Apparatus and method for producing chemical solution for semiconductor production

Abstract

The present invention relates to the field of semiconductor processing, and discloses a manufacturing apparatus and a manufacturing method for a liquid medicine for semiconductor manufacturing, the apparatus comprising a tank, a gas flow path, a filter, and a bent portion forming a part of the gas flow path; a liquid detection sensor that is provided closer to the tank than the rising section in the gas flow path and detects a liquid immersed in the gas flow path; and a mechanism that performs at least one of discharge of the liquid immersed in the gas flow path, interruption of injection of the liquid into the tank, and closing of the gas flow path when the liquid detection sensor detects the liquid, the problem that meshes of a filter of a gas flow path for gas-liquid exchange are blocked is solved.

Description

Technical Field

[0001] The present invention relates to the field of semiconductor processing, and in particular to a manufacturing device and a manufacturing method for a chemical solution for semiconductor manufacturing. Background Art

[0002] There is known a manufacturing device for manufacturing a semiconductor manufacturing chemical liquid (hereinafter referred to as a chemical liquid) used in a semiconductor manufacturing process, such as a cleaning liquid for cleaning semiconductor wafers (see Patent Documents 1 and 2). In the semiconductor manufacturing process, a circuit pattern including metal wiring and an insulating film is formed on the surface of the semiconductor wafer by repeatedly performing processes such as film formation, exposure, etching, and planarization on the surface of the semiconductor wafer. Planarization is performed, for example, by CMP (Chemical Mechanical Polishing). The cleaning liquid is used, for example, to remove residues remaining on the surface of the semiconductor wafer after CMP.

[0003] In recent years, the miniaturization of semiconductor components has continued to advance, and quality management in the semiconductor manufacturing process has become very strict. Since the cleaning effect of the cleaning solution is also a factor that affects the quality of semiconductor components, the quality management of cleaning solutions and other liquids is also very important. Patent Document 1 (CN115138229B) and Patent Document 2 (CN115178120B) disclose the following technology: In the manufacturing process of the liquid, the concentration of the cleaning solution is accurately managed when a plurality of liquids as raw materials are mixed to generate the cleaning solution. Specifically, an overflow mechanism is provided in a mixing tank for mixing a plurality of liquids, and the amount of the liquid added is controlled by the overflow mechanism.

[0004] As in the above-mentioned mixing tank, a tank for containing liquid is used for various purposes in the manufacturing process of the liquid medicine. When the liquid is injected into the tank and discharged from the tank, it is necessary to introduce and discharge gas into the tank in order to perform gas-liquid exchange. Therefore, a gas flow path for gas flow is provided in the tank. One end of the gas flow path for gas-liquid exchange is connected to the space above the liquid level in the tank, and the other end is open to the outside. In addition, a filter is provided in the gas flow path, and the filter is used to remove particles as impurities from the gas sucked in from the open end.

[0005] In a chemical solution manufacturing apparatus having such a tank, there is a case where the liquid in the tank that becomes bubbles near the liquid surface penetrates into the gas flow path, flows through the gas flow path and adheres to the filter, causing clogging of the filter.

[0006] When the mesh of the filter is clogged, the following situations may occur: gas-liquid exchange cannot be properly performed and various adverse conditions may occur. For example, when the gas cannot be properly introduced into the tank, the tank will become negative pressure, and poor discharge of liquid from the tank will occur. In addition, when the gas cannot be properly discharged from the tank, the positive pressure in the tank becomes too high, and poor injection of liquid occurs. When such poor discharge or poor injection of liquid occurs, there is a possibility that the concentration of the drug solution will be unstable, affecting the quality of the drug solution. In addition, when the manufacturing device continues to operate in a state where the filter is clogged, it is also possible that the pressure change in the tank becomes larger, and unnecessary loads are imposed on various parts of the manufacturing device such as the tank and the pump, which becomes the cause of the failure. Therefore, it is necessary to take countermeasures against the problems caused by the clogging of the mesh of the filter. Summary of the invention

[0007] The main purpose of the present application is to provide a manufacturing device and a manufacturing method for chemical liquid for semiconductor manufacturing, so as to solve the problem of mesh clogging of the filter of the gas flow path for gas-liquid exchange.

[0008] In order to achieve the above-mentioned objectives, in a first aspect, the present application provides a manufacturing device for a chemical solution for semiconductor manufacturing, comprising: a tank that contains at least one liquid as a raw material of the liquid medicine and performs injection and discharge of the liquid; a gas flow path, one end of which is connected to the tank and the other end of which is open to the outside and is used to introduce and discharge gas into and out of the tank when the liquid is injected and discharged; a filter disposed in the gas flow path and filtering the gas sucked in or discharged from the open end of the gas flow path; a curved portion constituting a part of the gas flow path, including a descending section descending toward the filter in a direction from the tank toward the filter, and an ascending section ascending toward the filter after the descending section; a liquid detection sensor disposed in the gas flow path closer to the tank than the ascending section, and detecting liquid immersed in the gas flow path; and A mechanism that, when the liquid detection sensor detects the liquid, performs at least one of discharging the liquid immersed in the gas flow path, interrupting the injection of the liquid into the tank, and closing the gas flow path.

[0009] Optionally, the mechanism includes a liquid discharge mechanism for discharging the liquid immersed in the gas flow path when the liquid detection sensor detects the liquid.

[0010] Optionally, the drainage mechanism includes a drainage flow path, and the drainage flow path is connected to the gas flow path between the liquid detection sensor and the filter.

[0011] Optionally, the drainage channel is connected to the curved portion.

[0012] Optionally, the drainage channel is connected to the lower end of the curved portion.

[0013] Optionally, the inner wall surface of the tank is provided with a fluororesin layer.

[0014] Optionally, a liquid storage portion for storing the liquid immersed in the gas flow path is provided in the curved portion.

[0015] Alternatively, the liquid detection sensor is provided in the gas flow path closer to the tank side than the bent portion.

[0016] Optionally, a cleaning mechanism is also included for cleaning the gas flow path immersed in the liquid.

[0017] Optionally, the cleaning mechanism includes an introduction flow path that introduces cleaning liquid into the gas flow path portion between the tank and the liquid detection sensor.

[0018] Optionally, the gas flow path includes a plurality of branch flow paths each having the open end, and the filter is provided in each of the branch flow paths.

[0019] Optionally, it further includes an infiltration suppression mechanism that suppresses the liquid in a bubble shape generated on the liquid surface in the tank from infiltrating into the gas flow path.

[0020] Optionally, the liquid comprises a surfactant.

[0021] Optionally, the tank is a dissolution tank for dissolving a solute in a solvent.

[0022] In order to achieve the above-mentioned purpose, in a second aspect, the present application provides a method for manufacturing a chemical solution for semiconductor manufacturing, including a manufacturing process using the above-mentioned manufacturing device for semiconductor manufacturing chemical solution.

[0023] The manufacturing device and manufacturing method of semiconductor manufacturing liquid provided by the present invention have the beneficial effect compared with the prior art, that is, by providing a liquid detection sensor, the liquid immersed in the gas flow path can be detected in real time, and when the immersed liquid is detected in the gas flow path, the liquid is discharged in real time through the mechanism, the liquid injection tank is interrupted or the gas flow path is closed, thereby avoiding filter clogging. In addition, a curved portion is provided, which includes a descending interval and an ascending interval. The ascending interval can partially suppress the flow of liquid to the filter, further reducing the risk of filter clogging. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] The drawings constituting a part of this application are used to provide a further understanding of this application, so that other features, purposes and advantages of this application become more obvious. The schematic embodiment drawings and their descriptions of this application are used to explain this application and do not constitute an improper limitation on this application. In the drawings: Figure 1 It is a figure which shows a manufacturing apparatus.

[0025] Figure 2 This is a diagram showing the detailed structure of the generation unit.

[0026] Figure 3 This is a diagram showing the state of gas-liquid exchange when a surfactant and pure water are injected into a dissolving tank.

[0027] Figure 4 It is a diagram showing the state of gas-liquid exchange when the first raw material is discharged from the dissolving tank.

[0028] Figure 5 This is a diagram showing a state where the foamy first raw material penetrates into the gas flow path.

[0029] Figure 6 It is a figure which shows a bending part.

[0030] Figure 7 It is a diagram showing the operating state of the discharge valve when the liquid detection sensor does not detect bubbles.

[0031] Figure 8 It is a diagram showing the operating state of the discharge valve when the liquid detection sensor detects bubbles.

[0032] Fig. 9 This is a flowchart showing the operation procedure of the generation unit.

[0033] Fig.10 This is a diagram showing an example in which a liquid storage portion is provided.

[0034] Fig.11 This is a flowchart showing the operation procedure of the generation unit according to the second embodiment.

[0035] Fig.12 The diagram shows the operating states of a pump for supplying a surfactant and pure water and a valve for supplying a surfactant and pure water when the liquid detection sensor detects bubbles.

[0036] Fig.13 This is a diagram showing the operating state of the valve of the branch flow path when the liquid detection sensor detects bubbles.

[0037] Fig.14 This is a diagram showing an example in which a valve is provided between the liquid detection sensor and the curved portion.

[0038] Fig.15 This is a diagram showing an example in which the drain valve is a three-way valve.

[0039] Fig.16 It is a diagram showing the operating state of the discharge valve when the liquid detection sensor detects bubbles.

[0040] Fig.17 This is a diagram showing an example in which a cleaning mechanism is provided.

[0041] Fig.18 This is a diagram showing an example in which a defoaming mechanism is provided.

[0042] Among them: 2, manufacturing device; 10, raw material supply unit; 11, mixing tank; 12, purification unit; 13, control unit; 15, generation unit; 16, 17, 50, 51, 111, storage tank; 18, 55, supply flow path; 19, 35, 56, 113, pump; 20, 40, 41, 57, 85, 95, valve; 21, 37, 86, filter; 25, 60, stirring blade; 29, circulation flow path; 30, output flow path; 31, return flow path; 32, filling flow path; 33, product container; 34, relay flow path; 36, 65, 114, switching valve; 38, branch flow path; 39 , measuring device; 52, dissolving tank; 52A, inner wall surface; 53, gas flow path; 61, fluororesin layer; 66, first drainage flow path; 67, drainage tank; 70, main flow path; 71, bending portion; 72, branch flow path; 73, liquid detection sensor; 75, open end; 78, descending section; 79, ascending section; 80, relay section; 82, second drainage flow path; 83, 100, drainage valve; 90, liquid storage section; 90A, inlet; 110, cleaning mechanism; 112, introduction flow path; 120, Defoaming mechanism; 121, mounting part; 122, suction port; 123, internal rotating body; 124, motor; 125, liquid outlet; 126, mounting hole; BRM1, foamy first raw material (bubble); CL, cleaning liquid; CS, liquid medicine; PW, pure water; RM1, first raw material; RM2, second raw material; RM3, third raw material; SF, surfactant. DETAILED DESCRIPTION

[0043] Hereinafter, the particle measuring device for semiconductor manufacturing chemical solution, the filtering method for semiconductor manufacturing chemical solution, and the manufacturing method for semiconductor manufacturing chemical solution of the present invention will be described in detail based on the preferred embodiments shown in the drawings.

[0044] In addition, the following drawings are used to illustrate the measuring device for manufacturing particles in semiconductor solution, but the structure of the measuring device for manufacturing particles in semiconductor solution shown below is simplified for the purpose of illustrating the present invention, and the present invention is not limited to the structure of the drawings shown below.

[0045] In addition, below, "to" indicating a numerical range includes the numerical values ​​described on both sides. For example, the so-called ε is a numerical value εα to a numerical value εβ, which means that the range of ε is a range including the numerical values ​​εα and εβ, and if expressed in mathematical symbols, it is εα≤ε≤εβ.

[0046] In addition, as for specific angles, parallelism and orthogonality, unless otherwise specified, they are within the error range generally allowed in the corresponding technical field. Also, as for length, temperature and pressure, unless otherwise specified, they are within the error range generally allowed in the corresponding technical field.

[0047] In addition, in this specification, each component can be used alone as a substance equivalent to each component, or two or more substances can be used in combination. Here, when two or more substances are used in combination for each component, unless otherwise specified, the content of the component refers to the total content of the substances used in combination.

[0048] Embodiment 1: As an example, Figure 1 As shown, the manufacturing device 2 manufactures a chemical solution CS for semiconductor manufacturing. The chemical solution CS is, for example, a cleaning solution for removing residues remaining on the surface of a semiconductor wafer after CMP in a semiconductor manufacturing process. The manufacturing device 2 includes a raw material supply unit 10, a mixing tank 11, a purification unit 12, and a control unit 13 (see Figure 2 ). The manufacturing device 2 is an example of the "manufacturing device for semiconductor manufacturing chemical solution" according to the present invention. In addition, the manufacturing device 2 implements the "manufacturing method for semiconductor manufacturing chemical solution" according to the present invention.

[0049] The raw material supply unit 10 has a first raw material RM1 (see Figure 2 ) of the first raw material RM1, a storage tank 16 for the second raw material RM2, and a storage tank 17 for the third raw material RM3. The generating unit 15 generates the first raw material RM1 under the control of the control unit 13. In addition, the control unit 13 is composed of a processor such as a CPU (Central Processing Unit), a memory, a storage device, and a bus connecting these processors, memories, and storage devices.

[0050] The first raw material RM1 is a liquid, for example, a surfactant SF dissolved in pure water PW (see Figure 2 ) of a surfactant aqueous solution. The second raw material RM2 is also a liquid, for example, an organic acid aqueous solution in which an organic acid such as carboxylic acid is dissolved in pure water. In addition, the third raw material RM3 is also a liquid, for example, an organic acid aqueous solution in which an organic acid such as phosphonic acid is dissolved in pure water.

[0051] One end of a supply flow path 18 is connected to the generation unit 15 and the storage tanks 16 and 17, respectively. The other end of the supply flow path 18 is connected to the upper portion of the mixing tank 11. The first to third raw materials RM1 to RM3 are supplied to the mixing tank 11 through the supply flow path 18. In addition, the supply flow path 18 also includes a gas flow path 53 described later, and the flow paths are composed of pipes.

[0052] A pump 19, a valve 20 and a filter 21 are provided in order from the upstream side on the supply flow path 18. The pump 19 is driven under the control of the control unit 13. The pump 19 delivers the first raw material RM1 to the third raw material RM3 to the mixing tank 11 at a set speed. The set speed is the flow rate per unit time. The valve 20 is opened and closed under the control of the control unit 13. The valve 20 adjusts the flow rate of the first raw material RM1 to the third raw material RM3 passing through the supply flow path 18 by changing its opening. The filter 21 removes impurity particles in the first raw material RM1 to the third raw material RM3 passing through the supply flow path 18.

[0053] A stirring blade 25 is provided in the mixing tank 11. The stirring blade 25 rotates at a set rotation speed under the control of the control unit 13. Thus, the first raw material RM1 to the third raw material RM3 are mixed in the mixing tank 11 to produce a chemical solution CS.

[0054] The purification section 12 performs a process of removing impurity particles contained in the drug solution CS as a purification process for the drug solution CS produced in the mixing tank 11. The purification section 12 is provided with a circulation flow path 29 that circulates the drug solution CS between the mixing tank 11 and the purification section 12 by temporarily discharging the drug solution CS from the mixing tank 11 and returning it to the mixing tank 11 again. The circulation flow path 29 is composed of, for example, an output flow path 30 and a return flow path 31. One end of the output flow path 30 is connected to the lower part of the mixing tank 11. One end of the return flow path 31 is connected to the upper part of the mixing tank 11. Moreover, the other ends of the output flow path 30 and the return flow path 31 are connected to each other, thereby forming the circulation flow path 29.

[0055] One end of the filling flow path 32 is connected to the circulation flow path 29, for example, near the connection point between the output flow path 30 and the return flow path 31. A product container 33 is connected to the other end of the filling flow path 32. The chemical solution CS that has passed through the output flow path 30 and the filling flow path 32 is filled in the product container 33. The product container 33 is shipped as a product to a factory that uses the chemical solution CS for semiconductor manufacturing.

[0056] On the output flow path 30, a pump 35, a switching valve 36 and a filter 37 are provided in order from the upstream side. The pump 35 is driven under the control of the control unit 13. The pump 35 sucks the liquid medicine CS from the mixing tank 11, circulates the sucked liquid medicine CS in the circulation flow path 29, or sends it from the output flow path 30 to the filling flow path 32. One end of the relay flow path 34 is connected to the switching valve 36. The other end of the relay flow path 34 is connected to the return flow path 31. The switching valve 36 is opened and closed under the control of the control unit 13. The switching valve 36 switches the flow path through which the liquid medicine CS passes to either the output flow path 30 or the relay flow path 34. The filter 37 removes foreign particles in the liquid medicine CS passing through the output flow path 30.

[0057] A branch flow path 38 is provided on the downstream side of the filter 37 of the output flow path 30. A measuring device 39 is arranged in the branch flow path 38. The measuring device 39 measures the amount of foreign particles in the drug solution CS passing through the branch flow path 38 in a unit period (for example, 1 second). More specifically, the measuring device 39 is a so-called particle counter that counts the number of foreign particles as the amount of foreign particles. The measuring device 39 is, for example, a light scattering particle counter that counts the number of foreign particles by the number of light receptions of scattered light generated by irradiating the measuring light to the foreign particles. Alternatively, the measuring device 39 may be a light shielding particle counter that counts the number of foreign particles by the number of times the measuring light is blocked by the foreign particles. The measuring device 39 outputs the counting result of the number of foreign particles to the control unit 13.

[0058] A valve 40 is provided on the circulation channel 29 side and a valve 41 is provided on the filling channel 32 side near the connection point between the circulation channel 29, the discharge channel 30 and the filling channel 32. These valves 40 and 41 are opened and closed under the control of the control unit 13.

[0059] The control unit 13 selects any one of the following three paths as the path for the drug solution CS to flow in the purification unit 12 by controlling the opening and closing states of the switching valve 36, the valve 40, and the valve 41. First, the first path is the circulation flow path 29. When the output flow path 30 side of the switching valve 36 is opened and the relay flow path 34 side is closed, and the valve 40 is opened and the valve 41 is closed, the circulation flow path 29 as the first path is selected. At this time, the drug solution CS flowing out of the mixing tank 11 returns to the mixing tank 11 from the output flow path 30 via the return flow path 31. At this time, the drug solution CS does not pass through the relay flow path 34. In addition, at this time, the drug solution CS passes through the filter 37. Therefore, the impurity particles in the drug solution CS are removed by the filter 37. Therefore, by repeatedly circulating the drug solution CS based on the circulation flow path 29, the removal of impurity particles in the drug solution CS can be promoted and the purity of the drug solution CS can be improved. When the count result of the number of impurity particles by the measuring device 39 does not satisfy the preset quality condition, the control unit 13 selects the circulation flow path 29 by switching the valve 36. Specifically, the quality condition is the upper limit value of the number of impurity particles required for the chemical solution CS. When the count result of the number of impurity particles does not satisfy the quality condition, it means that the count result of the number of impurity particles is above the upper limit value.

[0060] The second path is a path from the output flow path 30 toward the filling flow path 32. When the output flow path 30 side of the switching valve 36 is opened, the relay flow path 34 side is closed, and the valve 40 is closed and the valve 41 is opened, the second path is selected. At this time, the liquid medicine CS flowing out of the mixing tank 11 is filled into the product container 33 from the output flow path 30 via the filling flow path 32. When the counting result of the number of impurity particles of the measuring device 39 meets the quality condition, the control unit 13 selects the second path. When the counting result of the number of impurity particles meets the quality condition means when the counting result of the number of impurity particles is less than the upper limit value. Therefore, only the liquid medicine CS that meets the quality condition is filled into the product container 33, and the liquid medicine CS that does not meet the quality condition is not filled.

[0061] The third path is a path from the output flow path 30 to the return flow path 31 via the relay flow path 34. When the output flow path 30 side of the switching valve 36 is closed, the relay flow path 34 side is opened, and both the valve 40 and the valve 41 are closed, the third path is selected. At this time, the liquid medicine flowing out of the mixing tank 11 returns to the mixing tank 11 from the output flow path 30 via the relay flow path 34 and the return flow path 31. That is, although different from the circulation flow path 29, the third path from the output flow path 30 to the return flow path 31 via the relay flow path 34 also forms a circulation flow path for the liquid medicine CS. However, in the third path, since the liquid medicine CS does not pass through the filter 37, the impurity particles in the liquid medicine CS are not removed by the filter 37. When the filter 37 and / or the measuring instrument 39 are maintained, the control unit 13 selects the third path formed by the output flow path 30, the return flow path 31 and the relay flow path 34.

[0062] As an example, Figure 2 As shown, the generating unit 15 includes a storage tank 50 for the surfactant SF, a storage tank 51 for the pure water PW, a dissolving tank 52, and a gas flow path 53. The surfactant SF and the pure water PW are examples of "liquids" according to the present invention. The dissolving tank 52 is an example of "tank" according to the present invention.

[0063] One end of a supply flow path 55 is connected to the lower part of the storage tanks 50 and 51. The other end of the supply flow path 55 is connected to the upper part of the dissolution tank 52. The surfactant SF and the pure water PW are supplied to the dissolution tank 52 through the supply flow path 55. That is, the surfactant SF and the pure water PW are injected into the dissolution tank 52.

[0064] A pump 56 and a valve 57 are provided in order from the upstream side on the supply flow path 55. The pump 56 is driven under the control of the control unit 13. The pump 56 delivers the surfactant SF and the pure water PW to the dissolution tank 52 at set speeds. The valve 57 is opened and closed under the control of the control unit 13. The valve 57 adjusts the flow rate of the surfactant SF and the pure water PW passing through the supply flow path 55 by changing its opening. In addition, a filter may be provided on the downstream side of the valve 57.

[0065] The dissolving tank 52 is a closed space with airtightness and liquid-tightness. In addition, the dissolving tank 52 is made of metal such as stainless steel, aluminum or copper. However, the inner wall surface 52A of the dissolving tank 52 in contact with the first raw material RM1 is covered with a fluororesin layer 61 so that the metal component does not dissolve into the first raw material RM1. Specifically, the fluororesin layer 61 is polytetrafluoroethylene (PTFE) or perfluoroalkoxyalkane (PFA).

[0066] The dissolving tank 52 is provided with a stirring blade 60. The stirring blade 60 rotates at a set rotation speed under the control of the control unit 13. Thus, the surfactant SF is dissolved in the pure water PW in the dissolving tank 52 (the surfactant SF and the pure water PW are mixed), and the first raw material RM1 is generated.

[0067] The other end of the supply flow path 18 is connected to the lower part of the dissolving tank 52. The switching valve 65 is provided on the supply flow path 18. One end of the first drain flow path 66 is connected to the switching valve 65. The other end of the first drain flow path 66 is connected to the drain tank 67. The switching valve 65 is opened and closed under the control of the control unit 13. The switching valve 65 switches the flow path through which the first raw material RM1 passes to either the supply flow path 18 or the first drain flow path 66. That is, the first raw material RM1 is discharged from the dissolving tank 52 through the supply flow path 18 or the first drain flow path 66.

[0068] The gas flow path 53 is a flow path for gas-liquid exchange. Figure 3 As shown in FIG. 5 , when the surfactant SF and the pure water PW are injected into the dissolving tank 52, the gas flow path 53 discharges the gas in the dissolving tank 52 to the outside through the open end 75. Figure 4 As shown in FIG. 5 , when the first raw material RM1 is discharged from the dissolving tank 52, the gas flow path 53 introduces the gas from the outside into the dissolving tank 52 through the open end 75. Figure 3 and Figure 4 In the figure, the pump 56, the valve 57, and the bent portion 71 described later are omitted.

[0069] As an example, Figure 5 As shown in FIG. 1 , the first raw material RM1 often generates a foamy first raw material (hereinafter simply referred to as a bubble) BRM1 on the liquid surface due to stirring. In particular, since the first raw material RM1 contains a surfactant SF, bubbles BRM1 are easily generated. In addition, the bubbles BRM1 may be Figure 3 As shown in FIG. 1 , when the surfactant SF and the pure water PW are injected into the dissolving tank 52, the gas discharged together penetrates into the gas flow path 53. The present invention suppresses the filter 86 (refer to FIG. 1 ) caused by the bubbles BRM1 penetrating into the gas flow path 53. Figure 2 )’s mesh is clogged.

[0070] Back to Figure 2 The gas flow path 53 includes a main flow path 70, a curved portion 71, and three branch flow paths 72. The main flow path 70, the curved portion 71, and the branch flow paths 72 are provided in this order from the dissolution tank 52 side.

[0071] One end of the main flow path 70 is connected to the dissolving tank 52. More specifically, one end of the main flow path 70 is connected to the space above the liquid level of the first raw material RM1 in the dissolving tank 52. In addition, a liquid detection sensor 73 is provided in the main flow path 70. Since the main flow path 70 is located closer to the dissolving tank 52 than the curved portion 71, the liquid detection sensor 73 is provided closer to the dissolving tank 52 than the curved portion 71. Further, the liquid detection sensor 73 is provided in the rising section 79 (refer to Figure 6 ) is closer to the dissolving tank 52. The liquid detection sensor 73 detects the bubble BRM1 that enters the gas flow path 53 from the dissolving tank 52. When the liquid detection sensor 73 detects the bubble BRM1, it outputs a detection signal indicating that the bubble BRM1 is detected to the control unit 13.

[0072] The other end of the main flow path 70 and one end of the branch flow path 72 are connected to the curved portion 71. Figure 6As shown in the enlarged view, the curved portion 71 includes a descending section 78, an ascending section 79, and a relay section 80. The descending section 78 is a section that descends toward the branch flow path 72. The ascending section 79 is a section that ascends toward the branch flow path 72 after the descending section 78. The relay section 80 is a section connecting the descending section 78 and the ascending section 79. As an example, the descending section 78, the ascending section 79, and the relay section 80 are all formed by straight-line piping. Therefore, the curved portion 71 is U-shaped. As the names indicate, the descending section 78 and the ascending section 79 are the descending section and the ascending section of the piping constituting the gas flow path 53. Descending refers to a state in which the piping is inclined downward at a set angle from the horizontal direction. In addition, ascending refers to a state in which the piping is inclined upward at a set angle from the horizontal direction. The set angle is, for example, 90°. The piping constituting the relay section 80 is, for example, parallel to the horizontal direction.

[0073] exist Figure 2 In the embodiment, one end of the second drainage flow path 82 is connected to the lower end of the descending section 78. That is, the second drainage flow path 82 is connected to the gas flow path 53 between the liquid detection sensor 73 and the branch flow path 72. Further, the second drainage flow path 82 is connected to the curved portion 71, and further connected to the lower end of the curved portion 71. The other end of the second drainage flow path 82 is connected to the drainage tank 67.

[0074] A drain valve 83 is provided in the second drain flow path 82. The drain valve 83 is opened and closed under the control of the control unit 13. The control unit 13, the second drain flow path 82, and the drain valve 83 are an example of the "mechanism for discharging the liquid immersed in the gas flow path" according to the present invention. In addition, the second drain flow path 82 is an example of the "drain flow path" according to the present invention.

[0075] The other ends of the three branch channels 72 are all open ends 75 opened to the outside as described above. The branch channels 72 are provided with valves 85 and filters 86. The valves 85 and filters 86 are provided in order from the dissolution tank 52 side. The valves 85 are opened and closed under the control of the control unit 13. The valves 85 are closed when the filters 86 are replaced, etc. The filters 86 filter the gas discharged from the dissolution tank 52 and the gas introduced from the open end 75.

[0076] As an example, Figure 7 As shown, when the bubble BRM1 is not immersed in the gas flow path 53 and the detection signal is not output from the liquid detection sensor 73, the control unit 13 closes the drain valve 83. That is, when the detection signal is not output from the liquid detection sensor 73, the control unit 13 closes the second drain flow path 82.

[0077] On the other hand, as an example, Figure 8As shown, when the bubble BRM1 is immersed in the gas flow path 53, the liquid detection sensor 73 detects the immersed bubble BRM1 and a detection signal is output from the liquid detection sensor 73, the control unit 13 opens the drain valve 83. That is, when the detection signal is output from the liquid detection sensor 73, the control unit 13 opens the second drain flow path 82. In this way, by opening the second drain flow path 82, the bubble BRM1 immersed in the gas flow path 53 is discharged into the drain tank 67 through the second drain flow path 82.

[0078] Next, as an example, refer to Fig. 9 The flowchart shown in FIG. 1 illustrates the effect brought about by the above structure. In the generating unit 15, the generation of the first raw material RM1 is started (step ST100). Specifically, under the control of the control unit 13, the valve 57 is opened, and the pump 56 is further driven. As a result, the surfactant SF and the pure water PW stored in the storage tanks 50 and 51 are injected into the dissolving tank 52 through the supply flow path 55. The gas in the dissolving tank 52 is discharged to the outside through the gas flow path 53. Therefore, the positive pressure in the dissolving tank 52 is prevented from becoming too high, and the poor injection of the surfactant SF and the pure water PW into the dissolving tank 52 is suppressed.

[0079] In the dissolution tank 52, the stirring blade 60 rotates at a set rotation speed under the control of the control unit 13. Thus, the surfactant SF is dissolved in the pure water PW to generate the first raw material RM1.

[0080] The supply flow path 18 side of the switching valve 65 is opened under the control of the control unit 13, and the first raw material RM1 is supplied to the mixing tank 11 through the supply flow path 18. The gas is introduced into the dissolving tank 52 through the gas flow path 53. Therefore, the dissolving tank 52 is prevented from becoming negative pressure, and the discharge of the first raw material RM1 from the dissolving tank 52 is suppressed.

[0081] In addition to the first raw material RM1, the second raw material RM2 and the third raw material RM3 are supplied to the mixing tank 11. The first raw material RM1 to the third raw material RM3 are mixed in the mixing tank 11 to prepare a drug solution CS. The drug solution CS is purified in the purification unit 12 and then filled into the product container 33.

[0082] When the generation of the first raw material RM1 is started, Figure 7As shown, the drain valve 83 is closed. In the gas flow path 53, whether the bubble BRM1 is immersed is monitored by the liquid detection sensor 73 (step ST110). When the bubble BRM1 is not immersed in the gas flow path 53 and the detection signal is not output from the liquid detection sensor 73 ("No" in step ST110), the drain valve 83 remains in the closed state. On the other hand, when the bubble BRM1 is immersed in the gas flow path 53, the immersed bubble BRM1 is detected by the liquid detection sensor 73 and the detection signal is output from the liquid detection sensor 73 to the control unit 13 ("Yes" in step ST110), as shown in FIG. Figure 8 As shown, the drain valve 83 is opened under the control of the control unit 13. Thus, the second drain flow path 82 is opened (step ST120). The bubbles BRM1 immersed in the gas flow path 53 are discharged to the drain tank 67 through the second drain flow path 82 (step ST130).

[0083] When the bubble BRM1 continues to penetrate into the gas flow path 53, the penetrated bubble BRM1 is detected by the liquid detection sensor 73, and the detection signal is output from the liquid detection sensor 73 to the control unit 13 ("Yes" in step ST140), the drain valve 83 is maintained in the open state, and the bubble BRM1 immersed in the gas flow path 53 is discharged into the drain tank 67 (step ST130). On the other hand, when the bubble BRM1 is no longer immersed in the gas flow path 53 and the detection signal is no longer output from the liquid detection sensor 73 ("No" in step ST140), the drain valve 83 is closed under the control of the control unit 13. Thus, the second drain flow path 82 is closed (step ST150). When the production of the chemical solution CS is not completed ("No" in step ST160), the processing of these steps ST110 to ST150 is continuously repeated.

[0084] As described above, the production unit 15 of the manufacturing device 2 includes a dissolution tank 52, a gas flow path 53, a filter 86, a curved portion 71, and a liquid detection sensor 73. The dissolution tank 52 contains the first raw material RM1 (surfactant SF and pure water PW) of the chemical solution CS, and can inject the surfactant SF and pure water PW and discharge the first raw material RM1. One end of the gas flow path 53 is connected to the dissolution tank 52, and the other end is an open end 75 open to the outside. Figure 3 and Figure 4 As shown, the gas flow path 53 is a gas-liquid exchange flow path for introducing and discharging gas into and out of the dissolving tank 52 when the surfactant SF and pure water PW are injected and the first raw material RM1 is discharged. The filter 86 is provided in the gas flow path 53 to filter the gas sucked from the open end 75.

[0085] The bent portion 71 constitutes a part of the gas flow path 53. Figure 6As shown in FIG. 1 , the curved portion 71 includes a descending section 78 that descends toward the filter 86 in the direction from the dissolving tank 52 toward the filter 86, and an ascending section 79 that ascends toward the filter 86 after the descending section 78. By providing the curved portion 71, the distance from the dissolving tank 52 to the filter 86 can be made longer than in the case where the curved portion 71 is not provided. Therefore, it is difficult for the bubbles BRM1 immersed in the gas flow path 53 to reach the filter 86. In particular, by providing the ascending section 79, it is more difficult for the bubbles BRM1 immersed in the gas flow path 53 to reach the filter 86 due to the action of gravity. Therefore, compared with the conventional method, the filter 86 is less likely to be clogged.

[0086] The liquid detection sensor 73 is disposed in the gas flow path 53 closer to the dissolution tank 52 than the ascending section 79. The liquid detection sensor 73 detects the bubble BRM1 immersed in the gas flow path 53. Figure 8 As shown in FIG. 1 , when the liquid detection sensor 73 detects the bubble BRM1, the drain valve 83 is opened under the control of the control unit 13, and the second drain flow path 82 is opened. The bubble BRM1 is discharged into the drain tank 67 through the second drain flow path 82. Since the bubble BRM1 is discharged, it is more difficult for the bubble BRM1 to reach the filter 86. Therefore, the filter 86 is less likely to be clogged than before. As a result, it is possible to suppress the occurrence of inadequate injection of the surfactant SF and the pure water PW into the dissolving tank 52 and the inadequate discharge of the first raw material RM1 from the dissolving tank 52 due to the clogging of the filter 86.

[0087] The mechanism for discharging the bubbles BRM1, which is composed of the control unit 13, the second drain flow path 82, and the drain valve 83, discharges the bubbles BRM1, which is the root cause of the clogging of the filter 86, from the gas flow path 53. Therefore, the probability of the filter 86 being clogged by the bubbles BRM1 can be reduced to near zero.

[0088] In addition, according to the mechanism for discharging the bubble BRM1 composed of the control unit 13, the second drain flow path 82, and the drain valve 83, the bubble BRM1 can be discharged without closing the gas flow path 53. Therefore, during the discharge process of the bubble BRM1, the gas-liquid exchange is smoothly performed by the gas flow path 53. Therefore, it is difficult for the mesh of the filter 86 to be clogged without interrupting the production of the first raw material RM1.

[0089] The second liquid discharge channel 82 is connected to the gas channel 53 between the liquid detection sensor 73 and the filter 86. Therefore, the bubbles BRM1 passing through the liquid detection sensor 73 can be discharged before reaching the filter 86, and the probability of clogging of the filter 86 can be reduced to near zero.

[0090] The second drainage channel 82 is connected to the curved portion 71. Therefore, the bubbles BRM1 can be discharged before reaching the filter 86, and the probability of clogging of the filter 86 can be made infinitely close to zero.

[0091] The second drainage flow path 82 is connected to the lower end of the curved portion 71 (the lower end of the descending section 78). Therefore, the bubbles BRM1 can be smoothly discharged under the action of gravity.

[0092] The fluororesin layer 61 is provided on the inner wall surface 52A of the dissolving tank 52. If the filter 86 is clogged, the first raw material RM1 is poorly discharged from the dissolving tank 52, and the pressure in the dissolving tank 52 becomes negative, the fluororesin layer 61 may be peeled off. However, according to the present invention, the effect of making the filter 86 less likely to be clogged can be achieved, and the possibility of the fluororesin layer 61 being peeled off can be reduced.

[0093] The liquid detection sensor 73 is provided in the gas flow path 53 closer to the dissolution tank 52 than the curved portion 71. Therefore, the bubbles BRM1 infiltrating the gas flow path 53 can be detected quickly. Therefore, measures such as discharging the bubbles BRM1 to prevent the bubbles BRM1 from reaching the filter 86 can be taken immediately.

[0094] The gas flow path 53 is branched into three branch flow paths 72 each having an open end 75, and filters 86 are provided in each of the three branch flow paths 72. Therefore, even if one filter 86 is clogged, the production of the chemical solution CS can be continued as long as the other filters 86 are not clogged. Furthermore, the other filters 86 that are not clogged can be allowed to continue to operate and the clogged filter 86 can be replaced.

[0095] The first raw material RM1 contains a surfactant SF. The surfactant SF is easy to foam, so the bubbles BRM1 are more likely to penetrate into the gas flow path 53. Therefore, in the manufacturing device 2 that processes a liquid containing a surfactant SF that is easy to foam, such as the first raw material RM1, the present invention, which has the effect of suppressing the clogging of the mesh of the filter 86 caused by the bubbles BRM1, is particularly effective.

[0096] The dissolving tank 52 is a tank for dissolving the surfactant SF in the pure water PW. When the surfactant SF and the pure water PW are stirred by the stirring blade 60 in order to dissolve the surfactant SF in the pure water PW, bubbles are easily generated, so the bubbles BRM1 are more likely to penetrate into the gas flow path 53. Therefore, in the manufacturing device 2 that processes the liquid containing the surfactant SF that is easy to foam, such as the first raw material RM1, the present invention having the effect of suppressing the clogging of the mesh of the filter 86 caused by the bubbles BRM1 is particularly effective.

[0097] Modification 1 As long as the valve 85 is not closed, the gas flow path 53 is in an open state. Therefore, although there is almost no possibility that the bubbles BRM1 immersed in the gas flow path 53 can reach the filter 86, it cannot be said that there is no possibility at all. Therefore, as an example, Fig.10 As shown, a liquid storage portion 90 for storing the bubbles BRM1 immersed in the gas flow path 53 may be provided in the curved portion 71. The liquid storage portion 90 is provided between the descending section 78 and the ascending section 79, that is, in the relay section 80. In other words, the liquid storage portion 90 is provided at a position greater than Figure 2 The drain valve 83 disposed in the second drain flow path 82 shown is closer to the filter 86 side. In order to suppress the possibility of the bubble BRM1 passing to the downstream side, the inlet 90A of the reservoir 90 provided in the relay section 80 is formed to have a width that can reliably introduce the bubble BRM1 into the reservoir 90. By providing the reservoir 90, the bubble BRM1 can be recovered even when the bubble BRM1 does not flow to the drain flow path 82 but enters the relay section 80. In addition to the curved portion 71 and the mechanism for discharging the bubble BRM1, a double and triple defense countermeasure such as the reservoir 90 is taken, so that the following effect can be ensured: the filter 86 is less likely to be clogged than before, and the occurrence of inconvenience caused by the clogging of the filter 86 can be suppressed. In addition, the reservoir 90 can be connected to the drain tank 67 and the bubble BRM1 stored in the reservoir 90 can be discharged to the drain tank 67.

[0098] Embodiment 2: The first embodiment described above shows an example in which, when the bubble BRM1 enters the gas flow path 53, a defense measure is taken to prevent the bubble BRM1 from reaching the filter 86 without interrupting the generation of the first raw material RM1. In contrast, the second embodiment is an example in which a defense measure is taken to prevent the bubble BRM1 from reaching the filter 86 by interrupting the generation of the first raw material RM1.

[0099] As an example, Fig.11 As shown in the flowchart, in the second embodiment, when the bubble BRM1 is immersed in the gas flow path 53, the immersed bubble BRM1 is detected by the liquid detection sensor 73 and the detection signal is output from the liquid detection sensor 73 to the control unit 13 ("Yes" in step ST110), the generation of the first raw material RM1 is interrupted under the control of the control unit 13, and a defensive measure is taken to prevent the bubble BRM1 from reaching the filter 86 (step ST200).

[0100] When the bubble BRM1 continues to penetrate into the gas flow path 53, the penetrated bubble BRM1 is detected by the liquid detection sensor 73, and the detection signal is output from the liquid detection sensor 73 to the control unit 13 ("Yes" in step ST140), the defensive countermeasure is continued (step ST200). On the other hand, when the bubble BRM1 no longer penetrates into the gas flow path 53 and the detection signal is no longer output from the liquid detection sensor 73 ("No" in step ST140), the defensive countermeasure is released, and after the set time has passed, the production of the first raw material RM1 is restarted (step ST210). The set time is, for example, a time set based on the average time required for the bubble BRM1 immersed in the gas flow path 53 to disappear naturally. When the production of the chemical solution CS is not completed ("No" in step ST160), the processing of these steps ST110, ST200, ST140 and ST210 is continued to be repeated.

[0101] There are two types of defense measures. One type of defense measure is: as an example, Fig.12 As shown, the injection of the surfactant SF and the pure water PW into the dissolving tank 52 is interrupted. More specifically, when the bubble BRM1 penetrates into the gas flow path 53, the liquid detection sensor 73 detects the penetrated bubble BRM1 and a detection signal is output from the liquid detection sensor 73, the control unit 13 causes the pump (at Fig.12 "Pump for supplying surfactant and pure water") 56 (refer to Figure 2 ) is stopped and the valve is closed (at Fig.12 "Valves for surfactants and pure water") 57 (ref. Figure 2 ). The control unit 13, the pump 56, and the valve 57 are an example of the "mechanism for interrupting the injection of the liquid into the tank" according to the present invention.

[0102] In this way, by interrupting the injection of the surfactant SF and the pure water PW into the dissolving tank 52, the pressure applied to the gas flow path 53, that is, the positive pressure in the direction from the dissolving tank 52 toward the filter 86 is reduced. Therefore, it is difficult for the bubbles BRM1 immersed in the gas flow path 53 to reach the filter 86. In addition, the bubble BRM1 does not further penetrate into the gas flow path 53. Therefore, according to such a structure, the following effect can be exerted: the filter 86 is less likely to be clogged than before, and the occurrence of inconveniences caused by the clogging of the filter 86 can be suppressed.

[0103] Another defensive measure is: as an example, Fig.13 More specifically, when the bubble BRM1 is immersed in the gas flow path 53, the liquid detection sensor 73 detects the immersed bubble BRM1 and outputs a detection signal from the liquid detection sensor 73, the control unit 13 closes the valve (at Fig.13Indicated as "valve of branch flow path") 85 (refer to Figure 2 ), and the gas flow path 53 is closed. Thus, when the gas flow path 53 is closed, since gas-liquid exchange cannot be performed, the injection of the surfactant SF and the pure water PW into the dissolving tank 52 must be interrupted. Incidentally, the discharge of the first raw material RM1 from the dissolving tank 52 must also be interrupted. The control unit 13 and the valve 85 are an example of the "mechanism for implementing the closing of the gas flow path" involved in the present invention.

[0104] Thus, by closing the gas flow path 53, the bubbles BRM1 immersed in the gas flow path 53 are difficult to reach the filter 86. Therefore, according to such a structure, the filter 86 is less likely to be clogged than before, and the occurrence of problems caused by the clogging of the filter 86 can be suppressed.

[0105] Modification 2 As an example, Fig.14 As shown, a valve 95 may be provided between the liquid detection sensor 73 and the curved portion 71 in the main flow path 70 , and the gas flow path 53 may be closed by closing the valve 95 instead of the valve 85 .

[0106] Modification 3 In addition, as an example, Fig.15 As shown, the gas flow path 53 may be closed by a drain valve 100 which is a three-way valve. The drain valve 100 is connected to the lower end of the descending section 78, one end of the relay section 80, and one end of the drain flow path 82.

[0107] When the bubble BRM1 is not immersed in the gas flow path 53 and the detection signal is not output from the liquid detection sensor 73, the control unit 13 opens the gas flow path 53 side of the drain valve 100 and closes the second drain flow path 82 side. That is, when the detection signal is not output from the liquid detection sensor 73, the control unit 13 opens the gas flow path 53 and closes the second drain flow path 82.

[0108] On the other hand, as an example, Fig.16 As shown, when the bubble BRM1 is immersed in the gas flow path 53, the liquid detection sensor 73 detects the immersed bubble BRM1 and a detection signal is output from the liquid detection sensor 73, the control unit 13 closes the gas flow path 53 side of the drain valve 100 and opens the second drain flow path 82 side. That is, when the detection signal is output from the liquid detection sensor 73, the control unit 13 closes the gas flow path 53 and opens the second drain flow path 82. In this way, by closing the gas flow path 53, it is difficult for the bubble BRM1 immersed in the gas flow path 53 to reach the filter 86. In addition, by opening the second drain flow path 82, the bubble BRM1 immersed in the gas flow path 53 is discharged into the drain tank 67 through the second drain flow path 82.

[0109] Fig.15 and Fig.16 The example shown in the figure is an example in which both the discharge of the bubble BRM1 and the closing of the gas flow path 53 are performed when the liquid detection sensor 73 detects the bubble BRM1. In this way, the first embodiment and the second embodiment described above can also be implemented in combination. When the liquid detection sensor 73 detects the bubble BRM1, all operations of the discharge of the bubble BRM1, the interruption of the injection of the surfactant SF and the pure water PW into the dissolving tank 52, and the closing of the gas flow path 53 can be performed.

[0110] Here, closing the gas flow path 53 means that any part of the gas flow path 53 from the dissolving tank 52 to the filter 86 is closed in order to prevent the bubble BRM1 from reaching the filter 86. In the modification 3, when the detection signal is output from the liquid detection sensor 73, the gas flow path 53 is connected to the second drain flow path 82 through the drain valve 100. Therefore, the gas flow path 53 is opened through the second drain flow path 82. However, the gas flow path 53 from the dissolving tank 52 to the filter 86 is closed by the drain valve 100. Therefore, in the modification 3, it can be said that the gas flow path 53 is closed.

[0111] Modification 4 As an example, Fig.17 As shown, a cleaning mechanism 110 for cleaning the gas flow path 53 immersed in the bubble BRM1 can be provided. The cleaning mechanism 110 has a storage tank 111, an introduction flow path 112, a pump 113 and a switching valve 114. The storage tank 111 stores a cleaning liquid CL. The cleaning liquid CL is, for example, pure water PW. Therefore, the storage tank 51 can also serve as the storage tank 111. One end of the introduction flow path 112 is connected to the lower part of the storage tank 111. The other end of the introduction flow path 112 is connected to the switching valve 114. The switching valve 114 is arranged between the dissolution tank 52 of the main flow path 70 and the liquid detection sensor 73. Therefore, the cleaning liquid CL is introduced into the portion between the dissolution tank 52 and the liquid detection sensor 73 of the main flow path 70.

[0112] The pump 113 is provided in the introduction flow path 112. The pump 113 is driven under the control of the control unit 13. The pump 113 sends the cleaning liquid CL to the switching valve 114 at a set speed. The switching valve 114 is opened and closed under the control of the control unit 13.

[0113] When the bubble BRM1 enters the gas flow path 53, the liquid detection sensor 73 detects the entered bubble BRM1 and outputs a detection signal from the liquid detection sensor 73, the control unit 13 opens the drain valve 83 and opens the second drain flow path 82. In addition, the control unit 13 drives the pump 113, opens the introduction flow path 112 side of the switching valve 114, and connects the main flow path 70 to the introduction flow path 112. In this way, by connecting the main flow path 70 and the introduction flow path 112, the cleaning liquid CL is introduced from the introduction flow path 112 to the main flow path 70 via the switching valve 114. Then, the gas flow path 53 is cleaned by the introduced cleaning liquid CL.

[0114] The cleaning liquid CL flowing from the switching valve 114 to the dissolving tank 52 side is recovered in the dissolving tank 52 through the main flow path 70 on the dissolving tank 52 side. On the other hand, the cleaning liquid CL flowing from the switching valve 114 to the liquid detection sensor 73 side is recovered in the drain tank 67 through the main flow path 70 on the liquid detection sensor 73 side, the descending section 78 of the curved portion 71, and the second drain flow path 82.

[0115] According to the cleaning mechanism 110, the gas flow path 53 contaminated by the immersion of the bubble BRM1 can be cleaned, and the cleanliness of the gas flow path 53 can be maintained. In addition, the cleaning mechanism 110 has an introduction flow path 112 for introducing the cleaning liquid CL into the portion between the dissolution tank 52 and the liquid detection sensor 73 of the gas flow path 53. Therefore, the portion between the dissolution tank 52 and the liquid detection sensor 73 of the gas flow path 53 can be cleaned, and the cleanliness of the portion can be maintained.

[0116] Sometimes, the pure water PW as the solvent component of the bubble BRM1 immersed in the gas flow path 53 may volatilize, and the surfactant SF as the solid component may precipitate. In this case, the pollutants in the gas flow path 53 may be brought into the dissolution tank 52 together with the precipitated surfactant SF by the gas introduced from the gas flow path 53. Therefore, it is very important to keep the gas flow path 53 clean.

[0117] When the surfactant SF is precipitated in the detection portion of the liquid detection sensor 73, the infiltrated bubble BRM1 may not be accurately detected. Therefore, it is important to keep the portion between the dissolution tank 52 of the gas flow path 53 and the liquid detection sensor 73, especially the liquid detection sensor 73, clean.

[0118] In addition, although an example in which the cleaning liquid CL flows to both the dissolving tank 52 side and the liquid detection sensor 73 side has been described, the present invention is not limited thereto. A structure in which the cleaning liquid CL flows only to either the dissolving tank 52 side or the liquid detection sensor 73 side may also be adopted. In addition, although an example in which the cleaning liquid CL flowing to the dissolving tank 52 side is recovered to the dissolving tank 52 has been described, the present invention is not limited thereto. A switching valve, a drainage flow path, and a drainage tank may be provided on the main flow path 70 on the dissolving tank 52 side, and the cleaning liquid CL flowing to the dissolving tank 52 side may be discharged into the drainage tank through the switching valve and the drainage flow path. Alternatively, when the cleaning mechanism 110 is operated, the first raw material RM1 in the dissolving tank 52 may be completely discharged to empty the dissolving tank 52, and the inside of the dissolving tank 52 may also be cleaned using the cleaning liquid CL.

[0119] Modification 5 As an example, Fig.18 As shown, a defoaming mechanism 120 may be provided in the dissolving tank 52. The defoaming mechanism 120 includes a mounting member 121, a suction port 122, an internal rotating body 123, a motor 124, and a liquid outlet 125. The suction port 122, the internal rotating body 123, and the liquid outlet 125 are arranged below the mounting member 121, and the motor 124 is arranged above the mounting member 121. The defoaming mechanism 120 is an example of the "immersion suppression mechanism" involved in the present invention.

[0120] The defoaming mechanism 120 is mounted on a mounting hole 126 formed on the upper portion of the dissolving tank 52 through a mounting member 121. Therefore, the suction port 122, the internal rotating body 123, and the liquid outlet 125 are arranged in the dissolving tank 52. The suction port 122 faces the liquid surface of the first raw material RM1 in the dissolving tank 52. The suction port 122 sucks the first raw material RM1, more precisely, the bubbles BRM1 generated on the liquid surface, into the defoaming mechanism 120. The internal rotating body 123 is rotated at a set speed by the motor 124. The motor 124 is driven under the control of the control unit 13. The internal rotating body 123 crushes the bubbles BRM1 sucked by the suction port 122. The liquid outlet 125 returns the first raw material RM1 crushed by the internal rotating body 123 to the dissolving tank 52.

[0121] According to such defoaming mechanism 120, it is possible to reduce the bubbles BRM1 which are the root cause of the clogging of the filter 86. It is possible to further ensure the effect that the filter 86 is less likely to be clogged than in the past, and the occurrence of problems caused by the clogging of the filter 86 can be suppressed.

[0122] The curved portion 71 may be a portion formed by connecting the descending section 78 and the relay section 80, and the relay section 80 and the ascending section 79 in a curve. In addition, the curved portion 71 may be a V-shaped portion consisting of only the descending section 78 and the ascending section 79 without the relay section 80. Furthermore, the descending section 78 and the ascending section 79 may have both a straight section and a curved section. In addition, the descending section 78 and the ascending section 79 may be stepped. In short, the shape of the curved portion 71 is not particularly limited as long as it includes the descending section 78 and the ascending section 79.

[0123] The surfactant SF is not particularly limited as long as it is a compound having a hydrophilic group and a hydrophobic group (lipophilic group) in one molecule, and examples thereof include nonionic surfactants and anionic surfactants.

[0124] From the viewpoint of achieving better cleaning performance, the chemical solution CS preferably contains a surfactant SF. Surfactant SF often has at least one hydrophobic group selected from the group consisting of aliphatic hydrocarbon groups, aromatic hydrocarbon groups, and groups formed by combining these. The total number of carbon atoms in surfactant SF is preferably 16 to 100.

[0125] Examples of the nonionic surfactant include ester-type nonionic surfactants, ether-type nonionic surfactants, and ester-ether-type nonionic surfactants. Among them, ether-type nonionic surfactants are preferred.

[0126] As the nonionic surfactant, for example, the compounds exemplified in paragraph 0126 of International Publication No. 2022 / 044893 can also be cited, and the contents thereof are incorporated into the present specification.

[0127] Examples of the anionic surfactant include phosphate surfactants having a phosphate group, sulfonic acid surfactants having a sulfonic group, phosphonic acid surfactants having a phosphonic acid group, carboxylic acid surfactants having a carboxyl group, and sulfate surfactants having a sulfate group.

[0128] As the anionic surfactant, for example, the compounds exemplified in paragraphs 0116 to 0123 of International Publication No. 2022 / 044893 can also be cited, and the contents thereof are incorporated into the present specification.

[0129] The content of surfactant SF is preferably 0.0001 to 1.0 mass %, more preferably 0.001 to 0.8 mass %, relative to the total mass of the drug solution CS. Surfactant SF may be used alone or in combination. When two or more surfactants SF are used, their total content is preferably within the above range.

[0130] The solvent is not particularly limited as long as it does not affect the semiconductor substrate, and the exemplified pure water PW, distilled water or ion exchange water can be used. From the viewpoint of having a smaller impact on the semiconductor substrate, pure water PW or ion exchange water is preferred. The water content can be the remainder of the components that can be included in the drug solution CS. The water content is preferably 50.0 to 99.99% by mass, more preferably 60.0 to 98.0% by mass, and further preferably 65.0 to 85.0% by mass relative to the total mass of the drug solution CS.

[0131] From the viewpoint of improving the removal performance of metal-containing substances, the chemical solution CS preferably contains an organic acid. An organic acid is an organic compound having an acidic functional group. Examples of the acidic functional group include a carboxyl group, a phosphonic acid group, a sulfonic acid group, a phenolic hydroxyl group, and a mercapto group. In addition, in this specification, it is assumed that the organic acid does not contain a compound that functions as the above-mentioned anionic surfactant.

[0132] The organic acid is not particularly limited, and examples thereof include carboxylic acids having a carboxyl group in the molecule (organic carboxylic acids), phosphonic acids having a phosphonic acid group in the molecule (organic phosphonic acids), and sulfonic acids having a sulfonic group in the molecule (organic sulfonic acids). Among them, carboxylic acids or phosphonic acids are preferred.

[0133] The number of functional groups possessed by the organic acid is not particularly limited, but is preferably 1 to 4, and more preferably 1 to 3. In addition, from the viewpoint of achieving a better cleaning performance, the organic acid is preferably a compound having a chelating function with the metal contained in the residue, and more preferably a compound having two or more functional groups (ligands) that form a coordination bond with the metal ion in the molecule. As the ligand, the above-mentioned acidic functional groups can be cited, and preferably a carboxylic acid group or a phosphonic acid group.

[0134] The carboxylic acid may be a monocarboxylic acid having one carboxyl group or a polycarboxylic acid having two or more carboxyl groups. From the viewpoint of better cleaning performance, a polycarboxylic acid having two or more (more preferably 2 to 4, and even more preferably 2 or 3) carboxyl groups is preferred.

[0135] Examples of the carboxylic acid include aminopolycarboxylic acids, amino acids, hydroxycarboxylic acids, and aliphatic carboxylic acids.

[0136] Aminopolycarboxylic acid is a compound having one or more amino groups and two or more carboxyl groups as ligands in the molecule. Examples of aminopolycarboxylic acid include aspartic acid, glutamic acid, butanediaminetetraacetic acid, diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetrapropionic acid, triethylenetetraaminehexaacetic acid, 1,3-diamino-2-hydroxypropane-N,N,N',N'-tetraacetic acid, propylenediaminetetraacetic acid, ethylenediaminetetraacetic acid (EDTA), trans-1,2-cyclohexanediaminetetraacetic acid (CyDTA: 1,2-cyclohexanediaminetetraacetic acid acid), ethylenediaminediacetic acid, ethylenediaminedipropionic acid, 1,6-hexanediamine-N,N,N',N'-tetraacetic acid, N,N-bis(2-hydroxybenzyl)ethylenediamine-N,N-diacetic acid, diaminopropanetetraacetic acid, 1,4,7,10-tetraazacyclododecane-tetraacetic acid, diaminopropanoltetraacetic acid, (hydroxyethyl)ethylenediaminetriacetic acid, and iminodiacetic acid (IDA). Among them, DTPA, EDTA, CyDTA or IDA is preferred.

[0137] Amino acid is a compound having one carboxyl group and one or more amino groups in a molecule. As amino acid, for example, glycine, serine, α-alanine (2-aminopropionic acid), β-alanine (3-aminopropionic acid), lysine, leucine, isoleucine, cystine, cysteine, methionine, ethionine, threonine, tryptophan, tyrosine, valine, histidine, histidine derivatives, asparagine, glutamine, arginine, proline, phenylalanine, compounds described in paragraphs 0021 to 0023 of Japanese Patent Publication No. 2016-086094, and their salts. In addition, as histidine derivatives, compounds described in Japanese Patent Publication No. 2015-165561 and Japanese Patent Publication No. 2015-165562 can be cited, and their contents are incorporated into this specification. In addition, as salts, alkali metal salts such as sodium salts and potassium salts, ammonium salts, carbonates, and acetates can be mentioned.

[0138] Among them, histidine, histidine derivatives, or sulfur-containing amino acids containing sulfur atoms are preferred, and histidine or sulfur-containing amino acids are more preferred. Examples of sulfur-containing amino acids include cystine, cysteine, ethionine, and methionine, and cystine or cysteine ​​is preferred.

[0139] Hydroxycarboxylic acids are compounds having one or more hydroxyl groups and one or more amino groups in the molecule. Examples of hydroxycarboxylic acids include malic acid, citric acid, glycolic acid, gluconic acid, heptanoic acid, tartaric acid, and lactic acid, preferably gluconic acid, glycolic acid, malic acid, tartaric acid, or citric acid, and more preferably gluconic acid or citric acid.

[0140] Examples of the aliphatic carboxylic acid include oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, sebacic acid, and maleic acid. Among them, adipic acid is preferred from the viewpoint of enhancing the effect of the present invention and the cleaning performance.

[0141] Examples of carboxylic acids other than the aminopolycarboxylic acids, amino acids, hydroxycarboxylic acids and aliphatic carboxylic acids include monocarboxylic acids, and examples of monocarboxylic acids include lower (carbon number 1 to 4) aliphatic monocarboxylic acids such as formic acid, acetic acid, propionic acid and butyric acid.

[0142] The carboxylic acid is preferably an amino acid, a hydroxycarboxylic acid or an aliphatic carboxylic acid, more preferably cystine, cysteine, histidine, gluconic acid, glycolic acid, malic acid, tartaric acid, citric acid or adipic acid, further preferably cysteine, gluconic acid, citric acid or adipic acid.

[0143] The carboxylic acid may be used alone or in combination of two or more. The content of the carboxylic acid is not particularly limited, but is preferably 0.1 to 35.0% by mass, more preferably 1.0 to 35.0% by mass, relative to the total mass of the chemical solution CS.

[0144] The phosphonic acid may be a monophosphonic acid having one phosphonic acid group or a polyphosphonic acid having two or more phosphonic acid groups. From the viewpoint of achieving a more excellent cleaning performance, a polyphosphonic acid having two or more phosphonic acid groups is preferred.

[0145] As the polyphosphonic acid, the compounds represented by the general formulas 1 to 3 described in paragraphs 0013 to 0023 of the specification of International Publication No. 2013 / 162020, the compounds described in paragraphs 0026 to 0036 of the specification of International Publication No. 2018 / 020878, and the compounds ((co)polymers) described in paragraphs 0031 to 0046 of the specification of International Publication No. 2018 / 030006 can be cited, and their contents are incorporated into the present specification.

[0146] Examples of the polyphosphonic acid include ethylenediphosphonic acid, 1-hydroxyethylene-1,1'-diphosphonic acid (HEDPO: 1-hydroxyethane-1,1-diphosphonic acid), 1-hydroxypropylene-1,1'-diphosphonic acid, 1-hydroxybutylene-1,1'-diphosphonic acid, ethylaminobis(methylenephosphonic acid), dodecylaminobis(methylenephosphonic acid), nitrilotris(methylphosphonic acid) (NTPO: nitrilotris(methylphosphonic acid)), ethylenediaminebis(methylenephosphonic acid) (EDDPO: ethylenebis imino(methylene bisphosphonic acid)), 1,3-propylenediaminebis(methylenephosphonic acid), ethylenediaminetetra(methylenephosphonic acid) (EDTPO: ethylene diamine tetra(methylene phosphonic acid)), 1,3-propylenediaminetetra(methylenephosphonic acid) (PDTMP: propylenediamine tetra(methylene phosphonic acid) acid), 1,2-diaminopropane tetrakis(methylenephosphonic acid), 1,6-hexanediaminetetrakis(methylenephosphonic acid), diethylenetriaminepenta(methylenephosphonic acid) (DEPPO: diethylenetriaminepenta(methylenephosphonic acid)), diethylenetriaminepenta(ethylenephosphonic acid), triethylenetetraaminehexa(methylenephosphonic acid), and triethylenetetraaminehexa(ethylenephosphonic acid). Among them, HEDPO is preferred.

[0147] The number of phosphonic acid groups in phosphonic acid is preferably 2 to 5, more preferably 2 to 4, and even more preferably 2 or 3. The number of carbon atoms in phosphonic acid is preferably 12 or less, more preferably 10 or less, and even more preferably 8 or less. The lower limit is not particularly limited, but is preferably 1 or more.

[0148] The phosphonic acid may be used alone or in combination of two or more. The content of the phosphonic acid is not particularly limited, but is preferably 0.001 to 5.0% by mass, more preferably 0.01 to 2.0% by mass, relative to the total mass of the chemical solution CS.

[0149] The organic acid is preferably a low molecular weight. More specifically, the molecular weight of the organic acid is preferably 600 or less, more preferably 450 or less, and further preferably 300 or less. The lower limit of the molecular weight of the organic acid is not particularly limited, but is preferably 85 or more. In addition, the number of carbon atoms in the organic acid is preferably 15 or less, more preferably 12 or less, and further preferably 8 or less. The lower limit of the number of carbon atoms in the organic acid is not particularly limited, but is preferably 1 or more.

[0150] The organic acid may be used alone or in combination of two or more thereof. The content of the organic acid is not particularly limited, but is preferably 0.1 to 40% by mass, more preferably 1.0 to 35% by mass, relative to the total mass of the chemical solution CS.

[0151] From the viewpoint of achieving more excellent cleaning performance, the chemical solution CS preferably contains carboxylic acid and phosphonic acid.

[0152] The chemical solution CS may contain other components in addition to the above. Examples of other components include pH regulators (e.g., alkaline compounds and acidic compounds), organic solvents (e.g., alcohol solvents, glycol solvents, glycol ether solvents, and ketone solvents), water-soluble polymers (e.g., water-soluble polymers described in paragraphs 0043 to 0047 of Japanese Patent Application Laid-Open No. 2016-171294), and oxidants (e.g., peroxides, persulfides, and percarbonates, their acids, and their salts).

[0153] The properties of the chemical solution CS are described in detail below.

[0154] The drug solution CS may be alkaline or acidic. The pH of the drug solution CS is preferably 0.10 to 4.00. The pH of the drug solution CS may be adjusted using the above-mentioned pH adjusting agent. The pH of the drug solution CS may be measured using a known pH tester using a method according to JIS (Japanese Industrial Standards) Z8802-1984. The measurement temperature is set to 25°C.

[0155] The content (measured as ion concentration) of metals (e.g., metal elements such as Fe, Co, Na, Cu, Mg, Mn, Li, Al, Cr, Ni, Zn, Sn, and Ag) contained as impurities in the chemical solution CS is preferably 5 mass ppm or less, and more preferably 1 mass ppm or less. In the manufacture of the most advanced semiconductor elements, it is expected that a chemical solution CS with a higher purity will be required. Therefore, the metal content is further preferably a value lower than 1 mass ppm, that is, lower than the mass ppb level, particularly preferably lower than 100 mass ppb, and most preferably lower than 10 mass ppb. As the lower limit, it is preferably 0.

[0156] The drug solution CS may also contain coarse particles, but the content thereof is preferably small. Coarse particles refer to particles having a diameter (particle size) of 0.03 μm or more when the particle shape is regarded as a sphere. The coarse particles contained in the drug solution CS refer to particles such as dust, dirt, organic solids, and inorganic solids contained as impurities in the raw materials; and particles such as dust, dirt, organic solids, and inorganic solids introduced as contaminants in the preparation of the drug solution CS, which are equivalent to substances that do not dissolve in the drug solution CS and exist as particles.

[0157] The content of coarse particles in the drug solution CS is preferably 10,000 or less, and more preferably 5,000 or less, per 1 mL of the drug solution CS. As for the lower limit, it is preferably 0 or more, and more preferably 0.01 or more, per 1 mL of the drug solution CS. The content of coarse particles present in the drug solution CS can be measured in the liquid phase using a commercially available measuring device of a light scattering liquid particle measuring method using a laser as a light source.

[0158] The material of the filter 21 and 37 can include, for example, polyamides such as 6-nylon and 6,6-nylon, polyethylene, polypropylene, polystyrene, polyimide, polyamide-imide, and fluororesin. Polyimide and polyamide-imide may also have at least one selected from the group consisting of a carboxyl group, a salt-type carboxyl group, and an -NH- bond. Regarding solvent resistance, fluororesin, polyimide, and polyamide-imide are excellent. In addition, from the viewpoint of adsorbing metal ions, polyamides such as 6-nylon and 6,6-nylon are preferred, and nylon is more preferred.

[0159] The filters 21 and 37 may also be structures having metal ion adsorption filters and organic impurity adsorption filters. As metal ion adsorption filters, preferably, filters capable of ion exchange are used. As metal ion adsorption filters, for example, polyimide and / or polyamide-imide porous membranes described in Japanese Patent Publication No. 2016-155121 may be cited.

[0160] The organic impurity adsorption filter is not particularly limited, and a known organic impurity adsorption filter can be cited. Among them, as the organic impurity adsorption filter, from the viewpoint of improving the adsorption performance of organic impurities, it is preferred that the surface of the filter has an organic skeleton that can interact with the organic impurities, in other words, the surface is modified by the organic skeleton that can interact with the organic impurities. In addition, the organic impurity adsorption filter can also use a filter in which activated carbon is fixed to a non-woven fabric as described in Japanese Patent Publication No. 2002-273123 and Japanese Patent Publication No. 2013-150979.

[0161] The filters 21 and 37 are not particularly limited as long as they are filters that have been used for filtering purposes. For example, filters made of fluororesins such as polytetrafluoroethylene (PTFE) and tetrafluoroethylene perfluoroalkyl vinyl ether copolymers, polyamide resins such as nylon, and polyolefin resins (including high-density or ultra-high molecular weight) such as polyethylene and polypropylene (PP) can be cited. Among these materials, a material selected from the group consisting of polyethylene, polypropylene (including high-density polypropylene), fluororesins (including PTFE and PFA), and polyamide resins (including nylon) is preferred, and fluororesins are more preferred.

[0162] The semiconductor element to which the chemical solution CS is applied is not particularly limited. More specifically, examples of semiconductor elements include logic LSI (Large Scale Integration), ASIC (Application Specific Integrated Circuit), FPGA (Field Programmable Gate Array), ASSP (Application Specific Standard Product), and microprocessors (e.g., CPU, GPU (Graphics Processing Unit), etc.).In addition, there can be mentioned memories (e.g., DRAM (Dynamic Random Access Memory), SRAM (Static Random Access Memory), HMC (Hybrid Memory Cube), MRAM (Magnetic RAM), PCM (Phase-Change Memory), ReRAM (Resistive RAM), FeRAM (Ferroelectric RAM), flash memory, etc.), LED (Light Emitting Diode), power devices, analog IC (Integrated Circuit), such as DC (Direct Current)-DC converters, insulated gate bipolar transistors (IGBT: Insulated Gate Bipolar Transistor), MEMS (Micro Electro Mechanical Systems) such as acceleration sensors, pressure sensors, vibrators, gyroscope sensors, etc., such as GPS (Global Positioning System), FM (Frequency Modulation), NFC (Near field communication), RFEM (RF Expansion Module, RF extension module), MMIC (Monolithic Microwave Integrated Circuit), WLAN (Wireless Local Area Network), discrete components, BSI (Back Side Illumination), CIS (Contact Image Sensor), camera module, passive components, SAW (Surface Acoustic Wave) filter, RF (Radio Frequency) filter, RFIPD (Radio Frequency Integrated Passive Devices), BB (Broadband), etc.

[0163] The composition of the semiconductor constituting the semiconductor element is not particularly limited. Examples of the composition of the semiconductor include diamond, silicon (Si), germanium (Ge), silicon germanium (SiGe), silicon carbide (SiC), gallium arsenide (GaAs), gallium nitride (GaN), gallium oxide, and silicon on insulator (SOI).

[0164] The above description is only the preferred embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A device for producing a chemical solution for semiconductor manufacturing, characterized in that: include: a tank that contains at least one liquid as a raw material of the liquid medicine and performs injection and discharge of the liquid; a gas flow path, one end of which is connected to the tank and the other end of which is open to the outside and is used to introduce and discharge gas into and out of the tank when the liquid is injected and discharged; a filter disposed in the gas flow path and filtering the gas sucked in or discharged from the open end of the gas flow path; a curved portion constituting a part of the gas flow path, including a descending section descending toward the filter in a direction from the tank toward the filter, and an ascending section ascending toward the filter after the descending section; a liquid detection sensor disposed in the gas flow path closer to the tank than the ascending section, and detecting liquid immersed in the gas flow path; and A mechanism that, when the liquid detection sensor detects the liquid, performs at least one of discharging the liquid immersed in the gas flow path, interrupting the injection of the liquid into the tank, and closing the gas flow path.

2. The semiconductor manufacturing liquid manufacturing device according to claim 1, characterized in that: The mechanism includes a liquid discharge mechanism for discharging the liquid immersed in the gas flow path when the liquid detection sensor detects the liquid.

3. The semiconductor manufacturing liquid chemical manufacturing device according to claim 2, characterized in that: The liquid discharge mechanism includes a liquid discharge flow path connected to the gas flow path between the liquid detection sensor and the filter.

4. The semiconductor manufacturing liquid chemical manufacturing device according to claim 3, characterized in that: The drainage flow path is connected to the bent portion.

5. The semiconductor manufacturing liquid chemical manufacturing device according to claim 4, characterized in that: The drainage channel is connected to the lower end of the curved portion.

6. The semiconductor manufacturing liquid manufacturing device according to claim 1, characterized in that: The inner wall surface of the tank is provided with a fluororesin layer.

7. The semiconductor manufacturing liquid manufacturing device according to claim 1, characterized in that: The bent portion is provided with a liquid storage portion for storing the liquid immersed in the gas flow path.

8. The semiconductor manufacturing liquid manufacturing device according to claim 1, characterized in that: The liquid detection sensor is provided in the gas flow path closer to the tank than the bent portion.

9. The semiconductor manufacturing liquid chemical manufacturing apparatus according to claim 1, wherein: The invention also includes a cleaning mechanism for cleaning the gas flow path immersed in the liquid.

10. The semiconductor manufacturing liquid chemical manufacturing device according to claim 9, characterized in that: The cleaning mechanism includes an introduction flow path that introduces cleaning liquid into the gas flow path portion between the tank and the liquid detection sensor.

11. The semiconductor manufacturing liquid chemical manufacturing device according to claim 1, characterized in that: The gas flow path includes a plurality of branch flow paths each having the open end, and the filter is provided in each of the branch flow paths.

12. The semiconductor manufacturing liquid chemical manufacturing apparatus according to claim 1, wherein: The device further includes an infiltration suppression mechanism that suppresses the liquid in a bubble state generated on the liquid surface in the tank from infiltrating into the gas flow path.

13. The semiconductor manufacturing liquid chemical manufacturing apparatus according to claim 1, wherein: The liquid comprises a surfactant.

14. The semiconductor manufacturing liquid chemical manufacturing apparatus according to claim 1, wherein: The tank is a dissolution tank for dissolving a solute in a solvent.

15. A method for producing a chemical solution for semiconductor manufacturing, characterized in that: The method comprises the steps of using the semiconductor manufacturing chemical solution manufacturing apparatus according to any one of claims 1 to 14 to perform the manufacturing process.

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