.
  • An aqueous solution of phosphoric acid is supplied from the tank to the nozzle and supplied from the nozzle to the substrate.
  • the spent phosphoric acid aqueous solution used to process the substrate is collected into a tank.
  • the tank is supplied with a first phosphoric acid aqueous solution containing silicon at a first concentration and a phosphoric acid aqueous solution containing silicon at a second concentration.
  • the first phosphoric acid aqueous solution and the second phosphoric acid aqueous solution contain silicon at a first concentration and a second concentration, respectively, and the concentration values thereof may be fixed values, and no change is necessary. This is because, by appropriately determining the respective supply amounts of the first and second aqueous phosphoric acid solutions, the first aqueous phosphoric acid solution, the second aqueous phosphoric acid solution, and the aqueous phosphoric acid solution in the tank are mixed to obtain phosphorus in the specified silicon concentration range. This is because the aqueous acid solution can be stored in the tank.
  • the silicon concentration of the phosphoric acid aqueous solution in the tank can be adjusted by preparing the first phosphoric acid aqueous solution and the second phosphoric acid aqueous solution in advance and supplying only the necessary amount to the tank when necessary. Therefore, since the waiting time for replenishing the phosphoric acid aqueous solution to the tank can be reduced, it is possible to supply the phosphoric acid aqueous solution having a stable silicon concentration to the substrate without impairing the productivity of the substrate processing.
  • the silicon concentration of the first phosphoric acid aqueous solution and the second phosphoric acid aqueous solution can be controlled in real time Does not require such a configuration.
  • the phosphoric acid aqueous solution having the first or second concentration can be prepared by quantifying and mixing each of the stock solution of phosphoric acid aqueous solution not containing silicon and the silicon concentrate containing silicon at a predetermined concentration.
  • the concentration may be confirmed by a silicon densitometer, but the silicon densitometer is not an essential component. Therefore, a phosphoric acid aqueous solution having a stable silicon concentration can be supplied to the substrate with an inexpensive configuration.
  • the first concentration is a value within the defined silicon concentration range. According to this method, since the first concentration is a value within the defined silicon concentration range, the silicon concentration of the phosphoric acid aqueous solution in the tank is adjusted to a value within the defined silicon concentration range by supplying the first phosphoric acid aqueous solution. It is easy to guide.
  • the first concentration may be a reference silicon concentration (the most preferable silicon concentration value for substrate processing) within the defined silicon concentration range.
  • the second concentration is a value lower than the specified silicon concentration range.
  • the silicon concentration of the phosphoric acid aqueous solution in the tank is within the specified silicon concentration range by supplying the second phosphoric acid aqueous solution.
  • the silicon of the substrate material is eluted in the aqueous phosphoric acid solution by supplying the aqueous phosphoric acid solution to the substrate, so the concentration of the aqueous phosphoric acid solution collected in the tank is It is higher than before the supply. Therefore, by supplying the second phosphoric acid aqueous solution containing silicon at a second concentration lower than the prescribed silicon concentration range, the silicon concentration of the phosphoric acid aqueous solution in the tank can be easily led to the prescribed silicon concentration range.
  • the second concentration is zero. That is, in this embodiment, the secondary phosphoric acid aqueous solution is a phosphoric acid aqueous solution not containing silicon.
  • the silicon concentration of the phosphoric acid aqueous solution in the tank can be easily led to the specified silicon concentration range.
  • the first and second aqueous phosphoric acid solutions are mixed with the first and second aqueous phosphoric acid solutions by supplying the first and second aqueous phosphoric acid solutions to the tank at appropriately determined feed amounts.
  • the silicon concentration of the phosphoric acid aqueous solution in the tank can be derived to the reference silicon concentration.
  • a supply target amount of the first and second phosphoric acid aqueous solutions is set by taking the adjustment target value of the silicon concentration in the phosphoric acid aqueous solution in the tank as the first concentration. It is determined.
  • the supply amounts of the first and second aqueous phosphoric acid solutions are determined by setting the first concentration as the adjustment target value, and the first and second aqueous phosphoric acid solutions and the aqueous phosphoric acid solution recovered in the tank are By mixing, the silicon concentration of the phosphoric acid aqueous solution in the tank is led to the first concentration.
  • the silicon concentration of the phosphoric acid aqueous solution in the tank can be adjusted to the reference silicon concentration.
  • the silicon concentration of the phosphoric acid aqueous solution in the tank can be adjusted to the reference silicon concentration.
  • the phosphoric acid aqueous solution stored in the tank can be used as it is for processing the substrate without passing through the waiting time for achieving uniform concentration.
  • the supply amounts of the first and second aqueous phosphoric acid solutions are determined based on the type of the substrate. Based on the type of substrate, fluctuations in the silicon concentration in the aqueous phosphoric acid solution before and after substrate processing can be predicted. Therefore, the silicon concentration of the phosphoric acid aqueous solution in the tank can be appropriately adjusted by determining the supply amounts of the first and second phosphoric acid aqueous solutions based on the type of the substrate.
  • the type of substrate refers to the material of the substrate, the type of film formed on the surface of the substrate, the type of pattern formed on the surface of the substrate, and other substrates that affect the fluctuation of silicon concentration before and after use of the phosphoric acid aqueous solution Represents the attribute of.
  • the first and second phosphorus are dissolved based on the amount of silicon eluted from the substrate into the aqueous phosphoric acid solution by the aqueous phosphoric acid solution supplied from the nozzle.
  • the feed rate of the aqueous acid solution is determined.
  • silicon concentration of the phosphoric acid aqueous solution in the tank can be appropriately adjusted by determining the supply amounts of the first and second phosphoric acid aqueous solutions based on the amount of silicon eluted from the substrate.
  • the first and second ones of the phosphoric acid aqueous solution supplied to the substrate from the nozzle are collected based on the recovery rate of the phosphoric acid aqueous solution recovered in the tank.
  • the feed rate of the aqueous phosphoric acid solution is determined. Not all of the aqueous phosphoric acid solution discharged from the nozzles for processing the substrate is collected in the tank, and for example, part of the aqueous phosphoric acid solution is discarded along with the rinse process and the like.
  • the silicon concentration of the phosphoric acid aqueous solution in the tank can be increased while replenishing the necessary amount of phosphoric acid aqueous solution to the tank. It can be adjusted to the specified silicon concentration range.
  • the supply amounts of the first and second phosphoric acid aqueous solutions are determined based on the number of substrates processed by the phosphoric acid aqueous solution supplied from the nozzles. Ru.
  • the silicon concentration in the phosphoric acid aqueous solution in the tank deviates from the reference silicon concentration. Therefore, the silicon concentration of the aqueous phosphoric acid solution in the tank can be appropriately adjusted by determining the supply amounts of the first and second aqueous phosphoric acid solutions based on the number of substrates processed.
  • the number of processed substrates is, in this case, the number of substrates processed without adjusting the silicon concentration by the supply of the first and second aqueous phosphoric acid solutions.
  • the replenishment start condition includes a fluid volume condition related to the fluid volume stored in the tank.
  • the first and second aqueous phosphoric acid solutions are supplied with a fluid amount condition related to the fluid amount stored in the tank as a trigger.
  • the liquid amount in the tank may be reduced to a predetermined lower limit liquid amount as the liquid amount condition.
  • the replenishment start condition includes a processing number condition regarding the number of substrates processed by the phosphoric acid aqueous solution supplied from the nozzle.
  • the first and second aqueous phosphoric acid solutions are supplied triggered by the processing number condition regarding the number of processed substrates.
  • the silicon concentration in the phosphoric acid aqueous solution in the tank deviates from the reference silicon concentration.
  • the first and second aqueous phosphoric acid solutions are supplied to adjust the silicon concentration of the aqueous phosphoric acid solution in the tank.
  • the substrate can be treated with a stable silicon concentration phosphoric acid aqueous solution.
  • the replenishment start condition includes a silicon concentration condition related to a silicon concentration in an aqueous phosphoric acid solution supplied from the tank to the nozzle.
  • the first and second aqueous phosphoric acid solutions are supplied, triggered by the silicon concentration condition related to the silicon concentration in the aqueous phosphoric acid solution supplied from the tank toward the nozzle. More specifically, when the silicon concentration in the phosphoric acid aqueous solution supplied to the substrate deviates from the reference value by a predetermined value or more, the first and second phosphoric acid aqueous solutions are supplied to the tank to adjust the silicon concentration. It is also good.
  • the substrate can be treated with a stable silicon concentration phosphoric acid aqueous solution.
  • the method further includes a substrate holding step of holding the substrate horizontally, and the aqueous phosphoric acid solution is supplied from the nozzle to the surface of the substrate held in the substrate holding step.
  • the substrate is held horizontally, and an aqueous solution of phosphoric acid is supplied from the nozzle to the surface of the substrate.
  • one substrate is held horizontally by the substrate holder, and a phosphoric acid aqueous solution is discharged from the nozzle toward the surface of the substrate.
  • Insufficient adjustment of the silicon concentration may cause variation in processing quality among a plurality of processed substrates. It is preferable to perform the substrate rotation step of rotating the substrate held by the substrate holder in parallel when the phosphoric acid aqueous solution is supplied, in order to make the substrate processing uniform.
  • the method includes: supplying a third aqueous phosphoric acid solution containing silicon to the tank at a third concentration different from any of the first concentration and the second concentration. Further includes
  • a tertiary phosphoric acid aqueous solution containing silicon at a third concentration can be supplied to the tank.
  • the adjustment range of the silicon concentration in the phosphoric acid aqueous solution in the tank can be broadened.
  • the first phosphoric acid aqueous solution and the third phosphoric acid aqueous solution may be selectively used.
  • the step of supplying the third aqueous phosphoric acid solution is performed.
  • the third concentration is higher than the first concentration.
  • a tertiary phosphoric acid aqueous solution having a relatively high silicon concentration may be supplied to the tank.
  • the first phosphoric acid aqueous solution having a relatively low concentration is used in the tank It may be supplied.
  • the tank is a recovery tank in which an aqueous solution of phosphoric acid used for substrate processing is introduced through a recovery pipe, and an aqueous solution of phosphoric acid stored in the recovery tank is a preparation liquid supply pipe
  • the aqueous phosphoric acid solution stored in the supply tank is supplied to the nozzle via a supply pipe, and the first aqueous phosphoric acid solution and the second aqueous phosphoric acid solution are It is supplied to the recovery tank.
  • the treated aqueous phosphoric acid solution is introduced to a recovery tank through a recovery pipe. Then, the first and second aqueous phosphoric acid solutions are supplied to the recovery tank, and the silicon concentration in the aqueous phosphoric acid solution is adjusted in the recovery tank.
  • the silicon concentration adjusted phosphoric acid aqueous solution is sent from the preparation liquid supply pipe to the supply tank, and is supplied from the supply tank to the treatment liquid nozzle. Therefore, the silicon concentration in the phosphoric acid aqueous solution in the supply tank is stable since it is not affected by liquid recovery. As a result, it is possible to supply a phosphoric acid aqueous solution having a more stable silicon concentration from the processing liquid nozzle to the substrate.
  • a plurality of the recovery tanks are provided.
  • the said method is the collection destination selection process of selecting the collection destination of the phosphoric acid aqueous solution collect
  • the used phosphoric acid aqueous solution is collected in a collection tank selected from among a plurality of collection tanks, and a phosphoric acid aqueous solution whose silicon concentration has been adjusted is supplied from the non-selected collection tank to the supply tank.
  • a phosphoric acid aqueous solution whose silicon concentration has been adjusted is supplied from the non-selected collection tank to the supply tank.
  • the silicon concentration in the phosphoric acid aqueous solution in the recovery tank for supplying the phosphoric acid aqueous solution to the supply tank is stable, the silicon concentration in the phosphoric acid aqueous solution in the supply tank can be stably maintained. Thereby, the silicon concentration in the phosphoric acid aqueous solution used for substrate processing is further stabilized.
  • the supply amounts of the first and second aqueous phosphoric acid solutions can be accurately managed.
  • the silicon concentration in the phosphoric acid aqueous solution in the tank can be accurately adjusted.
  • An embodiment of the present invention further provides a substrate processing apparatus suitable for performing the substrate processing method as described above.
  • a substrate processing apparatus for holding a substrate having a silicon oxide film and a silicon nitride film exposed on the surface, and phosphoric acid containing silicon in the substrate held by the substrate holding means
  • a first phosphoric acid aqueous solution supply means for supplying a first phosphoric acid aqueous solution containing silicon at a first concentration to the tank, and a second concentration lower than the first concentration in the tank.
  • Second phosphoric acid aqueous solution feeding means for feeding the second phosphoric acid aqueous solution containing the first phosphoric acid aqueous solution, and the first phosphoric acid aqueous solution feeding means and the second li Supplying a first aqueous phosphoric acid solution and a second aqueous phosphoric acid solution to the tank by controlling an aqueous acid solution supply unit; supplying the first aqueous phosphoric acid solution and the second aqueous phosphoric acid solution Determining means for determining an amount.
  • the control means determines the type of substrate, the amount of silicon eluted from the substrate to the phosphoric acid aqueous solution by the phosphoric acid aqueous solution supplied from the nozzle, the nozzle Based on at least one of the recovery rate of the phosphoric acid aqueous solution recovered in the tank among the phosphoric acid aqueous solutions supplied to the substrate and the number of the substrates processed by the phosphoric acid aqueous solution supplied from the nozzle The supply amounts of the first aqueous phosphoric acid solution and the second aqueous phosphoric acid solution are determined.
  • the replenishment condition is a liquid amount condition related to the liquid amount stored in the tank, a processing number condition related to the number of substrates processed by the phosphoric acid aqueous solution supplied from the nozzle, and At least one of the silicon concentration conditions relating to the silicon concentration in the aqueous phosphoric acid solution supplied from the tank to the nozzle.
  • the substrate processing apparatus further comprises a third aqueous phosphoric acid solution for supplying a third aqueous phosphoric acid solution containing silicon to the tank at a third concentration different from any of the first concentration and the second concentration.
  • the apparatus further includes supply means, and the control means further controls the third aqueous phosphoric acid solution supply means.
  • the tank is a recovery tank in which an aqueous solution of phosphoric acid used for substrate processing is introduced through a recovery pipe, and an aqueous solution of phosphoric acid stored in the recovery tank is a preparation liquid supply pipe
  • the aqueous phosphoric acid solution stored in the supply tank is supplied to the nozzle via a supply pipe, and the first aqueous phosphoric acid solution and the second aqueous phosphoric acid solution are It is supplied to the recovery tank.
  • a plurality of the recovery tanks are provided. Then, the control unit further selects a recovery destination of the aqueous phosphoric acid solution recovered via the recovery pipe from among the plurality of recovery tanks, a recovery destination selecting step, the first aqueous phosphoric acid solution, and the first The supply destination selection step of selecting the supply destination of the dibasic acid aqueous solution as the collection tank selected in the collection destination selection step, and the recovery tank not selected in the collection tank selection step among the plurality of collection tanks, And a replenishment source selection step of selecting as a replenishment source for replenishing the supply tank with the aqueous phosphoric acid solution via the preparation liquid supply pipe.
  • the substrate processing apparatus further comprises: a first integrated flow meter for measuring a supply amount of the first phosphoric acid aqueous solution supplied to the tank by the first phosphoric acid aqueous solution supply unit; And a second integrated flow meter that measures the supply amount of the second aqueous phosphoric acid solution supplied to the tank by the aqueous phosphoric acid solution supply unit, and the control unit is configured to include the first integrated flow meter and the second integration Based on the measurement result of the flow meter, a supply amount management step of managing supply of the first phosphoric acid aqueous solution and the second phosphoric acid aqueous solution to the tank is further executed.
  • FIG. 1 is a schematic view of a processing unit provided in a substrate processing apparatus according to an embodiment of the present invention as viewed from the horizontal direction.
  • FIG. 2 is a schematic view for explaining the configuration of a phosphoric acid supply system provided in the substrate processing apparatus.
  • FIG. 3 is a block diagram for explaining the main electrical configuration of the substrate processing apparatus.
  • FIG. 4 is a cross-sectional view showing an example of a substrate processed by the substrate processing apparatus.
  • FIG. 5 is a process diagram for explaining an example of substrate processing performed by the substrate processing apparatus.
  • FIG. 6 is a flowchart for explaining the process related to the supply of the phosphoric acid aqueous solution in the substrate processing apparatus.
  • FIG. 1 is a schematic view of a processing unit provided in a substrate processing apparatus according to an embodiment of the present invention as viewed from the horizontal direction.
  • FIG. 2 is a schematic view for explaining the configuration of a phosphoric acid supply system provided in the substrate processing apparatus.
  • FIG. 3 is a block diagram for
  • FIG. 7 is a schematic view for explaining the configuration of a substrate processing apparatus according to another embodiment of the present invention, mainly showing the configuration of a phosphoric acid supply system.
  • FIG. 8 is a block diagram for explaining the electrical configuration of the substrate processing apparatus having the configuration of FIG.
  • FIG. 9 is a flow chart for explaining the process related to the supply of phosphoric acid aqueous solution in the substrate processing apparatus having the configuration of FIG.
  • FIG. 10 is a flow chart for explaining the process related to the supply of the phosphoric acid aqueous solution in the substrate processing apparatus having the configuration of FIG. 7, and shows the selection of the recovery destination of used phosphoric acid and the phosphoric acid aqueous solution replenishing source Represents an operation related to the selection of FIG.
  • FIG. 11 is a flow chart for explaining the processing related to the supply of the phosphoric acid aqueous solution in the substrate processing apparatus of the configuration of FIG. 7, and shows the operation regarding the replenishment of the new solution to the recovery tank.
  • FIG. 12 is a schematic view for explaining the configuration of a substrate processing apparatus according to still another embodiment of the present invention.
  • FIG. 1 is a schematic view of a processing unit provided in a substrate processing apparatus according to an embodiment of the present invention as viewed from the horizontal direction.
  • the substrate processing apparatus 1 is a sheet-fed apparatus that processes a substrate W such as a semiconductor wafer one by one.
  • the substrate processing apparatus 1 transports the substrate W to a plurality of processing units 2 (only one is shown in FIG. 1) that processes the substrate W with a processing fluid such as a processing liquid or processing gas, and a plurality of processing units 2
  • a robot not shown
  • a control device 3 control means for controlling the substrate processing apparatus 1 are included.
  • the processing unit 2 receives the processing liquid scattered outward from the substrate W, the spin chuck 5 rotated about the vertical rotation axis A1 passing through the central portion of the substrate W while holding the substrate W horizontally in the chamber 4 And a cylindrical processing cup 10.
  • the spin chuck 5 includes a disk-like spin base 7 held in a horizontal posture, a plurality of chuck pins 6 for holding the substrate W in a horizontal posture above the spin base 7, and a central portion of the spin base 7. It includes a spin shaft 8 extending downward, and a spin motor 9 for rotating the spin base 7 and the plurality of chuck pins 6 by rotating the spin shaft 8.
  • the spin chuck 5 is not limited to a sandwich type chuck for holding the plurality of chuck pins 6 in contact with the outer peripheral surface of the substrate W, but the back surface (lower surface) of the substrate W which is a non-device forming surface is the upper surface of the spin base 7 It may be a vacuum type chuck which holds the substrate W horizontally by suction.
  • the processing cup 10 includes a plurality of guards 11 that receive the liquid discharged outward from the substrate W, and a plurality of cups 12 that receive the liquid guided downward by the guard 11.
  • the guard 11 includes a cylindrical tubular portion 11b surrounding the spin chuck 5, and an annular ceiling portion 11a extending obliquely upward from the upper end of the tubular portion 11b toward the rotation axis A1.
  • the plurality of ceiling portions 11a overlap in the vertical direction, and the plurality of cylindrical portions 11b are arranged in a concentric cylindrical shape.
  • the plurality of cups 12 are respectively disposed below the plurality of cylindrical portions 11 b.
  • the cup 12 forms an annular receiving groove 12a opened upward.
  • the processing unit 2 includes a guard elevating unit 13 that raises and lowers the plurality of guards 11 individually.
  • the guard elevating unit 13 vertically raises and lowers the guard 11 between the upper position and the lower position.
  • the upper position the upper end of the guard 11 is positioned above the substrate holding position where the spin chuck 5 holds the substrate W.
  • the upper end of the guard 11 is located below the substrate holding position.
  • the annular upper end of the ceiling portion 11 a corresponds to the upper end of the guard 11.
  • the upper end of the guard 11 surrounds the substrate W and the spin base 7 in plan view.
  • the processing liquid supplied to the substrate W is shaken off around the substrate W by the centrifugal force.
  • the processing liquid supplied to the substrate W the upper end of at least one guard 11 is disposed above the substrate W. Therefore, the processing solution such as the chemical solution and the rinse solution discharged around the substrate W is received by any one of the guards 11 and guided to the cup 12 corresponding to the guard 11.
  • the processing unit 2 includes a phosphoric acid nozzle 14 which discharges a phosphoric acid aqueous solution downward toward the upper surface of the substrate W.
  • the phosphoric acid nozzle 14 is connected to a phosphoric acid piping 15 for guiding a phosphoric acid aqueous solution.
  • the phosphoric acid valve 16 inserted in the phosphoric acid piping 15 is opened, the aqueous phosphoric acid solution is continuously discharged downward from the discharge port of the phosphoric acid nozzle 14.
  • the phosphoric acid aqueous solution is an aqueous solution containing phosphoric acid (H 3 PO 4 ) as a main component.
  • the concentration of phosphoric acid in the aqueous phosphoric acid solution is, for example, in the range of 50% to 100%, preferably about 90%.
  • the boiling point of the aqueous phosphoric acid solution varies depending on the concentration of phosphoric acid in the aqueous phosphoric acid solution, but is approximately in the range of 140 ° C. to 195 ° C.
  • the phosphoric acid aqueous solution discharged from the phosphoric acid nozzle 14 contains silicon. The silicon concentration in the phosphoric acid aqueous solution is controlled within a prescribed silicon concentration range.
  • the specified silicon concentration range is, for example, 15 ppm to 150 ppm, preferably 40 ppm to 60 ppm.
  • the silicon contained in the phosphoric acid aqueous solution may be a single silicon, a silicon compound, or both of them.
  • silicon contained in the phosphoric acid aqueous solution may contain silicon dissolved from the substrate W by the supply of the phosphoric acid aqueous solution.
  • the silicon contained in the aqueous phosphoric acid solution may contain silicon added to the aqueous phosphoric acid solution.
  • the phosphoric acid valve 16 includes a valve body forming a flow path, a valve body disposed in the flow path, and an actuator for moving the valve body.
  • the actuator may be a pneumatic actuator, an electric actuator, or any other actuator.
  • the control device 3 controls the actuator to open / close the phosphoric acid valve 16 or to change its opening degree.
  • the phosphoric acid nozzle 14 has the form of a scan nozzle movable in the chamber 4 in this embodiment.
  • the phosphoric acid nozzle 14 is coupled to the first nozzle moving unit 17, and the first nozzle moving unit 17 moves the phosphoric acid nozzle 14 in at least one of the vertical direction and the horizontal direction.
  • the first nozzle moving unit 17 is a processing position at which the aqueous solution of phosphoric acid discharged from the phosphoric acid nozzle 14 is deposited on the upper surface of the substrate W, and the retraction where the phosphoric acid nozzle 14 is positioned outward of the spin chuck 5 in plan view.
  • the phosphoric acid nozzle 14 is moved between the positions.
  • the processing unit 2 includes an SC1 nozzle 18 that discharges SC1 (a mixed solution containing NH 4 OH and H 2 O 2 ) downward toward the upper surface of the substrate W.
  • the SC1 nozzle 18 is connected to an SC1 pipe 19 that guides the SC1.
  • SC1 valve 20 interposed in the SC1 pipe 19 is opened, SC1 is continuously discharged from the discharge port of the SC1 nozzle 18.
  • the SC1 nozzle 18 has the form of a scan nozzle movable in the chamber 4 in this embodiment.
  • the SC1 nozzle 18 is coupled to the second nozzle moving unit 21.
  • the second nozzle moving unit 21 moves the SC1 nozzle 18 in at least one of the vertical direction and the horizontal direction.
  • the second nozzle moving unit 21 is between the processing position where the SC1 discharged from the SC1 nozzle 18 lands on the upper surface of the substrate W and the retracted position where the SC1 nozzle 18 is located outward of the spin chuck 5 in plan view. To move the SC1 nozzle 18.
  • the processing unit 2 further includes a rinse liquid nozzle 22 that discharges the rinse liquid downward toward the upper surface of the substrate W.
  • the rinse liquid nozzle 22 is connected to a rinse liquid pipe 23 for guiding the rinse liquid.
  • the rinse liquid valve 24 interposed in the rinse liquid pipe 23 is opened, the rinse liquid is continuously discharged downward from the discharge port of the rinse liquid nozzle 22.
  • the rinse solution is, for example, pure water (deionized water).
  • Other examples of the rinse solution are electrolytic ion water, hydrogen water, ozone water, hydrochloric acid water of diluted concentration (for example, about 10 ppm to 100 ppm), and the like.
  • the rinse liquid nozzle 22 is a fixed nozzle that discharges the rinse liquid from the discharge port whose position is fixed.
  • the rinse liquid nozzle 22 is fixed to the bottom of the chamber 4.
  • the processing unit 2 is between the processing position where the rinse liquid discharged from the rinse liquid nozzle 22 lands on the upper surface of the substrate W and the retracted position where the rinse liquid nozzle 22 is located outward of the spin chuck 5 in plan view.
  • the nozzle moving unit for moving the rinse liquid nozzle 22 may be provided.
  • FIG. 2 is a schematic view for explaining the configuration of the phosphoric acid supply system 30 provided in the substrate processing apparatus 1.
  • the phosphoric acid supply system 30 includes a supply tank 31 (tank) storing the phosphoric acid aqueous solution discharged from the phosphoric acid nozzle 14 and a circulation pipe 32 circulating the phosphoric acid aqueous solution in the supply tank 31.
  • the phosphoric acid supply system 30 further includes a pump 33 for feeding the aqueous phosphoric acid solution in the supply tank 31 to the circulation pipe 32, and a heater for heating the aqueous phosphoric acid solution in the middle of the circulation path formed by the supply tank 31 and the circulation pipe 32.
  • the pump 33, the filter 35 and the heater 34 are interposed in the circulation pipe 32.
  • the supply tank 31 is an example of a tank for storing a phosphoric acid aqueous solution.
  • a phosphoric acid pipe 15 as a supply pipe for supplying a phosphoric acid aqueous solution to the phosphoric acid nozzle 14 is connected to a circulation pipe 32.
  • the pump 33 always sends the aqueous phosphoric acid solution in the supply tank 31 to the circulation pipe 32.
  • the phosphoric acid supply system 30 may be provided with a pressurizing device that pushes the aqueous solution of phosphoric acid in the supply tank 31 into the circulation pipe 32 by raising the pressure in the supply tank 31 instead of the pump 33.
  • the pump 33 and the pressurizing device are both examples of a liquid sending device that sends the aqueous solution of phosphoric acid in the supply tank 31 to the circulation pipe 32 and the phosphoric acid pipe 15.
  • the upstream end and the downstream end of the circulation pipe 32 are connected to the supply tank 31.
  • the phosphoric acid aqueous solution is sent from the supply tank 31 to the upstream end of the circulation pipe 32, and returns to the supply tank 31 from the downstream end of the circulation pipe 32.
  • the phosphoric acid aqueous solution in the supply tank 31 circulates through a circulation path.
  • foreign matter contained in the aqueous phosphoric acid solution is removed by the filter 35, and the aqueous phosphoric acid solution is heated by the heater 34.
  • the phosphoric acid aqueous solution in the supply tank 31 is maintained at a constant temperature higher than room temperature (for example, 5 ° C. to 30 ° C.).
  • the temperature of the phosphoric acid aqueous solution heated by the heater 34 may be a boiling point at the concentration (phosphoric acid concentration) of the phosphoric acid aqueous solution, or may be a temperature lower than the boiling point.
  • a branch pipe 36 is connected in the middle of the circulation pipe 32.
  • a silicon concentration meter 37 is interposed in the middle of the branch pipe 36, and the branch pipe 36 branches from the circulation pipe 32 and passes through the silicon concentration meter 37 and then joins the circulation pipe 32.
  • valves 38 and 39 are interposed on both the upstream side and the downstream side of the silicon densitometer 37, respectively.
  • a drain system 40 is provided to drain the aqueous phosphoric acid solution in the supply tank 31.
  • the drain system 40 includes a drain pipe 41 for discharging the phosphoric acid aqueous solution in the supply tank 31 and a drain valve 42 interposed in the drain pipe 41.
  • the drain pipe 41 may be provided with a drain flow control valve 43 for adjusting the discharge flow rate of the phosphoric acid aqueous solution.
  • the drain valve 42 By opening the drain valve 42, the phosphoric acid aqueous solution in the supply tank 31 is discharged to the drain pipe 41. Thereby, the amount of the phosphoric acid aqueous solution in the supply tank 31 can be reduced as needed, or the entire amount of the phosphoric acid aqueous solution in the supply tank 31 can be drained.
  • the plurality of liquid amount sensors 44 include an upper limit sensor 44 h, a lower limit sensor 44 L, and a target sensor 44 t.
  • the upper limit sensor 44 h detects whether the liquid volume of the phosphoric acid aqueous solution in the supply tank 31 is equal to or higher than the upper limit value of the specified liquid volume range.
  • the lower limit sensor 44L detects whether the liquid volume of the phosphoric acid aqueous solution in the supply tank 31 is less than or equal to the lower limit value of the specified liquid volume range.
  • the target sensor 44t detects whether the liquid volume of the phosphoric acid aqueous solution in the supply tank 31 is equal to or higher than the target value between the upper limit value and the lower limit value.
  • the fresh solution replenishment system 50 replenishes the unused phosphoric acid aqueous solution (fresh solution). The new solution is replenished until the volume of the aqueous solution of phosphoric acid in the supply tank 31 reaches a target value.
  • the new solution replenishment system 50 is interposed in the new solution preparation tank 51, the new solution replenishment piping 52 for guiding the unused phosphoric acid aqueous solution from the new solution preparation tank 51 to the supply tank 31, and the new solution replenishment piping 52 New liquid replenishment valve 53, and a pump 54 also interposed in the new liquid replenishment piping 52.
  • a stock solution of phosphoric acid aqueous solution (hereinafter referred to as “phosphoric acid stock solution”) is supplied to the fresh liquid preparation tank 51 through a phosphoric acid stock solution pipe 55.
  • the phosphoric acid stock solution is an aqueous solution of phosphoric acid not containing silicon.
  • the phosphoric acid stock solution pipe 55 is provided with a phosphoric acid stock solution valve 56 for opening and closing the flow path.
  • the silicon concentrate is supplied to the new liquid preparation tank 51 via the silicon concentrate pipe 57.
  • the silicon concentrate pipe 57 is provided with a silicon valve 58 for opening and closing the flow path.
  • the new solution replenishment system 50 further includes a phosphate solution replenishment pipe 59 for supplying the phosphate solution to the supply tank 31.
  • the phosphoric acid stock solution replenishment pipe 59 branches from the phosphoric acid stock solution pipe 55 on the upstream side of the phosphoric acid stock solution valve 56 and is connected to the supply tank 31 without passing through the new liquid preparation tank 51.
  • a phosphate stock solution replenishment valve 60 for opening and closing the flow path is interposed.
  • Integrated flow meters 61 and 62 are interposed in the new solution replenishment piping 52 and the phosphate stock solution replenishment piping 59, respectively.
  • the phosphoric acid stock solution valve 56 By opening the phosphoric acid stock solution valve 56 to supply a fixed amount of phosphoric acid stock solution to the new liquid preparation tank 51, and opening the silicon valve 58 to supply a fixed quantity of silicon concentrate to the new liquid preparation tank 51,
  • the acid stock solution and the silicon concentrate are mixed at a predetermined ratio.
  • the phosphoric acid stock solution and the silicon concentrate are respectively quantified so as to have a predetermined supply amount ratio and supplied to the new liquid preparation tank 51.
  • a phosphoric acid aqueous solution containing silicon of a reference silicon concentration for example, 50 ppm, an example of the first concentration
  • a circulation path 63 circulating through the silicon densitometer 37 is provided to check the silicon concentration as necessary It may be possible.
  • valves 64 and 65 are interposed upstream and downstream of the silicon densitometer 37, respectively.
  • the new solution (unused phosphoric acid aqueous solution containing silicon at a reference silicon concentration) prepared in the new solution preparation tank 51 can be replenished to the supply tank 31.
  • the replenishment amount can be measured by the integrated flow meter 61.
  • the phosphoric acid stock solution replenishment valve 60 the phosphoric acid stock solution (an unused phosphoric acid aqueous solution not containing silicon) can be replenished to the supply tank 31.
  • the replenishment amount can be measured by the integrating flow meter 62.
  • the silicon concentration in the phosphoric acid solution is zero (an example of the second concentration).
  • An aqueous acid solution supply means is configured.
  • secondary phosphoric acid aqueous solution supply means for supplying a phosphoric acid aqueous solution (second phosphoric acid aqueous solution) having a zero concentration (example of the second concentration) is configured by the phosphoric acid stock solution replenishment piping 59 and the phosphoric acid stock solution replenishment valve 60 etc. It is done.
  • the substrate processing apparatus 1 further includes a recovery system 70 for recovering the used aqueous phosphoric acid solution used for processing the substrate W.
  • the recovery system 70 includes a processing cup 10, a recovery pipe 71, and a recovery valve 72.
  • the recovery pipe 71 guides the aqueous solution of phosphoric acid received by the processing cup 10 to the supply tank 31.
  • the recovery valve 72 opens and closes the flow path of the recovery pipe 71.
  • the substrate processing apparatus 1 further includes a drainage system 80 for discarding the processing liquid used for processing the substrate W.
  • the drainage system 80 includes a drainage pipe 81 connected to the processing cup 10 or the recovery pipe 71, and a drainage valve 82 for opening and closing the flow path of the drainage pipe 81.
  • the recovery valve 72 When the recovery valve 72 is opened and the drainage valve 82 is closed, the aqueous phosphoric acid solution received by the processing cup 10 is recovered by the recovery pipe 71 into the supply tank 31. When the spent treatment liquid is discarded, the recovery valve 72 is closed, and the drainage valve 82 is opened. As a result, the phosphoric acid aqueous solution and the other treatment liquids received by the processing cup 10 are discharged to the drainage pipe 81.
  • FIG. 3 is a block diagram for explaining the main electrical configuration of the substrate processing apparatus 1.
  • Control device 3 includes a computer main body 3a and a peripheral device 3b connected to computer main body 3a.
  • the computer main body 3 a includes a processor (CPU) 91 and a main storage device 92.
  • the peripheral device 3b is a communication device for communicating with an external device such as the host computer HC, a reading device 94 for reading information from the removable medium M, an auxiliary storage device 93 for storing the program P executed by the processor 91, various data. And 95.
  • the input device 96 and a display device 97 are connected to the control device 3.
  • the input device 96 is a device operated by an operator such as a user or a maintenance person to input information to the substrate processing apparatus 1.
  • the display device 97 displays various information on the display screen and provides the operator or the like.
  • the input device 96 may be a keyboard, a pointing device, a touch panel or the like.
  • the processor 91 executes the program P stored in the auxiliary storage device 93.
  • the program P in the auxiliary storage device 93 may be installed in the control device 3 in advance.
  • the program P may be read from the removable medium M by the reading device 94 and introduced into the auxiliary storage device 93.
  • the program P may be acquired from the host computer HC or another external device via the communication device 95, and may be introduced into the auxiliary storage device.
  • the auxiliary storage device 93 and the removable medium M are non-volatile memories that retain storage even when power is not supplied.
  • the auxiliary storage device 93 may be, for example, a magnetic storage device such as a hard disk drive.
  • the removable medium M may be an optical disc or a semiconductor memory.
  • the auxiliary storage device 93 and the removable medium M are examples of computer readable recording media in which the program P is recorded.
  • the control device 3 controls the substrate processing apparatus 1 to process the substrate W in accordance with the recipe R specified by the host computer HC.
  • the control device 3 controls the processing unit 2 and each part of the phosphoric acid supply system 30. More specifically, the control device 3 controls the spin motor 9, the guard lifting unit 13, the nozzle moving unit 17, 21, the valves 16, 20, 24, and the like. Further, the control device 3 controls the pumps 33 and 54, the heater 34, the valves 38, 39, 42, 53, 56, 58, 60, 64, 65, 72, and the like. Furthermore, signals from sensors are input to the control device 3.
  • the sensors include a liquid amount sensor 44, a silicon densitometer 37, and integrated flow meters 61 and 62.
  • the auxiliary storage device 93 stores a plurality of recipes R.
  • the recipe R includes information that defines the processing content of the substrate W, the processing conditions, and the processing procedure.
  • the plurality of recipes R differ in at least one of the processing content of the substrate W, the processing conditions, and the processing procedure.
  • Each process of substrate processing is realized by the control device 3 controlling the substrate processing apparatus 1 according to the recipe R. That is, the control device 3 is programmed to execute each process of substrate processing.
  • FIG. 4 is a cross-sectional view showing an example of the substrate W processed by the substrate processing apparatus 1.
  • the substrate W is a silicon wafer having a surface (device formation surface) on which the silicon oxide film Fo and the silicon nitride film Fn are exposed.
  • an aqueous solution of phosphoric acid containing silicon is supplied to such a substrate W, whereby selective etching of the silicon nitride film Fn is performed. That is, the silicon nitride film Fn can be etched at a predetermined etching rate (etching amount per unit time) while suppressing the etching of the silicon oxide film Fo.
  • FIG. 5 is a process diagram for explaining an example of substrate processing performed by the substrate processing apparatus 1.
  • the substrate W to be processed is carried into the chamber 4 by the transfer robot and transferred to the spin chuck 5 (step S1).
  • the control device 3 rotates the spin chuck 5, thereby rotating the substrate W around the vertical rotation axis A1 (step S2).
  • an aqueous solution of phosphoric acid is supplied to the substrate W (step S3). More specifically, the first nozzle moving unit 17 moves the phosphoric acid nozzle 14 to the processing position, and the guard lifting and lowering unit 13 causes any one of the guards 11 to face the substrate W. Thereafter, the phosphoric acid valve 16 is opened, and a phosphoric acid aqueous solution is discharged from the phosphoric acid nozzle 14.
  • the first nozzle moving unit 17 has a central processing position at which the phosphoric acid aqueous solution discharged from the phosphoric acid nozzle 14 contacts the central portion of the upper surface of the substrate W;
  • the phosphoric acid nozzle 14 may be moved between the peripheral processing position where the aqueous phosphoric acid solution discharged from the phosphoric acid nozzle 14 adheres to the upper surface peripheral portion of the substrate W.
  • the phosphoric acid nozzle 14 may be stationary so that the landing position of the phosphoric acid aqueous solution is located at the central portion of the upper surface of the substrate W.
  • the phosphoric acid aqueous solution discharged from the phosphoric acid nozzle 14 is deposited on the upper surface of the substrate W, it flows outward along the upper surface of the rotating substrate W.
  • a liquid film of phosphoric acid aqueous solution covering the entire upper surface of the substrate W is formed, and the phosphoric acid aqueous solution is supplied to the entire upper surface of the substrate W.
  • the entire top surface of the substrate W is uniformly supplied. Thereby, the upper surface of the substrate W is uniformly processed.
  • the phosphoric acid valve 16 is closed, and the discharge of the aqueous phosphoric acid solution from the phosphoric acid valve 16 is stopped. Thereafter, the first nozzle moving unit 17 moves the phosphoric acid valve 16 to the retracted position.
  • the phosphoric acid aqueous solution jumps out of the substrate W by the centrifugal force and is received by the guard 11 facing the substrate W.
  • the aqueous phosphoric acid solution is further guided by the guard 11 to the corresponding cup 12, flows into the recovery pipe 71, and is recovered into the supply tank 31.
  • a first rinse liquid supply process of supplying pure water, which is an example of a rinse liquid, to the upper surface of the substrate W is performed (step S4).
  • the rinse liquid valve 24 is opened, and the rinse liquid nozzle 22 starts discharging the pure water.
  • the pure water deposited on the upper surface of the substrate W flows outward along the upper surface of the rotating substrate W.
  • the phosphoric acid aqueous solution on the substrate W is washed away by the pure water discharged from the rinse liquid nozzle 22. Thereby, a liquid film of pure water covering the upper surface of the substrate W is formed.
  • the rinse liquid valve 24 is closed and the discharge of pure water is stopped.
  • the treatment liquid (mainly rinse liquid) received by the guard 11 and guided to the cup 12 is drained through the drainage pipe 81.
  • an SC1 supply process of supplying SC1 to the substrate W is performed (step S5).
  • the second nozzle moving unit 21 moves the SC1 nozzle 18 to the processing position, and the guard lifting unit 13 makes the guard 11 different from that in the phosphoric acid supply process face the substrate W.
  • the SC1 valve 20 is opened, and the SC1 nozzle 18 starts discharging the SC1.
  • the SC1 nozzle 18 discharges from the central processing position where the SC1 discharged from the SC1 nozzle 18 contacts the center of the upper surface of the substrate W and the SC1 nozzle 18
  • the SC1 nozzle 18 may be moved between the outer peripheral processing position where the SC1 contacts the upper surface outer peripheral portion of the substrate W.
  • the SC1 may be made to stand still so that the liquid deposition position of the SC1 is positioned at the central portion of the upper surface of the substrate W.
  • SC1 discharged from the SC1 nozzle 18 flows along the upper surface of the rotating substrate W after being deposited on the upper surface of the substrate W.
  • a liquid film of SC1 covering the entire top surface of the substrate W is formed, and SC1 is supplied to the entire top surface of the substrate W.
  • the SC 1 supplied to the upper surface of the substrate W jumps out of the substrate W by centrifugal force, is received by the guard 11 facing the substrate W, and is guided to the corresponding cup 12. Similar to the phosphoric acid aqueous solution, the SC1 may be recovered and reused in the SC1 tank (not shown) or may be discarded without recovery.
  • a second rinse liquid supply process of supplying pure water, which is an example of a rinse liquid, to the upper surface of the substrate W is performed (step S6).
  • the rinse liquid valve 24 is opened, and discharge of pure water from the rinse liquid nozzle 22 is started.
  • the pure water deposited on the upper surface of the substrate W flows outward along the upper surface of the rotating substrate W.
  • the SC 1 on the substrate W is washed away by the pure water, and a liquid film of pure water covering the entire upper surface of the substrate W is formed.
  • the rinse liquid valve 24 is closed and the discharge of pure water is stopped.
  • the treatment liquid (mainly rinse liquid) received by the guard 11 and guided to the cup 12 is discarded.
  • step S7 a drying process of drying the substrate W by high-speed rotation of the substrate W is performed (step S7).
  • the spin motor 9 accelerates the rotation of the substrate W, and rotates the substrate W at a rotation speed (eg, several thousand rpm) larger than that in the liquid processing step (S3 to S6). Thereby, the liquid on the substrate W is removed by centrifugal force, and the substrate W is dried.
  • the rotation of the spin motor 9 is stopped (step S8).
  • step S9 an unloading step of unloading the substrate W from the chamber 4 is performed (step S9). Specifically, the guard lifting unit 13 lowers all the guards 11 to the lower position. Thereafter, the transfer robot causes the hand to enter the chamber 4, scoops the processed substrate W from the spin chuck 5, and carries it out of the chamber 4.
  • FIG. 6 is a flowchart for explaining the process related to the supply of the phosphoric acid aqueous solution.
  • the control device 3 opens the phosphoric acid valve 16 and supplies a phosphoric acid aqueous solution to the phosphoric acid nozzle 14 (step S11). Thereby, the phosphoric acid aqueous solution is supplied to the substrate W held by the spin chuck 5.
  • the controller 3 opens the recovery valve 72 and closes the drainage valve 82.
  • the used aqueous phosphoric acid solution supplied to the substrate W is collected into the supply tank 31 via the collection pipe 71 (step S12).
  • the control device 3 determines whether the condition (refilling start condition) to start the replenishment of the new solution to the supply tank 31 is satisfied (step S13).
  • the replenishment start conditions may include liquid volume conditions.
  • One specific example of the fluid amount condition is that the lower limit sensor 44L detects the fluid amount equal to or less than the lower limit value.
  • the replenishment start conditions may also include processing number conditions.
  • One specific example of the processing number condition is that the number of substrates W processed without replenishing the supply tank 31 with a new solution reaches a predetermined number.
  • the replenishment start conditions may include silicon concentration conditions.
  • the control device 3 may determine that the replenishment start condition is satisfied when at least one of the liquid amount condition, the processing number condition, and the silicon concentration condition is satisfied.
  • Control device 3 measures the silicon concentration by, for example, opening valves 38 and 39 at predetermined time intervals (for example, intervals of 10 minutes to several tens of minutes) to sample the phosphoric acid aqueous solution and introduce it into silicon densitometer 37. You may go.
  • the controller 3 determines the amount of liquid to be replenished in order to replenish the new liquid from the new liquid replenishment system 50 to the supply tank 31 (step S14).
  • the total amount of the liquid to be replenished may be, for example, the difference between the lower limit value detected by the lower limit sensor 44L and the target value detected by the target sensor 44t, which is a known value.
  • the liquid amount in the supply tank 31 may be larger than the lower limit value. In such a case, the control device 3 may drain the aqueous phosphoric acid solution in the supply tank 31 until the amount of liquid in the supply tank 31 reaches the lower limit value by opening the drain valve 42.
  • the control device 3 mixes the phosphoric acid aqueous solution in the supply tank 31, the new liquid (the unused phosphoric acid aqueous solution of the reference silicon concentration) prepared in the new liquid preparation tank 51, and the phosphoric acid stock solution to obtain the reference silicon concentration.
  • the replenishment liquid amount is determined so that the phosphoric acid aqueous solution of (adjustment target value) is stored in the supply tank 31 up to the liquid level of the target value.
  • the sum of the replenishment rate of the fresh solution and the replenishment rate of the phosphate stock solution is the total volume to be replenished, and its value is known as described above.
  • the control device 3 can determine the new solution replenishment amount and the phosphate stock solution replenishment amount based thereon. In other words, the ratio between the fresh solution replenishment rate and the phosphate stock solution replenishment rate can be determined.
  • the silicon concentration in the phosphoric acid aqueous solution collected in the supply tank 31 through the collection pipe 71 is higher than the silicon concentration in the phosphoric acid aqueous solution supplied from the phosphoric acid valve 16 to the substrate W. This is because the silicon material (including the silicon compound) constituting the substrate W is eluted in the aqueous phosphoric acid solution.
  • the elution amount varies depending on the type of the substrate W, and varies depending on the processing conditions for the substrate W.
  • the control device 3 can obtain these pieces of information from the recipe R.
  • the silicon concentration in the phosphoric acid aqueous solution in the supply tank 31 increases as the number of processed substrates increases. That is, the silicon concentration in the phosphoric acid aqueous solution depends on the number of treatments.
  • the control device 3 can obtain information on the number of processed substrates by counting the number of processed substrates.
  • the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 also depends on the recovery rate of the phosphoric acid aqueous solution.
  • the recovery rate is the ratio of the amount of phosphoric acid aqueous solution recovered to the supply tank 31 via the recovery pipe 71 to the amount of aqueous phosphoric acid solution discharged from the phosphoric acid nozzle 14.
  • the rinse step part of the phosphoric acid aqueous solution is drained together with the rinse liquid (pure water), so the recovery rate is less than 100%.
  • the controller 3 can obtain information on the recovery rate by referring to the recipe R. Of course, the operator may input information on the recovery rate by operating the input device 96.
  • control device 3 obtains information obtained from the recipe R (elution amount of silicon (type of substrate W and / or substrate processing conditions), recovery rate), information obtained in the process of controlling the substrate processing apparatus 1
  • the silicon concentration in the phosphoric acid aqueous solution at the start of replenishment can be determined from the number of processes and the information input from the input device 96.
  • the silicon concentration in the phosphoric acid aqueous solution collected in the supply tank 31 may be determined by calculation, and the silicon concentration value corresponds to the type of the substrate W, the condition of the substrate processing, the recovery rate, the number of processing, etc. It can also be determined using the attached table. Alternatively, a table may be prepared in which the amount of replenished new solution and the replenished amount of phosphoric acid solution are associated with the type of substrate W, the condition of substrate processing, the recovery rate, the number of treatments, and the like.
  • the control device 3 determines the new solution replenishment amount and the phosphate stock solution replenishment amount (step S14). Then, the control device 3 opens the new solution replenishment valve 53 and drives the pump 54 to replenish the new solution from the new solution preparation tank 51 to the supply tank 31 (step S15). The replenishment amount is measured by the integrated flow meter 61. When the measurement value of the integrated flow meter 61 reaches the new solution replenishment amount (step S16), the control device 3 stops the pump 54 and closes the new solution replenishment valve 53 (step S17). Further, the control device 3 opens the phosphate stock solution replenishment valve 60, and causes the supply tank 31 to be replenished with the phosphate stock solution via the phosphate stock solution replenishment pipe 59 (step S18).
  • the replenishment amount is measured by the integrating flow meter 62.
  • the control device 3 closes the phosphate stock solution replenishment valve 60 to stop the replenishment of the phosphate stock solution (step S20).
  • the silicon nitride film Fn exposed on the surface of the substrate W is selectively etched by processing the substrate W using a phosphoric acid aqueous solution.
  • concentration of silicon contained in the phosphoric acid aqueous solution is controlled to a prescribed silicon concentration range, whereby the etching of the silicon oxide film Fo exposed on the surface of the substrate W can be suppressed, and accordingly, the silicon nitride film Fn
  • the selectivity can be increased.
  • the phosphoric acid aqueous solution is supplied from the supply tank 31 to the phosphoric acid nozzle 14, and is supplied from the phosphoric acid nozzle 14 to the substrate W.
  • the spent phosphoric acid aqueous solution used for processing the substrate W is recovered to the supply tank 31.
  • the predetermined replenishment start condition is satisfied (Step S13: Satisfy)
  • the new solution containing silicon at the reference silicon concentration and the phosphate stock solution having no silicon concentration are replenished to the supply tank 31.
  • the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 can be controlled within the specified silicon concentration range.
  • the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 is defined within a predetermined silicon concentration range (preferably by preparing the new liquid and phosphoric acid stock solution of the reference silicon concentration in advance and supplying only the necessary amount to the supply tank 31 when necessary. Can be adjusted to the standard silicon concentration). Therefore, since the waiting time for replenishing the phosphoric acid aqueous solution to the supply tank 31 is not required, the phosphoric acid aqueous solution having a stable silicon concentration can be supplied to the substrate W without impairing the productivity of the substrate processing.
  • the silicon densitometer 37 is not an essential component, and a configuration for monitoring the silicon concentration in the phosphoric acid aqueous solution in real time is not necessary. Therefore, a phosphoric acid aqueous solution having a stable silicon concentration can be supplied to the substrate W with an inexpensive configuration.
  • the new solution supplied from the new solution preparation tank 51 to the supply tank 31 has a silicon concentration (more specifically, a reference silicon concentration) within the specified silicon concentration range. Therefore, the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 can be easily derived to a value within the specified silicon concentration range by the supply of the new solution. Moreover, when the phosphoric acid aqueous solution is stored in the supply tank 31 first, only the new liquid prepared in the new liquid preparation tank 51 may be supplied to the supply tank 31. As a result, the phosphoric acid aqueous solution stored in the supply tank 31 can be used as it is for processing the substrate W without passing through the waiting time for achieving uniform concentration.
  • the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 is derived to a value within the specified silicon concentration range.
  • Cheap when the substrate W contains silicon, the silicon of the substrate material is eluted in the aqueous phosphoric acid solution by supplying the aqueous phosphoric acid solution to the substrate W, so the concentration of the aqueous phosphoric acid solution recovered in the supply tank 31 Is higher than before the substrate W is supplied.
  • the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 is defined in the specified silicon concentration range by supplying the phosphoric acid stock solution containing silicon to the supply tank 31 at a concentration (zero in this embodiment) lower than the specified silicon concentration range. It can easily lead to
  • the replenishment amount of the new solution and the phosphate stock solution to the supply tank 31 is determined based on the type of the substrate W. Based on the type of the substrate W, fluctuations in the silicon concentration in the phosphoric acid aqueous solution before and after substrate processing can be predicted. Therefore, the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 can be appropriately adjusted by determining the replenishment amounts of the new solution and the phosphoric acid stock solution based on the type of the substrate W.
  • the supply tank is specified by specifying the amount of silicon eluted from the substrate W according to the type of the substrate W and the like, and determining each replenishment amount of the new solution and the phosphate stock solution based on the specified silicon elution amount.
  • the silicon concentration of the phosphoric acid aqueous solution in 31 can be appropriately adjusted.
  • the supply amount of the new solution and the phosphoric acid stock solution is based on the recovery rate of the phosphoric acid aqueous solution recovered in the supply tank 31 among the phosphoric acid aqueous solution supplied to the substrate W from the phosphoric acid nozzle 14. It is determined.
  • the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 can be adjusted to the defined silicon concentration range while replenishing the supply tank 31 with the necessary amount of phosphoric acid aqueous solution.
  • the replenishment amounts of the new solution and the phosphoric acid stock solution are determined based on the number (the number of processes) of the substrate W processed by the phosphoric acid aqueous solution supplied from the phosphoric acid nozzle 14. Thereby, the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 can be appropriately adjusted.
  • the above-described replenishment start condition includes the liquid amount condition regarding the liquid amount stored in the supply tank 31.
  • the new solution and the phosphate stock solution are replenished with the decrease in the amount of liquid stored in the supply tank 31 to the lower limit value as a trigger.
  • the new solution and the phosphoric acid stock solution are replenished to recover the amount of liquid, and at the same time, the silicon concentration is adjusted.
  • the replenishment start condition includes the processing number condition regarding the number of substrates W processed by the phosphoric acid aqueous solution supplied from the phosphoric acid nozzle 14. That is, when the number of processed substrates W reaches a predetermined number, the new solution and the phosphoric acid stock solution are replenished to the supply tank 31 using this as a trigger.
  • the substrate W can be treated with a stable silicon concentration phosphoric acid aqueous solution.
  • the replenishment start condition includes the silicon concentration condition regarding the silicon concentration in the phosphoric acid aqueous solution supplied from the supply tank 31 toward the phosphoric acid nozzle 14.
  • the silicon concentration in the phosphoric acid aqueous solution whose circulation temperature is regulated through the circulation pipe 32 is periodically measured by the silicon concentration meter 37.
  • the new solution and the phosphoric acid stock solution are replenished to the supply tank 31 with that as a trigger.
  • the silicon concentration of the phosphoric acid aqueous solution in the supply tank 31 is recovered to the specified silicon concentration range, so that the substrate W can be processed with the stable silicon concentration phosphoric acid aqueous solution.
  • the substrates W are held horizontally and processed by the spin chuck 5 one by one.
  • the integrated solution flow rate to the supply tank 31 is measured by the integrated flow meter 61, and the integrated solution flow rate to the supply tank 31 is measured by the integrated flow meter 62.
  • the control device 3 manages the new solution replenishment amount and the phosphate stock solution replenishment amount based on the measurement results of the integrated flow meters 61 and 62. Thereby, the silicon concentration in the phosphoric acid aqueous solution in the supply tank 31 can be accurately adjusted.
  • FIG. 7 is a schematic view for explaining the configuration of the substrate processing apparatus 1 according to the second embodiment of the present invention, and mainly shows the configuration of the phosphoric acid supply system 30. As shown in FIG. In FIG. 7, corresponding parts in FIG. 2 are indicated by the same reference numerals.
  • the phosphoric acid supply system 30 of the substrate processing apparatus 1 includes a first recovery tank 90A and a second recovery tank 90B.
  • the recovery pipe 71 is branched into two recovery branch pipes 71A and 71B.
  • the first recovery branch pipe 71A is connected to the first recovery tank 90A
  • the second recovery branch pipe 71B is connected to the second recovery tank 90B.
  • a first recovery valve 72A and a second recovery valve 72B are interposed in the first recovery branch pipe 71A and the second recovery branch pipe 71B.
  • the controller 3 controls the opening and closing of the first and second recovery valves 72A and 72B to select the recovery destination of the used aqueous phosphoric acid solution as one of the first recovery tank 90A and the second recovery tank 90B. Yes (collection destination selection process).
  • the phosphoric acid aqueous solution stored in the first recovery tank 90A and the second recovery tank 90B is replenished to the supply tank 31 via the replenishment pipe 100 (preparation liquid supply pipe).
  • the downstream end of the refilling pipe 100 is connected to the supply tank 31.
  • the upstream end of the refilling pipe 100 branches into a first branch pipe 100A and a second branch pipe 100B.
  • the first branch pipe 100A is connected to the first recovery tank 90A
  • the second branch pipe 100B is connected to the second recovery tank 90B.
  • a first refill valve 101A and a second refill valve 101B are interposed in the first branch pipe 100A and the second branch pipe 100B.
  • a pump 102 and a heater 103 are interposed in the refilling pipe 100.
  • the phosphoric acid aqueous solution can be supplied from the first recovery tank 90A to the supply tank 31 by driving the pump 102 in a state where the first replenishment valve 101A is opened and the second replenishment valve 101B is closed.
  • the phosphoric acid aqueous solution can be supplied from the second recovery tank 90B to the supply tank 31 by driving the pump 102 with the first replenishment valve 101A closed and the second replenishment valve 101B opened.
  • the aqueous phosphoric acid solution is heated by the heater 103. Therefore, the temperature-controlled phosphoric acid aqueous solution can be supplied to the supply tank 31.
  • the control device 3 controls the opening and closing of the first and second replenishment valves 101A and 101B to make the phosphoric acid aqueous solution replenishment source to the supply tank 31 one of the first recovery tank 90A and the second recovery tank 90B. Select to More specifically, the control device 3 selects the recovery tank 90A, 90B which is not selected as the recovery destination of the used aqueous phosphoric acid solution as a replenishment source to the supply tank 31 (replenishment source selection step).
  • the new solution replenishment piping 52 through which the new solution supplied from the new solution preparation tank 51 flows is branched into a first branch pipe 52A and a second branch pipe 52B.
  • the first branch pipe 52A is connected to the first recovery tank 90A
  • the second branch pipe 52B is connected to the second recovery tank 90B.
  • a first fresh fluid replenishment valve 53A and a second fresh fluid replenishment valve 53B are interposed in the first branch pipe 52A and the second branch pipe 52B, respectively.
  • the new solution (unused phosphoric acid aqueous solution of the reference silicon concentration) prepared in the new solution preparation tank 51 can be supplied to the first recovery tank 90A.
  • the new solution prepared in the new solution preparation tank 51 can be supplied to the second recovery tank 90B by opening the second new solution replenishment valve 53B.
  • the phosphate stock solution replenishment pipe 59 branches into a first branch pipe 59A and a second branch pipe 59B.
  • the first branch pipe 59A is connected to the first recovery tank 90A
  • the second branch pipe 59B is connected to the second recovery tank 90B.
  • a first phosphate stock solution replenishment valve 60A and a second phosphate stock solution replenishment valve 60B are respectively interposed in the first branch pipe 59A and the second branch pipe 59B.
  • the control device 3 controls the opening and closing of the first and second new solution refilling valves 53A, 53B and the first and second phosphate stock solution refilling valves 60A, 60B, thereby providing a replacement destination of the new solution and the phosphate solution.
  • One of the first recovery tank 90A and the second recovery tank 90B is selected. More specifically, the control device 3 selects the recovery tanks 90A and 90B selected as the recovery destinations of the used aqueous phosphoric acid solution as the replenishment destinations of the new solution and the phosphate stock solution (supply destination selection process).
  • First drain systems 45A and 45B are provided to drain the aqueous phosphoric acid solutions in the first and second recovery tanks 90A and 90B, respectively.
  • the drain systems 45A, 45B include drain pipes 46A, 46B for discharging the phosphoric acid aqueous solution in the recovery tanks 90A, 90B, and drain valves 47A, 47B interposed in the drain pipes 46A, 46B.
  • a drain flow rate adjustment valve for adjusting the discharge flow rate of the phosphoric acid aqueous solution may be interposed in the drain pipes 46A and 46B.
  • the phosphoric acid aqueous solution in the collection tanks 90A and 90B is discharged to the drain pipes 46A and 46B.
  • the amount of phosphoric acid aqueous solution in the recovery tank 90A, 90B can be reduced as needed, or the entire amount of phosphoric acid aqueous solution in the recovery tank 90A, 90B can be drained.
  • the lower limit liquid amount sensors 75A and 75B In order to detect the amount of liquid stored in the first and second collection tanks 90A and 90B, the lower limit liquid amount sensors 75A and 75B, the collection stop liquid amount sensors 76A and 76B, and the target liquid amount sensors 77A and 77B are provided. It is done.
  • the lower limit liquid amount sensor 75A, 75B detects that the lower limit liquid amount has been reached when the amount of liquid in the recovery tank 90A, 90B decreases due to the supply of the phosphoric acid aqueous solution from the recovery tank 90A, 90B to the supply tank 31. Do.
  • the recovery stop fluid amount sensors 76A and 76B detect that the upper limit fluid amount has been reached when the used phosphoric acid aqueous solution is recovered in the recovery tanks 90A and 90B and the liquid volume in the recovery tanks 90A and 90B increases. Do.
  • the target fluid volume sensors 77A and 77B stop the replenishment when replenishing the recovery tanks 90A and 90B with an unused phosphoric acid aqueous solution from the new solution replenishment system 50 to increase the volume in the recovery tanks 90A and 90B. It detects that the liquid volume (target liquid volume) to be reached has been reached.
  • a valve 29 is interposed in the circulation pipe 32.
  • a valve 29 may be provided also in the configuration shown in FIG.
  • the valve 29 is opened and closed by the controller 3.
  • FIG. 8 is a block diagram for explaining the electrical configuration of the substrate processing apparatus 1 having the configuration of FIG. In FIG. 8, the corresponding parts in FIG. 3 described above are indicated by the same reference numerals.
  • the controller 3 controls the processing unit 2 and the phosphoric acid supply system 30. With regard to the phosphoric acid supply system 30, the controller 3 controls the pumps 33, 54, 102 and controls the heaters 34, 103 so that the valves 38, 39, 42, 53A, 53B, 56, 58, 60A, 60B, 64. , 65, 72A, 72B.
  • an output signal of the liquid amount sensor 44 of the supply tank 31 an output signal of the densitometer 37, an output signal of the integrating flowmeter 61, 62, and a liquid amount sensor 75A, 75B of the collection tank 90A, 90B.
  • 76A, 76B, 77A, 77B are input.
  • FIG. 9, FIG. 10 and FIG. 11 are flowcharts for explaining the process related to the supply of the phosphoric acid aqueous solution.
  • FIG. 9 shows an operation related to supplying the aqueous phosphoric acid solution to the substrate W and replenishing the aqueous phosphoric acid solution to the supply tank 31, and
  • FIG. 11 shows an operation relating to the replenishment of the new solution to the recovery tank 90A, 90B.
  • the control device 3 opens the phosphoric acid valve 16 and supplies a phosphoric acid aqueous solution to the phosphoric acid nozzle 14 (step S21). Thereby, the phosphoric acid aqueous solution is supplied to the substrate W held by the spin chuck 5. By the supply of the phosphoric acid aqueous solution, the liquid amount of the phosphoric acid aqueous solution in the supply tank 31 decreases. Then, when it is detected by the lower limit sensor 44L that the liquid amount of the phosphoric acid aqueous solution in the supply tank 31 has become the lower limit value (step S22: YES), the control device 3 is selected as the phosphoric acid aqueous solution replenishment source.
  • the phosphoric acid aqueous solution is replenished to the supply tank 31 from any one of the recovery tanks 90A and 90B (step S23). That is, the control device 3 opens the replenishment valves 101A and 101B corresponding to any one of the recovery tanks 90A and 90B selected as the replenishment source, and drives the pump 102.
  • the control device 3 ends the replenishment operation (step S24) S25). By repeating the same operation, the liquid volume of the phosphoric acid aqueous solution in the supply tank 31 is maintained in the appropriate range between the lower limit value and the target value.
  • control device 3 selects the recovery destination of the used aqueous phosphoric acid solution used for substrate processing as one of the recovery tanks 90A and 90B (step S31).
  • the other is selected as a phosphoric acid aqueous solution replenishment source to the supply tank 31 (step S32).
  • the recovery valves 72A and 72B corresponding to the recovery reservoirs 90A and 90B selected as the recovery destination are opened, and the recovery valves 72A and 72B corresponding to the recovery reservoirs 90A and 90B not selected as the recovery destination are closed.
  • the replenishment valves 101A and 101B corresponding to the recovery tanks 90A and 90B selected as the phosphoric acid aqueous solution replenishment source are opened.
  • the replenishment valves 101A and 101B corresponding to the recovery tanks 90A and 90B which are not selected as the phosphoric acid aqueous solution replenishment source are kept closed.
  • the control device 3 further detects that the lower limit liquid amount sensor 75A, 75B corresponding to the collection tank 90A, 90B selected as the replenishment source has reduced the liquid amount of the collection tank 90A, 90B to the lower limit liquid amount (Ste S33: YES), switching between the recovery destination and the phosphoric acid aqueous solution replenishment source (steps S31 and S32). That is, the collection tank 90A, 90B in which the liquid volume has decreased to the lower limit liquid volume is selected as the collection destination (step S31), and the other collection tank 90A, 90B is selected as the phosphoric acid aqueous solution replenishment source (step S32).
  • the roles of the first recovery tank 90A and the second recovery tank 90B are alternately switched between the recovery destination and the phosphoric acid aqueous solution replenishment source, triggered by a decrease in liquid volume.
  • the control device 3 determines whether or not replenishment of new solution to the collection tank 90A, 90B selected as the collection destination should be started (step S41). Specifically, the control device 3 determines whether the condition (replenishment start condition) to start the replenishment of the new solution to the collection tank 90A, 90B is satisfied.
  • the replenishment start conditions may include liquid volume conditions (recovery liquid volume conditions). In one specific example of the liquid amount condition, the amount of collected liquid stored in the collection tank 90A, 90B selected as the collection destination increases, and the corresponding collected stop liquid amount sensor 76A, 76B detects the amount of collected stop liquid It is.
  • the replenishment start conditions may also include processing number conditions.
  • the processing number condition is that the number of substrates W processed without replenishing the recovery tank 90A, 90B with a new solution reaches a predetermined number.
  • the replenishment start conditions may include silicon concentration conditions.
  • the silicon concentration condition is that the silicon concentration in the phosphoric acid aqueous solution supplied from the supply tank 31 toward the phosphoric acid nozzle 14 reaches a predetermined concentration.
  • the control device 3 may determine that the replenishment start condition is satisfied when at least one of the liquid amount condition, the processing number condition, and the silicon concentration condition is satisfied.
  • step S41 satisfaction
  • the control device 3 stops the recovery operation (step S42). That is, the control device 3 closes the recovery valves 72A and 72B corresponding to the recovery tanks 90A and 90B selected as recovery destinations, and opens the drainage valve 82.
  • control device 3 determines the amount of liquid to be replenished in order to replenish the new solution from the new solution replenishment system 50 to the recovery tank 90A, 90B of the recovery destination (step S43).
  • the total amount of the fluid to be replenished is, for example, the recovery stop fluid amount detected by the recovery stop fluid amount sensor 76A, 76B of the recovery tank 90A, 90B of the recovery destination and the target fluid amount detected by the target fluid amount sensor 77A, 77B. It may be a difference, which is a known value.
  • the replenishment start condition is satisfied by satisfying the processing number condition or the silicon concentration condition, the liquid amount in the collection tanks 90A and 90B of the collection destination may be larger than the recovery stop liquid amount.
  • control device 3 opens the corresponding drain valves 47A and 47B, and the phosphorus in the collection tanks 90A and 90B until the liquid quantity in the collection tanks 90A and 90B reaches the collection stop liquid quantity.
  • the aqueous acid solution may be drained.
  • the control device 3 controls the phosphoric acid aqueous solution in the recovery tank 90A, 90B selected as the recovery destination, the new solution (unused phosphoric acid aqueous solution with reference silicon concentration) prepared in the new solution mixing tank 51, and the phosphoric acid stock solution
  • the amount of replenishing liquid is determined so that the phosphoric acid aqueous solution of the reference silicon concentration (adjustment target value) is stored in the collection tanks 90A and 90B up to the target liquid volume by mixing.
  • the sum of the fresh solution replacement amount and the phosphate stock solution replacement amount is the total amount of solution replenished, and its value is known as described above.
  • the control device 3 can determine the new solution replenishment amount and the phosphate stock solution replenishment amount based thereon. In other words, the ratio between the fresh solution replenishment rate and the phosphate stock solution replenishment rate can be determined.
  • the silicon concentration in the phosphoric acid aqueous solution recovered and stored in the recovery tanks 90A and 90B can be predicted based on the recipe and the number of processed wafers. This is as already described in relation to the first embodiment.
  • the silicon concentration may be obtained by calculation, or a table in which the silicon concentration value is associated with the type of substrate W, substrate processing conditions, recovery rate, number of processing, etc. It can also be determined using. Alternatively, a table may be prepared in which the amount of replenished new solution and the replenished amount of phosphoric acid solution are associated with the type of substrate W, the condition of substrate processing, the recovery rate, the number of treatments, and the like.
  • the control device 3 determines the new solution replenishment amount and the phosphate stock solution replenishment amount (step S43). Then, the control device 3 opens the replenishment valves 53A and 53B corresponding to the recovery tanks 90A and 90B selected as the recovery destination, drives the pump 54, and transfers the new liquid preparation tank 51 to the recovery tanks 90A and 90B. And replenish the new solution (step S44).
  • the replenishment amount is measured by the integrated flow meter 61.
  • the control device 3 stops the pump 54 and closes the replenishment valves 53A and 53B (step S46).
  • control device 3 opens the phosphate stock solution replenishment valves 60A and 60B corresponding to the recovery tanks 90A and 90B selected as the recovery destination, and transfers them to the recovery tanks 90A and 90B through the phosphate stock solution pipe 55.
  • the phosphate stock solution is replenished (step S47).
  • the replenishment amount is measured by the integrating flow meter 62.
  • the controller 3 closes the first phosphate stock solution replenishment valve 60A to stop the replenishment of the phosphate stock solution ( Step S49).
  • the phosphoric acid aqueous solution of the reference silicon concentration can be prepared. Since the recovery destination and the phosphoric acid aqueous solution replenishment source are alternately switched as described above, the phosphoric acid aqueous solution preparation operation by the new solution replenishment to the first and second recovery tanks 90A and 90B is alternately executed. .
  • the tank for storing the phosphoric acid aqueous solution is the first and second collecting tanks 90A, through which the phosphoric acid aqueous solution used for the substrate processing is guided through the collecting pipe 71, 90B and a supply tank 31 to which a phosphoric acid aqueous solution stored in the first and second recovery tanks 90A and 90B is supplied via a replenishment pipe 100. Then, the phosphoric acid aqueous solution stored in the supply tank 31 is supplied to the phosphoric acid nozzle 14 through the phosphoric acid pipe 15.
  • the fresh solution replenishment system 50 supplies unused phosphoric acid aqueous solution (fresh solution and phosphoric acid stock solution) to the recovery tanks 90A and 90B.
  • the adjustment of the silicon concentration in the phosphoric acid aqueous solution is performed in the recovery tanks 90A and 90B, and the phosphoric acid aqueous solution whose silicon concentration has been adjusted is sent from the recovery tanks 90A and 90B to the supply tank 31 via the replenishment piping 100. Therefore, the silicon concentration in the phosphoric acid aqueous solution in the supply tank 31 is stable because it is not affected by the liquid recovery. As a result, it is possible to supply a phosphoric acid aqueous solution having a more stable silicon concentration to the substrate W from the phosphoric acid nozzle 14.
  • one of the first recovery tank 90A and the second recovery tank 90B is selected as a phosphoric acid aqueous solution replenishment source to the supply tank 31, and the other is selected as a recovery destination of the used phosphoric acid aqueous solution. Ru.
  • the phosphoric acid aqueous solution whose silicon concentration has been adjusted can be supplied to the supply tank 31 without any delay, the supply of the phosphoric acid aqueous solution to the substrate W is not delayed. Thereby, the productivity of substrate processing can be enhanced.
  • the new solution and the phosphoric acid stock solution are supplied to the recovered phosphoric acid aqueous solution to adjust the silicon concentration.
  • the silicon concentration in the phosphoric acid aqueous solution in the recovery tanks 90A and 90B for supplying the phosphoric acid aqueous solution to the supply tank 31 is stable, the silicon concentration in the phosphoric acid aqueous solution in the supply tank 31 can be stably maintained. Thereby, the silicon concentration in the phosphoric acid aqueous solution used for substrate processing is further stabilized.
  • FIG. 12 is a schematic view for explaining the configuration of a substrate processing apparatus 1 according to a third embodiment of the present invention.
  • the new solution replenishment system 50 includes a first new solution preparation tank 51 and a second new solution preparation tank 111.
  • a phosphoric acid stock solution is supplied to the first fresh liquid preparation tank 51 from the phosphoric acid stock solution pipe 55 via the first phosphoric acid stock solution valve 56, and a second phosphoric acid stock solution valve 112 is supplied to the second fresh liquid preparation tank 111.
  • the phosphate stock solution is supplied from the phosphate stock solution pipe 113 via the
  • the silicon concentrate is supplied to the first new liquid preparation tank 51 from the silicon concentrate pipe 57 via the first silicon valve 58, and the second new liquid preparation tank 111 is provided with the second silicon valve 114.
  • the silicon concentrate is supplied from the silicon concentrate pipe 115.
  • the first new liquid preparation tank 51 is connected to the new liquid replenishment piping 52 via the first new liquid replenishment source selection valve 121.
  • the second new liquid preparation tank 111 is connected to the new liquid replenishment piping 52 via the second new liquid replenishment source valve 122.
  • the second fresh solution preparation tank 111, the second fresh solution replenishment source valve 122, the pump 54, and the fresh solution replenishment valves 53A and 53B constitute a tertiary phosphoric acid aqueous solution supply means.
  • the control device 3 controls the opening and closing of the valves 112, 114, 121 and 122 described above.
  • unused phosphoric acid aqueous solution to which silicon is added is supplied from the first new liquid preparation tank 51 and / or the second new liquid preparation tank 111 to the first recovery tank 90A and the second recovery tank 90B. can do.
  • the controller 3 prepares, for example, a phosphoric acid aqueous solution having a silicon concentration (an example of the first concentration) lower than the reference silicon concentration in the first new liquid preparation tank 51. Further, the control device 3 prepares a phosphoric acid aqueous solution having a reference silicon concentration (an example of the third concentration) in the second new liquid preparation tank 111.
  • the second new liquid replenishment source selection valve 122 is opened, the first new liquid replenishment source selection valve 121 is closed, and the second liquid preparation tank 111 is opened.
  • a phosphoric acid aqueous solution (fresh solution) having a reference silicon concentration is supplied and stored in one of the recovery tanks 90A and 90B (for example, the first recovery tank 90A). Then, a phosphoric acid aqueous solution having the reference silicon concentration is supplied from the first recovery tank 90A to the supply tank 31, and the phosphoric acid aqueous solution is used for substrate processing.
  • the used aqueous phosphoric acid solution is recovered in the other of the recovery tanks 90A and 90B (for example, the second recovery tank 90B).
  • the control device 3 opens the first new solution replenishment source selection valve 121 and closes the second new solution replenishment source selection valve 122 . Thereby, the control device 3 supplies the new solution having a silicon concentration lower than the reference silicon concentration from the first new solution preparation tank 51 to the second recovery tank 90B.
  • the silicon concentration in the used phosphoric acid aqueous solution is higher than the reference silicon concentration, the silicon concentration of the phosphoric acid aqueous solution in the second recovery tank 90B can be easily adjusted by mixing the phosphoric acid aqueous solution having a low silicon concentration. it can.
  • the new solution of the reference silicon concentration is replenished from the second new solution mixing tank 111 up to the predetermined number of processed sheets, and when the predetermined number of processed sheets is exceeded, the new liquid of low silicon concentration is extracted from the first new solution mixing tank 51. May be replenished.
  • the silicon concentration of the phosphoric acid aqueous solution in the recovery tank 90A, 90B is measured, and depending on the measurement result, the first new solution mixing tank 51 or the second new solution mixing tank 111 Either may be selected as a new solution replenishment source.
  • either the first new liquid preparation tank 51 or the second new liquid preparation tank 111 may be selected as a new liquid replenishment source.
  • a new solution with a silicon concentration larger than zero and smaller than the reference silicon concentration is prepared in the first new solution mixing tank 51, and a new solution with the reference silicon concentration is the second new solution mixing tank 111.
  • the silicon concentration adjustment range of the phosphoric acid aqueous solution in the recovery tanks 90A and 90B can be increased.
  • the present invention can also be practiced in other forms.
  • a phosphoric acid aqueous solution of reference silicon concentration a zero concentration phosphoric acid aqueous solution (phosphoric acid stock solution), and
  • the phosphoric acid aqueous solution having a silicon concentration lower than the reference silicon concentration is exemplified.
  • phosphoric acid aqueous solution of silicon concentration other than these may be used.
  • the configuration in which two recovery tanks are provided is shown.
  • the configuration may include one recovery tank, or may include three or more recovery tanks.
  • by providing a plurality of (two or more) recovery tanks it is possible to distinguish the recovery tank which is the recovery destination of the used aqueous phosphoric acid solution and the recovery tank which is the replenishment source to the supply tank.
  • an aqueous solution of phosphoric acid having a stable silicon concentration can be supplied without failure.
  • Reference Signs List 1 substrate processing apparatus 2 processing unit 3 controller 5 spin chuck 9 spin motor 10 processing cup 12 cup 14 phosphoric acid nozzle 15 phosphoric acid piping 16 phosphoric acid valve 30 phosphoric acid supply system 31 supply tank (tank) 33 pump 37 silicon densitometer 44 liquid level sensor 44h upper limit sensor 44L lower limit sensor 44t target sensor 50 new solution replenishment system 51 new solution mixing tank 52 new solution replenishment piping 53 new solution replenishment valve 53A first solution replenishment valve 53B second solution Liquid refilling valve 54 Pump 55 Phosphoric acid stock piping 56 Phosphoric acid stock piping 57 Silicon concentrate piping 58 Silicon valve 59 Phosphoric acid stock refilling piping 60 Phosphate stock solution refilling valve 60A Primary phosphate stock solution refilling valve 60B Secondary phosphate stock replenishment Valve 61 integrated flow meter 62 integrated flow meter 70 collection system 71 collection piping 72 collection valve 72A first collection valve 72B second collection valve 75A, 75B lower limit liquid volume sensor 76A, 76B collection stop liquid

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