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WO2018123193A1 - Dispositif de fabrication de liquide dilué et procédé de fabrication de liquide dilué - Google Patents

Dispositif de fabrication de liquide dilué et procédé de fabrication de liquide dilué Download PDF

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Publication number
WO2018123193A1
WO2018123193A1 PCT/JP2017/036436 JP2017036436W WO2018123193A1 WO 2018123193 A1 WO2018123193 A1 WO 2018123193A1 JP 2017036436 W JP2017036436 W JP 2017036436W WO 2018123193 A1 WO2018123193 A1 WO 2018123193A1
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WO
WIPO (PCT)
Prior art keywords
liquid
tank
pipe
pressure
dilution
Prior art date
Application number
PCT/JP2017/036436
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English (en)
Japanese (ja)
Inventor
山下　幸福
翔太 森野
山中　弘次
Original Assignee
オルガノ株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2016254939A external-priority patent/JP6777534B2/ja
Priority claimed from JP2016254938A external-priority patent/JP6777533B2/ja
Priority claimed from JP2016254940A external-priority patent/JP6738726B2/ja
Application filed by オルガノ株式会社 filed Critical オルガノ株式会社
Priority to CN201780066541.6A priority Critical patent/CN109890494B/zh
Priority to KR1020197015953A priority patent/KR102275626B1/ko
Publication of WO2018123193A1 publication Critical patent/WO2018123193A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F21/00—Dissolving
    • B01F21/20—Dissolving using flow mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F21/00—Dissolving
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/405—Methods of mixing liquids with liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/22—Control or regulation
    • B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
    • B01F35/2213—Pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/80—Forming a predetermined ratio of the substances to be mixed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting

Definitions

  • the present invention relates to a diluent manufacturing apparatus and a diluent manufacturing method.
  • ultrapure water from which impurities are highly removed is used as a cleaning liquid for cleaning electronic components such as semiconductor wafers and glass substrates.
  • the use of ultrapure water having a high specific resistance value tends to generate static electricity during cleaning, which may cause electrostatic breakdown of the insulating film and reattachment of fine particles.
  • chemical solutions such as ammonia water and carbonated water have been added to ultra-pure water with high accuracy for the purpose of adjusting the specific resistance value (conductivity) to a predetermined range and suppressing the generation of static electricity.
  • the diluted solution adjusted to a predetermined concentration is used.
  • Patent Document 1 discloses, as such a diluent manufacturing apparatus, a first pipe for supplying ultrapure water, a tank for storing a chemical solution, and a second pipe for connecting the tank and the first pipe. And a pressure regulator for adjusting the pressure in the tank, and the chemical solution in the tank is pumped through the second pipe by the pressure regulator and added to the ultrapure water in the first pipe to produce a diluted liquid.
  • a manufacturing apparatus is described. According to this manufacturing apparatus, the amount of chemical solution added can be adjusted with high accuracy by appropriately controlling the pressure in the tank based on the measured values of the flow rate of the ultrapure water or diluent and the concentration of the diluent. As a result, a diluted solution adjusted to a predetermined concentration can be produced.
  • the diluted liquid adjusted to a predetermined concentration is continuously and stably used. It is required to supply points.
  • the manufacturing apparatus described in Patent Document 1 when the chemical liquid in the tank becomes empty, the operation of the apparatus is stopped, the pressure in the tank is released and the chemical liquid is replenished, or the chemical liquid is filled. It is necessary to change to another tank. In such a case, it may take time for the concentration of the diluted solution to be stabilized after the operation of the apparatus is resumed.
  • the chemical liquid is replenished to the tank while the chemical liquid is continuously supplied from the tank before the chemical liquid in the tank becomes empty.
  • a replenishment method is performed by controlling the inside of the tank to be pressurized with the pressurizing gas, the supply of the chemical from the tank leads to disturbance of the pressure control in the tank, and the diluted liquid produced. It leads to destabilizing the concentration.
  • an object of the present invention is to provide a diluent manufacturing apparatus and a diluent manufacturing method capable of continuously and stably manufacturing a diluent adjusted to a predetermined concentration.
  • the diluent manufacturing apparatus of the present invention manufactures a second liquid diluent by adding the second liquid to the first liquid, and uses the diluent as a use point.
  • a pressure adjusting unit that adjusts the pressure in the second pipe and the first tank, the pressure supplying the first liquid by pumping the second liquid in the first tank through the second pipe Based on the adjustment unit and the measured value of the flow rate of the first liquid or dilution liquid flowing in the first pipe and the concentration of the dilution liquid, the pressure adjustment unit adjusts the concentration of the dilution liquid to a predetermined concentration.
  • a control unit that adjusts the amount of the second liquid added to the first liquid.
  • the dilution liquid manufacturing apparatus of the present invention includes a second tank that is connected in series to the first tank and temporarily stores the second liquid that is replenished to the first tank.
  • the second tank is connected in parallel to the first tank and stores the second liquid supplied to the first pipe instead of the first tank.
  • the method for producing a diluent according to the present invention is a method for producing a diluent that produces a diluent of the second liquid by adding the second liquid to the first liquid and supplies the diluent to the use point.
  • the first liquid is supplied to the first pipe and the pressure in the first tank for storing the second liquid is adjusted to connect the first tank and the first pipe.
  • the method for producing a diluent according to the present invention includes a step of temporarily storing a second liquid in a second tank connected in series to the first tank, and a liquid in the first tank.
  • a diluent adjusted to a predetermined concentration can be continuously and stably produced.
  • FIG. 2 is a graph plotting the conductivity of dilute ammonia water against the amount of ammonia water added in Example 1.
  • FIG. It is a graph which shows the time change of the flow volume of the 1st liquid in Example 2, the pressure in a 1st tank, and the electrical conductivity of diluted ammonia water. It is a graph which shows the time change of the flow volume of the 1st liquid, the pressure in a 1st tank, and the electrical conductivity of diluted ammonia water in a comparative example.
  • FIG. 1 is a schematic configuration diagram of a diluent manufacturing apparatus according to the first embodiment of the present invention. Note that the illustrated configuration is merely an example, and it is needless to say that the configuration can be appropriately changed according to the use purpose, application, and required performance of the apparatus, for example, by adding a valve or a filter.
  • the dilution liquid manufacturing apparatus 10 includes a first pipe 11 that supplies a first liquid, two tanks 12a and 12b that store a second liquid, two tanks 12a and 12b, and a first pipe 11. And a plurality of second pipes 13 connected in parallel to each other.
  • the second liquid is a chemical liquid to be diluted
  • the first liquid is a dilution medium for diluting the second liquid. Therefore, the diluent manufacturing apparatus 10 manufactures the second liquid diluent by adding the second liquid to the first liquid flowing through the first pipe 11 through the second pipe 13.
  • the diluted solution is supplied to the use point 1 through the first pipe 11.
  • the type of the first liquid is not particularly limited, and ultrapure water, pure water, water in which an electrolyte or gas is dissolved, or alcohols such as isopropyl alcohol can be used according to the intended use.
  • the type of the second liquid is not particularly limited, and an electrolyte such as carbonated water or hydrogen water, or water in which a gas is dissolved, or an alcohol such as isopropyl alcohol. Can be used according to the intended use.
  • the diluted liquid to be manufactured is used for cleaning a semiconductor wafer, it is preferable to use ultrapure water as the first liquid and an aqueous ammonia solution as the second liquid.
  • an aqueous tetramethylammonium hydroxide (TMAH) solution can also be suitably used as the second liquid.
  • the ultrapure water mentioned here means treated water obtained by removing ions and nonionic substances from the treated water (raw water) using an ultrapure water production apparatus. It means treated water having a resistance value of 18 M ⁇ ⁇ cm or more.
  • the two tanks 12a and 12b are connected in parallel to each other. That is, the two tanks 12a and 12b are connected in series to the plurality of second pipes 13 via the valves 14a and 14b, respectively, on the outlet side. Valves 13a are provided on the inlet sides of the plurality of second pipes 13, respectively. A filter F1 is provided between the two valves 14a and 14b and the plurality of valves 13a. A three-way valve may be provided on the outlet side of the two tanks 12a and 12b instead of the two valves 14a and 14b. Further, a chemical liquid supply line (liquid supply means) 16 for supplying a second liquid to the tanks 12a and 12b is connected to the two tanks 12a and 12b via valves 15a and 15b, respectively.
  • a chemical liquid supply line (liquid supply means) 16 for supplying a second liquid to the tanks 12a and 12b is connected to the two tanks 12a and 12b via valves 15a and 15b, respectively.
  • Filters F2 and F3 are provided between the valve 15a and the tank 12a and between the valve 15b and the tank 12b, respectively, and the chemical solution supply line 16 is provided with a valve 16a. Further, the two tanks 12a and 12b are provided with air release valves 17a and 17b, respectively. A three-way valve may be provided on the inlet side of the two tanks 12a and 12b instead of the two valves 15a and 15b.
  • the diluent manufacturing apparatus 10 uses the pressure in the tanks 12a and 12b as a means for pumping the second liquid in the tanks 12a and 12b through the second pipe 13 and supplying the second liquid to the first pipe 11. It has the pressure adjustment part 18 to adjust.
  • the pressure adjustment unit 18 includes a tank pressurization gas supply line 18a for supplying tank pressurization gas into the tanks 12a and 12b, and a supply / exhaust mechanism 18b provided in the tank pressurization gas supply line 18a.
  • the air supply / exhaust mechanism 18b includes an air supply valve 18c and an exhaust valve 18d, and the tanks 12a and 12b can be pressurized or depressurized by opening and closing them.
  • the supply / exhaust mechanism 18b is not limited to the illustrated configuration, that is, the supply / pressurization mechanism (supply valve 18c) and the exhaust pressure reduction mechanism (exhaust valve 18d) are configured separately.
  • an air supply pressurizing mechanism such as an electropneumatic regulator and an exhaust pressure reducing mechanism may be integrally configured.
  • the tank pressurization gas supply line 18a is connected to one tank (first tank) 12a via a valve 19a, and is connected to the other tank (second tank) 12b via a valve 19b.
  • the gas supply line 18a is provided with a pressure gauge 19c for measuring the supply pressure of the tank pressurizing gas.
  • the tank pressurizing gas is not particularly limited, but it is preferable to use an inert gas, nitrogen gas, which can be used relatively easily.
  • an inert gas nitrogen gas
  • the tank pressurizing gas should be avoided. For this reason, even when an inert gas such as nitrogen is used, it may be affected by oxygen contained as an impurity, so that it is necessary to sufficiently consider its purity.
  • the second liquid is alternately supplied from the two tanks 12a and 12b to the first pipe 11 during the normal operation in which the diluent is manufactured. That is, the first supply mode in which the second liquid is supplied from the first tank 12 a to the first pipe 11, and the second liquid in which the second liquid is supplied from the second tank 12 b to the first pipe 11.
  • the two supply modes are appropriately switched based on the liquid level in each tank 12a, 12b. For example, in the first supply mode, when the liquid level in the first tank 12a falls below a predetermined lower limit liquid level, the supply of the second liquid from the first tank 12a is stopped, and the second tank 12b. The second liquid is supplied from. This switching operation will be described later.
  • the supply of the second liquid to the first pipe 11 is performed through one of the plurality of second pipes 13, but the plurality of second pipes 13 are connected to the second pipe 13.
  • the plurality of second pipes 13 have at least one of an inner diameter and a length that allow the second liquid to pass at different flow rates even when the pressure in each of the tanks 12a and 12b is constant, for example. Configured differently. The configuration of these second pipes 13 will also be described later.
  • the diluent manufacturing apparatus 10 has a control unit 20 that controls various operation operations of the diluent manufacturing apparatus 10.
  • the control unit 20 is based on at least the measurement results of the flow rate measurement unit 21 that measures the flow rate of the first liquid flowing in the first pipe 11 and the concentration measurement unit 22 that measures the concentration of the diluent.
  • the amount of the second liquid added to the first liquid by the pressure adjusting unit 18 can be adjusted so that the concentration of the diluted liquid becomes a predetermined concentration.
  • a method for adjusting the amount of addition of the second liquid by the control unit 20 will be described. Before that, Hagen-Poiseuille's law, which is the basis for adjusting the amount of addition, will be briefly described.
  • Hagen-Poiseuille's law is a law related to the loss head of laminar flow in a circular pipe.
  • the inner diameter of the pipe is D [m]
  • the length of the pipe is L [m]
  • the pressure gradient at both ends of the pipe is ⁇ P.
  • [Pa] the viscosity coefficient of the liquid is ⁇ [Pa ⁇ s]
  • the flow rate of the liquid flowing in the pipe is Q [m 3 / s]
  • Q ( ⁇ ⁇ D 4 ⁇ ⁇ P) / (128 ⁇ ⁇ ⁇ L) It is expressed by the relationship.
  • the flow rate Q of the liquid flowing through the circular tube is proportional to the fourth power of the inner diameter D of the circular tube and the pressure gradient ⁇ P at both ends, and the length L of the circular tube and the viscosity of the liquid It is inversely proportional to the coefficient ⁇ .
  • Hagen-Poiseuille's law is applied to the supply of the second liquid through each second pipe.
  • the length L and the inner diameter D of each of the second pipes are fixed values. If the type of the second liquid is determined, the viscosity coefficient ⁇ is also a fixed value. Therefore, it is possible to proportionally control the flow rate Q in each second pipe only by controlling the pressure in the tank corresponding to the pressure gradient ⁇ P between both ends of each second pipe.
  • the target value of the concentration of the diluted liquid to be manufactured is set, and the amount of the second liquid added is calculated with respect to the set target concentration.
  • the flow rate of the first liquid is measured by the flow rate measuring means 21, and the target addition amount of the second liquid for achieving the target concentration is calculated.
  • one second pipe 13 to be used is determined for the calculated target addition amount, and the target addition is performed on the determined second pipe 13.
  • a target value of the pressure in the first tank 12a for realizing the amount (flow rate) is calculated.
  • the pressure adjusting unit 18 adjusts the pressure in the first tank 12a to the calculated target pressure, so that the first tank 12a
  • the second liquid is added to the first liquid in the first pipe 11 through the second pipe 13 in a predetermined addition amount.
  • the flow rate Q of the second liquid flowing through the second pipe 13 is proportional to the pressure gradient ⁇ P at both ends of the second pipe 13. Therefore, for example, when the flow rate of the first liquid changes, the pressure in the first tank 12a is changed so that the pressure gradient ⁇ P is proportional to the change by a certain proportional constant.
  • the pressure gradient ⁇ P is halved and the flow rate of the second liquid is also halved.
  • the concentration of the second liquid itself may not be constant due to volatilization or decomposition of the second liquid in the first tank 12a.
  • the concentration of the diluted solution to be manufactured is initially adjusted within a predetermined concentration range including the target concentration, there is a possibility that it gradually deviates from the concentration range. Therefore, in this embodiment, when the concentration of the diluent is measured by the concentration measuring means 22 and the measured concentration of the diluent is out of the predetermined concentration range, the concentration of the diluent falls within the predetermined concentration range.
  • the proportionality constant described above is modified to fit.
  • the proportionality constant can be automatically changed to an optimum value even when the apparatus is initially operated or when the target value of the concentration of the diluent is changed. As a result, a diluted solution adjusted to a predetermined concentration can be stably produced.
  • the configuration of the flow rate measuring means 21 is not particularly limited, and for example, a Karman vortex flow meter or an ultrasonic flow meter can be used. Moreover, the flow rate measuring means 21 should just be installed in the position which can monitor the flow volume fluctuation
  • the flow rate measuring means 21 is provided on the upstream side of the connection portion of the first pipe 11 with the plurality of second pipes 13, but on the downstream side of the connection portion. The flow rate of the diluent flowing through the first pipe 11 may be measured. This is because the supply amount (flow rate) of the second liquid is much smaller than the flow rate of the first liquid, and the flow rate of the diluent can be handled equivalently to the flow rate of the first liquid.
  • the concentration measuring means 22 is not particularly limited as long as it can measure the concentration of the diluent as an electrochemical constant.
  • an electric conductivity meter, a pH meter, a specific resistance meter, an ORP meter (an oxidation meter) Reduction electrometer) or an ion electrode meter can be used.
  • an electric conductivity meter or a specific resistance meter as the concentration measuring means 22.
  • the concentration measuring means 22 is installed on the downstream side of the connection portion of the first pipe 11 with the plurality of second pipes 13. At this installation position, the first pipe 11 is provided. It may be directly attached to, or may be attached to a bypass pipe provided in parallel with the first pipe 11.
  • the accuracy of the second liquid supply amount (flow rate Q) is greatly influenced by the pressure gradient ⁇ P at both ends of the second pipe 13. Therefore, when the pressure at the connection portion between the first pipe 11 and the second pipe 13 fluctuates greatly, it becomes difficult to stably manufacture a diluent adjusted to a predetermined concentration.
  • a pressure measuring means 23 for measuring the pressure in the first pipe 11 is provided. Therefore, the control unit 20 sets the target of the pressure in the first tank 12a for setting the concentration of the diluent to the target concentration based on the measurement results of the flow rate measuring unit 21, the concentration measuring unit 22, and the pressure measuring unit 23.
  • the value is calculated and the amount of addition of the second liquid is adjusted.
  • the configuration of the pressure measurement means 23 is not particularly limited, and in the illustrated embodiment, the installation position is also upstream of the connection portion with the plurality of second pipes 13. If it can be measured, it may be downstream from the connecting portion.
  • the flow rate Q of the second liquid flowing in the second pipe 13 is proportional to the pressure gradient ⁇ P at both ends of the second pipe 13. Therefore, if this pressure gradient ⁇ P can be changed greatly, a wide supply amount (flow rate) of the second liquid can be realized and a wide concentration range can be dealt with.
  • a wide supply amount (flow rate) of the second liquid can be realized and a wide concentration range can be dealt with.
  • the pressure gradient ⁇ P since there is an upper limit to the pressure applied to each of the tanks 12a and 12b, it is difficult to greatly change the pressure gradient ⁇ P, and the adjustment range of the amount of addition of the second liquid is also limited.
  • the flow rate Q of the second liquid is also proportional to the inner diameter D (the fourth power) of the second pipe 13 and inversely proportional to its length L.
  • the plurality of second pipes 13 are configured such that at least one of the inner diameter and the length is different from each other. Has been. That is, the plurality of second pipes 13 are different from each other in at least one of the inner diameter and the length. For example, even if the pressure in each of the tanks 12a and 12b is constant, the second pipes 13 pass the second liquid at different flow rates. It is configured to let you. Thereby, it becomes possible to widen the adjustment range of the addition amount of the second liquid as the whole apparatus, and it becomes possible to manufacture a dilute solution having a wide concentration range.
  • the inner diameters of the individual second pipes 13 are not limited to specific dimensions, but in order to more precisely control the concentration of the diluent to be produced, the inner diameters of the respective second pipes 13 are It is preferably more than 0.1 mm and 4 mm or less, more preferably more than 0.2 mm and 0.5 mm or less. This is because the flow of the second liquid in the second pipe 13 tends to be a laminar flow (regular and orderly flow). That is, when the flow in the pipe becomes a turbulent flow (irregular flow), the Hagen-Poiseuille law described above does not hold, and the flow rate Q of the second liquid flowing in the second pipe is changed to the both ends of the second pipe.
  • each second pipe 13 has a laminar flow of the second liquid flowing in the pipe.
  • each second pipe 13 is not limited to a specific dimension. However, if the length is too short, the flow rate in the pipe is likely to be affected, and the liquid flow rate is reduced at both ends of the pipe. Proportional control with a pressure gradient becomes difficult. If the length is too long, it is difficult to install the pipe, and the contact area between the pipe and the liquid is increased, which may increase the contamination of the liquid in the pipe. Therefore, the length of each second pipe 13 is preferably in the range of 0.01 m to 100 m, and more preferably in the range of 0.1 m to 10 m.
  • the second pipe 13 having an inner diameter of 0.1 mm or less or a length exceeding 100 m depends on the combination, but the resistance when the second liquid flows through the pipe 13 is likely to increase. That is, the pressure in the tank tends to be high. Therefore, such an inner diameter and length are not preferable because it is difficult to select components (piping, valves, etc.) constituting the apparatus from the viewpoint of pressure resistance.
  • the second pipe 13 having an inner diameter of more than 4 mm or a length of less than 0.01 m tends to reduce the resistance when the second liquid flows through the pipe 13 depending on the combination. That is, the flow rate of the second liquid is easily changed by a slight change in the pressure in the tank. Therefore, such an inner diameter and length are not preferable because it is difficult to control the pressure in the tank.
  • the material and shape of the second pipe 13 are not particularly limited, but a resin-made flexible tube is preferably used.
  • resins include fluororesins such as PFA and ETFE, polyethylene resins, polypropylene resins, and the like, and when the diluted solution produced is used for cleaning or rinsing semiconductor wafers, there is little elution. A fluororesin is particularly preferred.
  • the second liquid is a volatile liquid
  • the second pipe 13 has gas permeability in order to suppress the concentration fluctuation of the liquid due to the liquid in the tube volatilizing and diffusing outside. It is preferable to use a low one.
  • oxygen contained in the diluent may have an adverse effect depending on the intended use of the diluent to be produced. Therefore, oxygen in the air moves from the outside of the second pipe 13 to the inside. It is also preferable in that it can suppress diffusion and suppress an increase in dissolved oxygen concentration in the second liquid.
  • the method of connecting the second pipe 13 to the first pipe 11 is not particularly limited as long as the first liquid and the second liquid are appropriately mixed.
  • the second pipe 13 is preferably connected to the first pipe 11 such that the tip thereof is located at the center of the first pipe 11, thereby efficiently connecting the first liquid and the first pipe 11.
  • the second liquid can be mixed.
  • the plurality of second pipes 13 are preferably individually connected to the first pipe 11 in that the structure is simple and the liquid pool is small.
  • the four second pipes 13 are provided, but the number of the second pipes 13 is not limited to four, depending on the required concentration range of the diluent, For example, it can be appropriately changed to two, three, or five or more. Accordingly, the combination of the inner diameter and the length is not limited to a specific combination and can be appropriately changed. As a combination of the inner diameter and the length, only one of them may be different. In this case, as described above, since there is an upper limit to the pressure applied to each of the tanks 12a and 12b, the inner diameters are different from each other in that the adjustment range of the amount of addition of the second liquid can be further expanded. A combination is preferred.
  • the length L affects the flow rate Q of the second liquid flowing through the second pipe 13, while the inner diameter D affects the fourth power. It is clear from what to do.
  • the second liquid is supplied to the first pipe 11 through one of the plurality of second pipes 13, but depending on the required concentration range of the diluent, a plurality of the second liquids may be supplied. Of these second pipes 13, two or more second pipes 13 may be used.
  • the first supply mode in which the second liquid is supplied from the first tank 12a to the first pipe 11 during the normal operation in which the dilution liquid is manufactured, and the second Switching to the second supply mode in which the second liquid is supplied from the tank 12b to the first pipe 11 is performed.
  • this switching operation will be described by taking as an example a case where switching from the first supply mode to the second supply mode is performed.
  • the valve 19a for connecting the tank pressurizing gas supply line 18a and the first tank 12a is opened, so that the tank pressurizing gas is supplied to the first tank 12a through the tank pressurizing gas supply line 18a.
  • a gas eg, nitrogen gas
  • the measured value (pressure in the first tank 12a) by the pressure gauge 19c is adjusted by the air supply / exhaust mechanism 18b so as to become the target pressure.
  • the second liquid in the first tank 12 a is added to the first liquid in the first pipe 11 in a predetermined addition amount through the designated second pipe 13.
  • valve 19b for connecting the tank pressurization gas supply line 18a and the second tank 12b, a valve 16a for the chemical supply line 16, and the chemical supply line 16 and the first tank 12a 15b, the valve 15b between the chemical solution supply line 16 and the second tank 12b, the atmosphere release valve 17a of the first tank 12a, and the atmosphere release valve 17b of the second tank 12b are all closed. It is in the state that was done. Further, the second tank 12b is in a standby state in which a small amount of the second liquid is stored.
  • the valve 16a of the chemical liquid supply line 16 is The air release valve 17b of the second tank 12b is opened. Subsequently, the valve 15b between the chemical liquid supply line 16 and the second tank 12b is opened, and the second liquid is supplied to the second tank 12b through the chemical liquid supply line 16 and stored.
  • the valve 16a of the chemical liquid supply line 16, the air release valve 17b of the second tank 12b, and the chemical liquid supply line 16 and the second tank Valve 15b between 12b is closed.
  • the valve 19b connecting the tank pressurization gas supply line 18a and the second tank 12b is opened, and the tank pressurization gas is introduced into the second tank 12b through the tank pressurization gas supply line 18a.
  • the measured value by the pressure gauge 19c is adjusted to the target pressure by the air supply / exhaust mechanism 18b. That is, the pressure in the second tank 12b is adjusted to the target pressure while maintaining the state in which the pressure in the first tank 12a is adjusted to the target pressure.
  • the valve 14b connecting the second tank 12b and the second pipe 13 is opened, and then the first tank 12a and the second pipe are connected. 13 is closed.
  • the supply mode is changed from the first supply mode in which the second liquid is supplied from the first tank 12a to the second supply mode in which the supply of the second liquid is supplied from the second tank 12b.
  • the switch is complete. Thereafter, the valve 19a connecting the tank pressurization gas supply line 18a and the first tank 12a is closed, and the first tank 12a is replenished with the second liquid for the next first supply mode. Wait until.
  • the supply of the second liquid from the second tank 12b is adjusted so that the pressure in the second tank 12b matches the pressure in the first tank 12a. Done later.
  • the first liquid in the first pipe 11 is added to the second liquid in the first tank 12a with a predetermined addition amount. Can be added to the liquid.
  • fluctuations in the amount of the second liquid added can be suppressed as much as possible. Therefore, fluctuations in the concentration of the diluted liquid produced can be suppressed as much as possible.
  • the atmosphere release valve 17b when the second tank 12b is in a standby state, the atmosphere release valve 17b is closed. This is to suppress the entry of oxygen into the second tank 12b and to suppress the dissolution of oxygen into the second liquid when the second liquid is replenished to the second tank 12b thereafter. However, if the dissolution of oxygen into the second liquid in the second tank 12b is not a problem, the atmosphere release valve 17b may not be closed. In addition, when replenishing the second liquid to the second tank 12b to the extent that the gas component in the tank is exhausted, the air in the tank is exhausted from the atmosphere release valve 17b, whereby the second liquid is discharged. Since the dissolution of oxygen into the liquid can be reduced, the atmosphere release valve 17b may be in either an open state or a closed state.
  • the replenishment of the second liquid to the second tank 12b is performed just before the end of the first supply mode, but the replenishment timing is not limited to this.
  • the second liquid can be replenished at an arbitrary timing in the first supply mode, such as immediately after switching to the first supply mode.
  • the atmosphere release valve 17b is preferably kept closed after the second liquid is replenished in order to suppress volatilization of the second liquid.
  • the switching from the first supply mode to the second supply mode is preferably started before the first tank 12a is emptied, as described above.
  • the dilution liquid manufacturing apparatus 10 of this embodiment temporarily stops supply of the first liquid to the first pipe 11 between normal operations, such as when there is no demand for the dilution liquid at the use point 1.
  • a transition to a standby mode in which the production of the diluted solution is temporarily stopped may occur.
  • the pressure in the first tank 12a that has been adjusted to the target pressure is preferably returned to the atmospheric pressure in consideration of safety. Conceivable.
  • depressurization to atmospheric pressure is actually not preferable in the following points.
  • the pressure in the first tank 12a is maintained and adjusted to a pressure exceeding the atmospheric pressure.
  • the atmospheric pressure Preferably it is.
  • the pressure in the first tank 12a in the standby mode is large in order to suppress the volatilization of the second liquid and suppress the concentration fluctuation. It is preferably higher than atmospheric pressure and higher than the saturated vapor pressure of the second liquid.
  • the tank pressurizing gas may be dissolved in the second liquid during normal operation. Therefore, in such a case, the pressure in the first tank 12a in the standby mode takes into account the solubility of the tank pressurizing gas in the second liquid in addition to the saturated vapor pressure of the second liquid. Preferably it is determined. On the other hand, since the good addition amount adjustment can be resumed more quickly after the normal operation is resumed, the pressure in the first tank 12a is adjusted to the target pressure as in the first supply mode even in the standby mode. May be maintained. Such adjustment is particularly suitable when the second liquid is water in which an electrolyte or gas such as carbonated water or hydrogen water is dissolved. *
  • FIG. 2 is a schematic configuration diagram of a diluent manufacturing apparatus according to the second embodiment of the present invention.
  • the same reference numerals are given to the same components as those in the first embodiment, the description thereof is omitted, and only the components different from those in the first embodiment will be described.
  • This embodiment is different from the first embodiment in that the function of the second tank 12b is changed.
  • the second tank 12b is connected in series via the connection line 31, not in parallel with the first tank 12a. More specifically, the second tank 12b is connected to the first tank 12a so that the second liquid in the second tank 12b is supplied to the first tank 12a by hydraulic head pressure. . Accordingly, the valves 14a, 14b, 15a, 15b of the first embodiment are omitted, and a plurality of second pipes 13 are provided only between the first tank 12a and the first pipe 11, The chemical solution supply line 16 is connected only to the second tank 12b.
  • the pressure gauge 19c is provided in the first tank 12a, and the connection line 31 is provided with a valve 31a and a check valve (not shown).
  • the second tank 12b functions as a temporary storage tank that temporarily stores the second liquid that is replenished to the first tank 12a. That is, during the normal operation in which the dilution liquid is manufactured, the second liquid is appropriately replenished from the second tank 12b to the first tank 12a based on the liquid level of the first tank 12a. The second liquid is continuously supplied from the tank 12 a to the first pipe 11. This eliminates the need for tank replacement and eliminates the need to stop the operation of the apparatus, thereby making it possible to continuously and stably manufacture the diluent. Hereinafter, this replenishment operation will be described.
  • tank pressurization gas for example, nitrogen gas
  • a measured value pressure in the first tank 12a
  • the target pressure is adjusted by the exhaust mechanism 18b.
  • the second liquid in the first tank 12 a is added to the first liquid in the first pipe 11 in a predetermined addition amount through the designated second pipe 13.
  • the following valves that is, a valve 19b for connecting the tank pressurization gas supply line 18a and the second tank 12b, a valve 16a for the chemical liquid supply line 16, an air release valve 17b for the second tank 12b,
  • the valve 31a of the connection line 31 is in a closed state.
  • the state of the air release valve 17b of the second tank 12b at this time is not limited to a closed state, as in the first embodiment, and is in an open state as necessary. May be.
  • the second tank 12b When the second liquid is supplied from the first tank 12a to the first pipe 11 and the liquid level in the first tank 12a falls below a predetermined lower limit liquid level, the second tank 12b is opened to the atmosphere. The valve 17b is opened. Subsequently, the valve 16a of the chemical liquid supply line 16 is opened, and the second liquid is supplied to the second tank 12b through the chemical liquid supply line 16 and stored. When the liquid level in the second tank 12b reaches a predetermined upper limit liquid level, the valve 16a of the chemical liquid supply line 16 is closed, and the air release valve 17b of the second tank 12b is closed.
  • the valve 19b connecting the tank pressurization gas supply line 18a and the second tank 12b is opened, and the tank pressurization gas is introduced into the second tank 12b through the tank pressurization gas supply line 18a.
  • the measured value by the pressure gauge 19c is adjusted to the target pressure by the air supply / exhaust mechanism 18b. That is, the pressure in the second tank 12b is adjusted to the target pressure while maintaining the state in which the pressure in the first tank 12a is adjusted to the target pressure.
  • the valve 31a of the connection line 31 is opened, and the second liquid is transferred from the second tank 12b to the first tank 12a by the hydraulic head pressure. .
  • the valve 31a of the connection line 31 is closed, and the second tank 12b is in a standby state until the next refilling operation.
  • the pressure in the second tank 12b matches the pressure in the first tank 12a. After being adjusted to do.
  • the pressure fluctuation of the first tank 12a can be suppressed as much as possible, and Concentration fluctuation can be suppressed as much as possible.
  • the bottom surface of the second tank 12b may be higher than the top surface of the first tank 12a so that the second liquid is reliably transferred to the first tank 12a by the head pressure. preferable.
  • the storage of the second liquid in the second tank 12b is started when the liquid level in the first tank 12a falls below a predetermined lower limit liquid level, but is limited to this timing. It can be performed at any timing.
  • the second liquid is a volatile liquid
  • the atmosphere release valve 17b remains closed after the replenishment of the second liquid.
  • the transfer of the second liquid from the second tank 12b to the first tank 12a can be performed at an arbitrary timing after the second liquid is stored in the second tank 12b.
  • the tank pressurizing gas is accumulated in the second pipe, and the gas is supplied to the first pipe and manufactured. Concentration fluctuations may occur in the diluted solution. Therefore, at least the transfer of the second liquid from the second tank 12b to the first tank 12a is performed at the above-described timing, that is, the second liquid is continuously supplied from the first tank 12a. It is preferably started before the first tank 12a is empty.
  • Example 1 diluted ammonia water was manufactured as a diluent using the diluent manufacturing apparatus 10 having the configuration shown in FIG. 3, and the conductivity of the diluted ammonia water was measured.
  • each tube A to E is as follows.
  • the thing made from PFA was used as the 1st piping 11, the 1st tank 12a, and the 2nd tank 12b, respectively.
  • the first liquid ultrapure water having a specific resistance value of 18 M ⁇ ⁇ cm or more and total organic carbon (TOC) of 1.0 ppb or less is used.
  • the first pipe 11 has a flow rate of 40 L / min and a water pressure of 0.35 MPa. We let water pass.
  • the second liquid 29 wt% ammonia water (for electronics industry, manufactured by Kanto Chemical Co., Inc.) was used, and nitrogen gas was used as the tank pressurizing gas introduced into the first tank 12a.
  • the conductivity of the diluted ammonia water when the pressure in the first tank 12a is changed and the amount of ammonia water added to the ultrapure water is changed is defined as the conductivity. Measurement was performed using a meter (product number “M300”, manufactured by METTLER TOLEDO).
  • FIG. 4 is a graph showing the measurement results at this time, the horizontal axis indicates the amount of ammonia water added to ultrapure water, and the vertical axis indicates the conductivity of the obtained diluted solution (dilute ammonia water). Yes.
  • Ammonia water is a weak base, and the change in conductivity with respect to the amount added is large in the low concentration range, but the change in conductivity with respect to the amount added becomes dull in the high concentration range. Therefore, the minimum amount of ammonia water in tube A and the electrical conductivity of the diluent at that time are 0.015 mL / min and 1.2 ⁇ S / cm, respectively, whereas the maximum amount of ammonia water in tube E is The amount and the electrical conductivity of the diluent at that time were 8.18 mL / min and 62.1 ⁇ S / cm, respectively.
  • the amount of ammonia water added is 0.015 mL / min (tube It was necessary to change about 545 times from A) to 8.18 mL / min (tube E).
  • the adjustment range of the ammonia water addition amount can be dealt with by using five tubes having different inner diameters and lengths. It was confirmed that dilute ammonia water in the concentration range could be produced continuously.
  • Example 2 In the present embodiment, using the dilution liquid manufacturing apparatus 10 having the configuration shown in FIG. 3, except that ultrapure water as the first liquid was passed through the first pipe 11 at a water pressure of 0.16 MPa. Dilute aqueous ammonia was produced under the same conditions as in Example 1. Then, the supply of the first liquid was temporarily stopped, that is, the production of the diluted solution was temporarily stopped, and the conductivity of the diluted ammonia water before and after that was measured. The temperature of ultrapure water and ammonia water was adjusted to 23 ° C., and the target value of the conductivity of the diluted solution was set to 40 ⁇ S / cm. FIG.
  • FIG. 5A shows the measurement results at this time (the flow rate of the first liquid, the pressure in the first tank, and the change over time in the conductivity of the diluted ammonia water).
  • FIG. 5B also shows a measurement result when the pressure in the first tank 12a is returned to atmospheric pressure when the supply of the first liquid is temporarily stopped as a comparative example.

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  • Condensed Matter Physics & Semiconductors (AREA)
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Abstract

Un dispositif 10 de fabrication d'un liquide dilué a : une première tuyauterie 11 pour fournir un premier liquide; un premier réservoir 12a pour stocker un second liquide; une seconde tuyauterie 13 qui relie le premier réservoir 12 et la première tuyauterie 11 ; une unité de réglage de pression 18 pour ajuster la pression dans le premier réservoir 12a, l'unité de réglage de pression 18 envoyant le second liquide à l'intérieur du premier réservoir 12a par l'intermédiaire de la seconde tuyauterie 13 et fournissant le second liquide à la première tuyauterie 11 ; une unité de contrôle 20 qui ajuste la quantité d'addition du second liquide au premier liquide par l'unité de réglage de pression 18 de telle sorte que la concentration du liquide dilué atteint une concentration prescrite sur la base du débit du premier liquide ou du liquide dilué s'écoulant dans la première tuyauterie 11, et la concentration du liquide dilué; et un second réservoir 12b connecté en série au premier réservoir 12a, le second réservoir 12b stockant temporairement le second liquide pour recharger le premier réservoir 12a.
PCT/JP2017/036436 2016-12-28 2017-10-06 Dispositif de fabrication de liquide dilué et procédé de fabrication de liquide dilué WO2018123193A1 (fr)

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CN111550673B (zh) * 2020-04-15 2022-04-19 北京航天试验技术研究所 一种多贮罐并联加注装置

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JPH10263379A (ja) * 1997-03-21 1998-10-06 Nikkiso Co Ltd 自動希釈装置
JPH1170328A (ja) * 1997-08-29 1999-03-16 Urutora Clean Technol Kaihatsu Kenkyusho:Kk 薬液定量注入装置および方法
JP2005175183A (ja) * 2003-12-11 2005-06-30 Kitz Sct:Kk 液体加圧機構及びこれを用いた液体制御装置と液体制御方法
JP2015158399A (ja) * 2014-02-24 2015-09-03 スガ試験機株式会社 耐候性試験機および希釈溶液供給装置
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KR102275626B1 (ko) 2021-07-09
KR20190077501A (ko) 2019-07-03

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