Apparatus and method for producing cleaning water for electronic devices

Abstract

To provide a manufacturing apparatus capable of manufacturing cleaning water for an electronic device at a large flow rate.SOLUTION: An apparatus for producing washing water for electronic devices, the apparatus comprising: a pH adjusting apparatus that adds a pH adjuster to ultrapure water to prepare pH adjusted water; a degassing apparatus that degasses the pH adjusted water; a gas dissolving membrane apparatus that dissolves a functional gas in the degassed pH adjusted water via a gas permeable membrane to prepare washing water; and a transfer line capable of transferring each of the ultrapure water, the pH adjusted water, and the washing water at a flow rate of 25L / min or more.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present disclosure relates to an apparatus for producing cleaning water for electronic devices and a method for producing the cleaning water. [Background technology]

[0002] In the manufacturing process of electronic devices such as semiconductor devices, contaminants on the surface of electronic devices can lead to deterioration of the performance of the electronic devices or a decrease in the yield of the manufacturing line. For this reason, the surfaces of electronic devices are cleaned using ultrapure water or cleaning water prepared by dissolving chemicals in ultrapure water. Conventionally, cleaning water prepared by dissolving ammonia, hydrogen gas, etc. in ultrapure water as raw water has been used as the cleaning water (see, for example, Patent Documents 1 to 3). [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Application Publication No. 10-064867 [Patent Document 2] Japanese Patent Application Laid-Open No. 2000-354729 [Patent Document 3] Japanese Patent Application Publication No. 2018-022749 Summary of the Invention [Problem to be solved by the invention]

[0004] In recent years, with the improvement in the performance of electronic devices, the miniaturization of circuit fabrication technology has progressed significantly. Since even the smallest amount of contaminants can cause problems, the amount of cleaning water used is increasing year by year. An object of the present disclosure is to provide a manufacturing apparatus capable of producing cleaning water for electronic devices at a large flow rate. [Means for solving the problem]

[0005] One aspect of the apparatus for producing cleaning water for electronic devices according to the present disclosure includes: a pH adjusting device that prepares pH-adjusted water by adding a pH adjuster to ultrapure water; a degassing device for degassing the pH-adjusted water; a gas-dissolving membrane type device that dissolves a functional gas in the degassed pH-adjusted water via a gas-permeable membrane to prepare cleaning water; transfer lines capable of transferring the ultrapure water, the pH-adjusted water, and the cleaning water at a flow rate of 25 L / min or more; Equipped with. [Effects of the Invention]

[0006] The apparatus for producing cleaning water for electronic devices according to the present disclosure can produce cleaning water at a large flow rate. [Brief explanation of the drawings]

[0007] [Figure 1] FIG. 1 is a block diagram that schematically shows one embodiment of an apparatus for producing cleaning water. [Figure 2] FIG. 2 is a block diagram that schematically shows one embodiment of an apparatus for producing cleaning water. [Figure 3] FIG. 3 is a block diagram that schematically shows one embodiment of an apparatus for producing cleaning water. DETAILED DESCRIPTION OF THE INVENTION

[0008] In this specification, the numerical range N1 to N2 means N1 or more and N2 or less. In this specification, when the units of the numerical values ​​written before and after "~" indicating a numerical range are the same, the unit of the numerical value written before "~" may be omitted.

[0009] [Electronic device cleaning water manufacturing equipment] Hereinafter, embodiments of the present disclosure will be described in detail with reference to the drawings. The manufacturing apparatus for cleaning water for electronic devices of the present disclosure (hereinafter also simply referred to as the "manufacturing apparatus of the present disclosure") comprises a pH adjusting apparatus that adds a pH adjuster to ultrapure water to prepare pH-adjusted water, a degassing apparatus that degasses the pH-adjusted water, a gas-dissolving membrane type apparatus that prepares cleaning water by dissolving a functional gas in the degassed pH-adjusted water via a gas-permeable membrane, and transfer lines that can transport the ultrapure water, pH-adjusted water, and cleaning water at a flow rate of 25 L / min or more.

[0010] The manufacturing apparatus of the present disclosure produces cleaning water for electronic devices from ultrapure water. Ultrapure water is produced, for example, by removing ionic substances, organic matter, dissolved gases, and particulates from raw water. Examples of raw water include city water, well water, river water, lake water, and industrial water. Ultrapure water preferably has a resistivity of 18.1 MΩ·cm or more, particulates with a particle size of 50 nm or more and 1000 particles / L or less, viable bacteria of 1 particle / L or less, TOC (Total Organic Carbon) of 1 μg / L or less, total silicon of 0.1 μg / L or less, metals of 1 ng / L or less, ions of 10 ng / L or less, hydrogen peroxide of 30 μg / L or less, and a water temperature of 25±2°C, but is not particularly limited thereto.

[0011] The cleaning water for electronic devices (hereinafter simply referred to as "cleaning water") produced using the manufacturing apparatus of the present disclosure is transported to a point of use (UP). Examples of the point of use include a cleaning apparatus provided in an electronic device manufacturing process apparatus for manufacturing semiconductor devices or the like.

[0012] The manufacturing apparatus of the present disclosure includes a pH adjuster, a degasser, and a gas dissolved film device in this order on the transfer line. Ultrapure water as raw water flowing through the transfer line passes through the pH adjuster to become pH-adjusted water, which passes through the degasser to be degassed, and the degassed pH-adjusted water passes through the gas dissolved film device to become cleaning water.

[0013] The manufacturing apparatus of the present disclosure preferably further comprises a switching device for switching the flow path of the cleaning water, located on the transfer line downstream of the gas dissolved film device. At the switching device, the transfer line branches into, for example, a transfer line connected to a use point of the cleaning water, and a drain line for draining the cleaning water, or a circulation line that joins the transfer line at a junction located upstream of the transfer line and uses the circulated cleaning water.

[0014] <Flow path> In the manufacturing apparatus of the present disclosure, the flow paths (e.g., transfer lines or supply lines) through which ultrapure water, pH-adjusted water, cleaning water, pH adjuster, oxidation-reduction potential adjuster, functional gas, etc. flow are configured, for example, with piping. The flow paths may be provided with equipment such as tanks, pumps, joints, and valves.

[0015] Examples of materials for piping include polymeric materials such as polyvinyl chloride (PVC), polyphenylene sulfide (PPS), polyvinylidene fluoride (PVDF), tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), and polypropylene (PP), as well as fiber-reinforced plastics (FRP) and stainless steel. Of these, PVDF is preferred.

[0016] The raw water, i.e., ultrapure water, pH-adjusted water, and cleaning water, is transferred via a transfer line. The transfer line can deliver water at a flow rate of 25 L / min or more, preferably 25 to 700 L / min, more preferably 30 to 500 L / min, even more preferably 40 to 300 L / min, and particularly preferably 50 to 200 L / min. In the production apparatus of the present disclosure, the flow rate is preferably set within the above range. A production apparatus equipped with such a transfer line can produce cleaning water at a large flow rate. The inner diameter of the pipe constituting the transfer line is, for example, 55 to 300 mm, preferably 60 to 250 mm, and more preferably 70 to 130 mm.

[0017] In an electronic device manufacturing process apparatus, for example, it has changed to a single wafer processing type where each semiconductor wafer is processed one by one, and each wafer may be processed in one chamber. When processing wafers one by one, the manufacturing lead time will be significantly extended. Therefore, a plurality of chambers may be installed in one electronic device manufacturing process apparatus to process wafers simultaneously. As a result, the required flow rate of cleaning water in the electronic device manufacturing process apparatus is also increasing. The manufacturing apparatus of the present disclosure can produce cleaning water with a large flow rate of 25 L / min or more and can meet such requirements.

[0018] <pH Adjustment Device> The manufacturing apparatus of the present disclosure includes a pH adjustment device that prepares pH-adjusted water by adding a pH adjuster to ultrapure water. The pH adjustment device is a device that measures and supplies a pH adjuster to a transfer line of ultrapure water to prepare pH-adjusted water having a desired pH. The pH adjustment device includes, for example, a tank containing a pH adjuster, a supply line for supplying the pH adjuster from the tank to the transfer line, and a pump for adjusting the supply rate of the pH adjuster if desired.

[0019] The pH-adjusted water obtained by adding a pH adjuster to ultrapure water has a higher electrical conductivity than ultrapure water. Therefore, it is possible to suppress the charging of the piping and the liquid flowing inside the piping, and to suppress the mixing of fine particles into the cleaning water.

[0020] The tank containing the pH adjuster may include at least one selected from the group consisting of a device for purging the inside of the tank with an inert gas (for example, N2 gas) and a degassing membrane for removing dissolved gas (for example, dissolved oxygen) in the pH adjuster in the tank.

[0021] Examples of the pump include a diaphragm pump. As the pump, for example, a pressure extrusion type pump may be used in which the pH adjuster is placed in the tank together with an inert gas (for example, N2 gas), and the pH adjuster is extruded by the pressure of the inert gas.

[0022] Examples of pH adjusters include aqueous solutions of alkaline compounds and gaseous alkaline compounds when adjusting the pH of ultrapure water to 7 or higher. The alkaline compound is the active ingredient of the pH adjuster. Examples of alkaline compounds include ammonia, tetramethylammonium hydroxide, 2-hydroxyethyltrimethylammonium hydroxide, sodium hydroxide, and potassium hydroxide. Examples of alkaline compound gases include ammonia gas. One type of alkaline compound may be used, or two or more types may be used.

[0023] Among these, an aqueous ammonia solution or ammonia gas is preferred, and an aqueous ammonia solution is more preferred. By dissolving a small amount of ammonia in ultrapure water, for example, the effect of suppressing dissolution and charging of semiconductor materials can be obtained.

[0024] The concentration of an alkaline compound (e.g., ammonia) in the pH-adjusted water obtained by the pH adjuster is preferably 2 to 100 mg / L, more preferably 5 to 80 mg / L, and even more preferably 10 to 50 mg / L. When an aqueous ammonia solution is used as the pH adjuster, the aqueous ammonia solution is preferably added so that the ammonia concentration in the pH-adjusted water is 2 to 100 mg / L.

[0025] When adjusting the pH of ultrapure water to less than 7, examples of pH adjusters include aqueous solutions of acidic compounds such as hydrochloric acid, nitric acid, sulfuric acid, formic acid, acetic acid, and citric acid, as well as gases such as CO2 gas. The acidic compounds and carbon dioxide gas (CO2 gas) are active ingredients of pH adjusters. One or more types of acidic compounds may be used.

[0026] The pH adjuster is preferably a liquid, more preferably an aqueous solution of an alkaline compound, and even more preferably an aqueous ammonia solution. The mass concentration of the alkaline compound in the aqueous solution of the pH adjuster, for example, the mass concentration of the aqueous ammonia solution, is not particularly limited, but is preferably 20 to 40%, more preferably 25 to 30%.

[0027] When the pH adjuster is a gas, a direct gas-liquid contact device such as a gas permeable membrane module or an ejector may be used as the pH adjuster.

[0028] In one embodiment, the pH adjuster prepares pH-adjusted water having a pH of preferably 8 to 11, more preferably 9 to 11. A pH of 8 or higher tends to suppress the generation of static electricity in various devices located downstream of the pH adjuster. A pH of 11 or lower tends to suppress corrosion of the surface to be cleaned and deterioration of membranes and the like included in a degassing device or a gas-dissolved membrane device.

[0029] In recent years, with the improvement in the performance of electronic devices, there has been great progress in miniaturization of circuit fabrication technology. Because even the smallest amount of contaminants can be a problem, the amount of cleaning water used is increasing year by year. Because cleaning water is produced from ultrapure water, efforts to conserve water are required.

[0030] Cleaning water is produced, for example, by mixing a pH adjuster or dissolving a functional gas in ultrapure water. After the start of cleaning water production, it takes a certain amount of time for the quality of the cleaning water (e.g., the concentration of the active ingredient in the pH adjuster and the concentration of the functional gas) to reach the water quality required by the electronic device manufacturing process equipment (hereinafter also referred to as the "set water quality"). Therefore, when cleaning water is supplied to an electronic device manufacturing process equipment that requires a flow rate of, for example, several tens of L / min or more, the cleaning water may be disposed of as wastewater without being supplied to the process equipment until the quality of the cleaning water reaches the set water quality.

[0031] Here, the supply rate (flow rate) of the pH adjuster in the pH adjuster can be calculated, for example, from the set concentration of the active ingredient of the pH adjuster in the cleaning water, the concentration of the active ingredient in the pH adjuster, and the transfer rate (flow rate) of the ultrapure water. The set concentration of the active ingredient of the pH adjuster in the cleaning water means the concentration of the active ingredient in the cleaning water required at the point of use of the cleaning water, such as in electronic device manufacturing process equipment.

[0032] In one embodiment, the pH adjuster supplies the pH adjuster for a predetermined time at a flow rate (hereinafter also referred to as the "initial flow rate" of the pH adjuster) that is higher than the flow rate of the pH adjuster calculated from the set concentration, etc., in the initial stage of cleaning water production, and after the predetermined time has elapsed, supplies the pH adjuster at the flow rate of the pH adjuster calculated from the set concentration, etc. (hereinafter also referred to as the "set flow rate" of the pH adjuster). The timing for changing the flow rate of the pH adjuster from the initial flow rate to the set flow rate may be when the concentration of the active ingredient of the pH adjuster in the cleaning water reaches the set concentration, or may be before that time. The timing for changing the flow rate of the pH adjuster may be, for example, when the concentration of the active ingredient of the pH adjuster in the cleaning water reaches preferably 50% or more, more preferably 60% or more, even more preferably 70% or more, even more preferably 80% or more, and particularly preferably 90% or more of the set concentration. The predetermined time is not particularly limited, but is preferably within 10 minutes, more preferably within 7 minutes, and even more preferably within 5 minutes.

[0033] This allows for a shorter rise time (time required for the concentration of the active ingredient of the pH adjuster in the cleaning water to reach the set concentration) even when ultrapure water is flowed at a high flow rate to produce cleaning water at a high flow rate. Therefore, the cleaning water production apparatus of the present disclosure can accommodate the cleaning water flow rates (especially high flow rates) required by electronic device manufacturing process equipment, and can reduce the amount of cleaning water produced in which the concentration of the active ingredient of the pH adjuster has not yet reached the set concentration, thereby reducing the amount of wastewater. These points also apply to the oxidation-reduction potential adjuster and functional gas described below.

[0034] The ratio of the initial flow rate of the pH adjuster to the set flow rate in producing the cleaning water (initial flow rate / set flow rate) is preferably more than 1.0 and not more than 10.0, more preferably 1.1 to 8.0, even more preferably 1.2 to 6.0, still more preferably 1.3 to 4.0, and particularly preferably 1.4 to 3.0.

[0035] <Oxidation-reduction potential regulator> The manufacturing apparatus of the present disclosure may further include an oxidation-reduction potential adjuster (hereinafter also referred to as "ORP adjuster") that adjusts the oxidation-reduction potential (hereinafter also referred to as "ORP adjuster") of the ultrapure water or pH-adjusted water. The ORP adjuster is preferably located downstream of the pH adjuster and upstream of the degassing device on the transfer line. Therefore, the ORP of the pH-adjusted water may be adjusted by the ORP adjuster.

[0036] The ORP adjuster is a device that adjusts the ORP of ultrapure water or pH-adjusted water by measuring and supplying an oxidation-reduction potential adjuster (hereinafter also referred to as "ORP adjuster") to the transfer line. The ORP adjuster includes, for example, a tank containing the ORP adjuster, a supply line that supplies the ORP adjuster from the tank to the transfer line, and, if desired, a pump that adjusts the supply rate of the ORP adjuster.

[0037] The tank containing the ORP adjuster may be equipped with at least one selected from the group consisting of a device for purging the tank with an inert gas (e.g., N2 gas) and a degassing membrane for removing dissolved gas (e.g., dissolved oxygen) from the ORP adjuster in the tank.

[0038] The pump may be, for example, a diaphragm pump. Alternatively, a pressure extrusion pump may be used, in which the ORP adjuster is placed in a tank together with an inert gas (e.g., N2 gas) and the pressure of the inert gas is used to extrude the ORP adjuster.

[0039] Examples of ORP adjusters for adjusting the oxidation-reduction potential of the target water higher (positive side) include aqueous solutions such as hydrogen peroxide solution, and gases such as ozone gas and oxygen gas. Examples of ORP adjusters for adjusting the oxidation-reduction potential of the target water lower include aqueous solutions of compounds such as oxalic acid, hydrogen sulfide, and potassium iodide, and gases such as hydrogen gas. One or more of the above compounds may be used. One or more of the above gases may be used.

[0040] When the ORP adjuster is a gas, a direct gas-liquid contact device such as a gas permeable membrane module or an ejector may be used as the ORP adjuster.

[0041] The supply rate (flow rate) of the ORP adjuster in the ORP adjuster can be calculated, for example, from the set concentration of the active ingredient in the ORP adjuster in the cleaning water, the concentration of the active ingredient in the ORP adjuster, and the transfer rate (flow rate) of ultrapure water or pH-adjusted water. The set concentration of the active ingredient in the ORP adjuster in the cleaning water means the concentration of the active ingredient in the cleaning water required at the point of use of the cleaning water, such as in electronic device manufacturing process equipment.

[0042] In one embodiment, the ORP adjusting device supplies the ORP adjuster for a predetermined time at a flow rate (hereinafter also referred to as the "initial flow rate" of the ORP adjuster) that is greater than the flow rate of the ORP adjuster calculated from the above-mentioned set concentration, etc., during the initial stage of cleaning water production, and after the predetermined time has elapsed, supplies the ORP adjuster at the flow rate (hereinafter also referred to as the "set flow rate" of the ORP adjuster) of the ORP adjuster calculated from the above-mentioned set concentration, etc. The timing for changing the flow rate of the ORP adjuster from the initial flow rate to the set flow rate may be when the concentration of the active ingredient of the ORP adjuster in the cleaning water reaches the set concentration, or may be before that time. The timing for changing the flow rate of the ORP adjuster may be, for example, when the concentration of the active ingredient of the ORP adjuster in the cleaning water reaches preferably 50% or more, more preferably 60% or more, even more preferably 70% or more, even more preferably 80% or more, and particularly preferably 90% or more of the set concentration. The predetermined time is not particularly limited, but is preferably within 10 minutes, more preferably within 7 minutes, and even more preferably within 5 minutes.

[0043] The ratio of the initial flow rate of the ORP adjuster to the set flow rate in producing cleaning water (initial flow rate / set flow rate) is preferably more than 1.0 and not more than 10.0, more preferably 1.1 to 8.0, even more preferably 1.2 to 6.0, still more preferably 1.3 to 4.0, and particularly preferably 1.4 to 3.0.

[0044] <Hydrogen peroxide removal device> The manufacturing apparatus of the present disclosure may further include a hydrogen peroxide removal device. For example, it is preferable that at least a portion of the hydrogen peroxide has been removed from the ultrapure water or pH-adjusted water to which the ORP adjuster is supplied. Therefore, the hydrogen peroxide remover is preferably located upstream of the ORP adjuster on the transfer line, and more preferably upstream of the pH adjuster and the ORP adjuster. By providing the hydrogen peroxide remover, the ORP adjuster can accurately control the ORP of the cleaning water.

[0045] The hydrogen peroxide removal device includes, for example, a platinum group metal-supported resin column, which includes a resin (hereinafter also referred to as a "carrier resin") and a platinum group metal supported on the resin. Examples of carrier resins include ion exchange resins. Among ion exchange resins, anion exchange resins are preferred. Platinum group metals are negatively charged, so they are stably supported on anion exchange resins and are less likely to fall off. The exchange groups of the anion exchange resins are preferably in the OH form. The OH-type anion exchange resins have an alkaline resin surface, which promotes the decomposition of hydrogen peroxide. Examples of platinum group metals include ruthenium, rhodium, palladium, osmium, iridium, and platinum. Platinum group metals may be used alone, two or more, or as an alloy of two or more, or purified products of naturally occurring mixtures may be used without separating them into individual elements. Among these, platinum, palladium, platinum / palladium alloys, or mixtures of two or more of these, are preferably used because of their strong catalytic activity. Nano-sized particles of these metals can also be preferably used.

[0046] <Pump> The manufacturing apparatus of the present disclosure may further include a pump. By using the pump, it becomes easy to increase the flow rate and water pressure and produce cleaning water at a large flow rate. The pump pressurizes, for example, ultrapure water, pH-adjusted water, or cleaning water to a predetermined water pressure. The pump is preferably a pump whose pressure can be controlled. The production apparatus of the present disclosure preferably includes a pump between the pH adjuster and the degasser on the transfer line. If the production apparatus includes an ORP adjuster, it is preferable to include a pump between the ORP adjuster and the degasser.

[0047] Examples of pumps include rotary positive displacement pumps that continuously suck in and discharge by changing the volume, reciprocating positive displacement pumps that repeatedly suck in and discharge by changing the volume, and centrifugal pumps that discharge liquid by using centrifugal force or thrust generated by the rotation of an impeller or propeller inside the pump.

[0048] Examples of rotary positive displacement pumps include tube pumps, rotary pumps, gear pumps, and snake pumps. Examples of reciprocating positive displacement pumps include diaphragm pumps and plunger pumps. Examples of centrifugal pumps include volute pumps. Among these, rotary positive displacement pumps and centrifugal pumps are preferred, centrifugal pumps are more preferred, and volute pumps, which are centrifugal pumps, are even more preferred, in that they cause less fluid pulsation and maintain a substantially constant and stable discharge pressure.

[0049] The pressure of the ultrapure water, pH-adjusted water, or cleaning water pressurized by the pump is preferably 0.1 MPa or higher, more preferably 0.2 to 1.0 MPa, even more preferably 0.3 to 0.8 MPa, and particularly preferably 0.4 to 0.6 MPa. If the pressure is 0.1 MPa or higher, a sufficient flow rate of the ultrapure water, pH-adjusted water, or cleaning water is easily obtained. If the pressure is 1.0 MPa or lower, static electricity is less likely to be generated within the pump.

[0050] <Degassing device> The manufacturing apparatus of the present disclosure is equipped with a degassing device that degasses the pH-adjusted water. The degassing device removes at least a portion of the dissolved gases in the pH-adjusted water, reducing the amount of dissolved gases. This removal can increase the solubility of functional gases in the pH-adjusted water, for example, in a gas-dissolved film type device. Dissolved gases include, for example, dissolved oxygen and dissolved nitrogen.

[0051] The degassing device is preferably located downstream of the pH adjuster or downstream of the pH adjuster and ORP adjuster on the transfer line. Although this type of manufacturing apparatus is equipped with a degassing device, it can suppress static electricity and prevent fine particles from accumulating on the gas-permeable membrane surface. This prevents fine particles from getting into the cleaning water.

[0052] As the degassing device, a membrane type degassing device is preferred, and a membrane type degassing device equipped with a gas-permeable membrane is more preferred. In one embodiment, the membrane type degassing device flows pH-adjusted water on one side (liquid phase chamber) of the gas-permeable membrane, and the other side (gas phase chamber) is depressurized with a vacuum pump, thereby causing at least a portion of the dissolved gas to permeate through the gas-permeable membrane and migrate to the gas phase chamber side for removal. The degassing device, for example, reduces the dissolved oxygen concentration in the pH-adjusted water supplied to the gas-dissolved membrane type device to 0.1 mg / L or less.

[0053] The gas-permeable membrane may be any membrane that allows gases such as oxygen, nitrogen, and steam to pass through but does not allow water to pass through. Examples of materials constituting the gas-permeable membrane include polymeric materials such as silicone rubber, polytetrafluoroethylene, polyvinylidene fluoride, polyolefins (e.g., polypropylene and poly(4-methylpentene-1)), and polyurethane. One or more polymeric materials may be used. Among these, at least one selected from the group consisting of poly(4-methylpentene-1), polypropylene, and polyvinylidene fluoride is preferred.

[0054] <Gas-dissolved film type device> The manufacturing apparatus of the present disclosure includes a gas dissolved film type apparatus. The gas-dissolved membrane device is preferably located downstream of the degassing device on the transfer line. The gas-dissolved membrane device dissolves a functional gas in degassed pH-adjusted water through a gas-permeable membrane.

[0055] A functional gas is a gas that imparts a specific function to cleaning water. Examples of functional gases include hydrogen gas, ozone gas, carbon dioxide gas, and rare gases. Among these, hydrogen gas is preferred. The concentration of hydrogen gas in cleaning water obtained using a gas-dissolved film type device is preferably 1.0 to 1.6 mg / L. By using cleaning water in which hydrogen gas is dissolved, a good effect of removing fine particles from electronic devices can be obtained. One type of functional gas may be used, or two or more types may be used.

[0056] The functional gas is supplied from a functional gas supply device. The functional gas supply device includes, for example, a functional gas storage device that generates or stores the functional gas and a mass flow controller that adjusts the supply rate of the functional gas. The functional gas supply device is connected to the gas dissolved film type device by a functional gas supply line and supplies the functional gas to the gas dissolved film type device.

[0057] The supply rate (flow rate) of the functional gas in the functional gas supply device can be calculated, for example, from the set concentration of the functional gas in the cleaning water and the transfer rate (flow rate) of the degassed pH-adjusted water. The set concentration of the functional gas in the cleaning water means the concentration of the functional gas in the cleaning water required at the point of use of the cleaning water, such as in an electronic device manufacturing process equipment.

[0058] In one embodiment, the functional gas supply device supplies the functional gas to the gas dissolved film type device for a predetermined time at a flow rate (hereinafter also referred to as the "initial flow rate" of the functional gas) that is higher than the flow rate of the functional gas calculated from the above-mentioned set concentration, etc., in the initial stage of cleaning water production, and after the predetermined time has elapsed, supplies the functional gas to the gas dissolved film type device at the flow rate of the functional gas calculated from the above-mentioned set concentration, etc. (hereinafter also referred to as the "set flow rate" of the functional gas). The timing for changing the flow rate of the functional gas from the initial flow rate to the set flow rate may be when the concentration of the functional gas in the cleaning water reaches the set concentration, or may be before that time. The timing for changing the flow rate of the functional gas may be, for example, when the concentration of the functional gas in the cleaning water reaches preferably 50% or more, more preferably 60% or more, even more preferably 70% or more, even more preferably 80% or more, and particularly preferably 90% or more of the set concentration. The predetermined time is not particularly limited, but is preferably within 10 minutes, more preferably within 7 minutes, and even more preferably within 5 minutes.

[0059] The ratio of the initial flow rate of the functional gas to the set flow rate in producing cleaning water (initial flow rate / set flow rate) is preferably more than 1.0 and not more than 10.0, more preferably 1.1 to 8.0, even more preferably 1.2 to 6.0, still more preferably 1.2 to 4.0, and particularly preferably 1.2 to 3.0.

[0060] In one embodiment, the gas-dissolved membrane device flows degassed pH-adjusted water on one side (liquid phase chamber) of a gas-permeable membrane and supplies a functional gas to the other side (gas phase chamber), allowing the functional gas to permeate the gas-permeable membrane, migrate to the liquid phase chamber, and dissolve in the pH-adjusted water.

[0061] Examples of materials constituting the gas-permeable membrane are as described above, and will not be repeated here. Among the above materials, at least one selected from the group consisting of poly(4-methylpentene-1), polypropylene, and polyvinylidene fluoride is preferred.

[0062] The gas-permeable membrane may be, for example, a hollow fiber membrane. In this case, the gas-dissolved membrane device includes a hollow fiber membrane unit containing a hollow fiber membrane. Connected to the interior of the hollow fiber membrane unit are a liquid supply pipe for supplying degassed pH-adjusted water to the hollow fiber membrane unit, a gas supply pipe for supplying functional gas to the hollow fiber membrane unit, and a drain pipe for discharging cleaning water with the functional gas dissolved therein.

[0063] <Water quality or flow rate monitoring device> The manufacturing apparatus of the present disclosure preferably further includes a water quality monitoring device for the cleaning water. The water quality monitoring device is a device that measures the quality of the wash water. The water quality monitoring device is preferably located downstream of the gas dissolved film device on the transfer line. The water quality monitoring device measures at least one selected from the group consisting of the concentration of the active ingredient of the pH adjuster and the concentration of the functional gas in the cleaning water, and preferably measures at least one selected from the group consisting of the concentration of the active ingredient of the pH adjuster, the concentration of the active ingredient of the ORP adjuster, pH, oxidation-reduction potential (ORP), and the concentration of the functional gas in the cleaning water, and monitors whether the concentration of the active ingredient, pH, ORP, or the concentration of the functional gas is at a desired value.

[0064] The pH of the cleaning water can be measured using a known pH meter. The ORP of the cleaning water can be measured using a known ORP meter. The concentration of the active ingredient in the cleaning water can be measured using a known conductivity meter. The concentration of the functional gas in the cleaning water can be measured using a known gas concentration meter (e.g., a DH meter for hydrogen gas).

[0065] The manufacturing apparatus of the present disclosure preferably further includes a device for monitoring the flow rate of the cleaning water. The flow rate monitor is a device that measures the flow rate of the wash water. The flow rate monitor is preferably located downstream of the gas dissolved film device on the transfer line. Examples of the flow rate monitor include a known flow meter.

[0066] <Control device> The manufacturing apparatus of the present disclosure preferably further includes a control device, such as a computer, in addition to one or both of a water quality monitor and a flow rate monitor for the cleaning water. The water quality monitoring device or the flow rate monitoring device may be connected to the control device, for example, electrically or wirelessly. The control device may be connected to at least one device selected from the group consisting of a pH adjusting device, an ORP adjusting device, and a gas dissolved film device, for example, electrically or wirelessly.

[0067] The control device is, for example, a device that controls at least one selected from the group consisting of the supply rate of a pH adjuster in a pH adjustment device and the supply rate of a functional gas in a gas-dissolved membrane type device based on the water quality measured by a water quality monitoring device for cleaning water, and is preferably a device that controls at least one selected from the group consisting of the supply rate of the pH adjuster, the supply rate of an ORP adjuster in an ORP adjustment device, and the supply rate of the functional gas. The control device can control the cleaning water to have at least one selected from the group consisting of a set concentration of the active ingredient, a set pH value, a set ORP value, and a set concentration of the functional gas. The control of at least one selected from the group consisting of the concentration of the active ingredient, pH, ORP, and the concentration of the functional gas by such a control device can be controlled by a known method, for example, feedback control such as PI control or PID control.

[0068] The control device can transmit a signal to the pH adjustment device based on the water quality (e.g., the concentration of the active ingredient in the pH adjuster or pH) measured by a water quality monitoring device for the cleaning water, and control the supply rate of the pH adjuster in the pH adjustment device using a pump or the like. The control device can transmit a signal to the ORP adjustment device based on the water quality (e.g., the concentration of the active ingredient in the ORP adjustment agent or the ORP) measured by a water quality monitoring device for the cleaning water, and control the supply rate of the ORP adjustment agent in the ORP adjustment device using a pump or the like. The control device can transmit a signal to a mass flow controller of the functional gas based on the water quality (e.g., the concentration of the functional gas) measured by a water quality monitoring device for the cleaning water, and can control the supply rate of the functional gas supplied from the functional gas supply device using a mass flow controller, etc.

[0069] For example, based on the water quality (e.g., the concentration of the active ingredient of a pH adjuster, the active ingredient of an ORP adjuster, or a functional gas) measured by a cleaning water quality monitoring device, the control device controls the supply of the adjuster, etc. at a flow rate greater than the flow rate of the adjuster, etc. calculated from the set concentration, etc. at the cleaning water use point for a predetermined time in the initial stage of cleaning water production, and after the predetermined time has elapsed, controls the supply of the adjuster, etc. in the adjusting device, etc. at the flow rate of the adjuster, etc. calculated from the set concentration, etc. The adjuster, etc. is, for example, a pH adjuster, ORP adjuster, or functional gas. The adjusting device, etc. is, for example, a pH adjuster, ORP adjuster, or gas-dissolved membrane type device.

[0070] In one embodiment, the control device controls at least one selected from the group consisting of the transfer rate of the ultrapure water, which is the raw water, the supply rate of the pH adjuster in the pH adjuster, the supply rate of the ORP adjuster in the ORP adjuster, and the supply rate of the functional gas supplied from the functional gas supply device, based on the flow rate measured by the cleaning water flow rate monitoring device.

[0071] The control device can transmit a signal to the pH adjusting device based on the flow rate of the cleaning water measured by the flow rate monitoring device, for example, and control the supply rate of the pH adjusting agent in the pH adjusting device using a pump or the like. The control device can transmit a signal to the ORP adjusting device based on the flow rate of the cleaning water measured by the flow rate monitoring device, for example, and control the supply rate of the ORP adjusting agent in the ORP adjusting device using a pump or the like. The control device can transmit a signal to a mass flow controller of the functional gas based on the flow rate measured by the cleaning water flow rate monitoring device, for example, and control the supply rate of the functional gas supplied from the functional gas supply device using the mass flow controller, etc.

[0072] The control device is preferably a device that further controls the flow path of the cleaning water. Note that the function of controlling at least one selected from the group consisting of the supply rate of the pH adjuster in the pH adjuster and the supply rate of the functional gas in the gas dissolved film type device based on the water quality measured by the water quality monitoring device and the function of controlling the flow path of the cleaning water may be possessed by the same control device or different control devices.

[0073] In one embodiment, after the manufacturing apparatus starts operating, the control device controls the flow path switching device in accordance with the quality of the wash water measured by the water quality monitoring device. Specifically, the control device (1) controls the switching device so that the wash water is not transferred to the use point, for example, to a drain line or a circulation line, if the quality of the wash water measured by the water quality monitoring device has not reached the set water quality at the use point; (2) sends a signal to the switching device to switch the wash water flow path, thereby controlling the switching device to transfer the wash water to the use point, if the quality of the wash water measured by the water quality monitoring device has reached the set water quality at the use point.

[0074] <Cleaning water flow path switching device> The manufacturing apparatus of the present disclosure preferably further comprises a device for switching the flow path of the cleaning water (flow path switching device) between the monitoring device and the point of use of the cleaning water. The switching device is preferably located downstream of the water quality monitoring device on the transfer line. An example of such a device is a three-way switching valve.

[0075] The transfer line is branched by the switching device into, for example, a transfer line connected to a use point of cleaning water, a drainage line for draining cleaning water, or a circulation line for circulating and using cleaning water, which joins at a junction located upstream on the transfer line. Circulating cleaning water can reduce the amount of produced cleaning water that is discharged. The junction is located, for example, upstream of a pH adjuster or a hydrogen peroxide remover on the transfer line. The switching device switches the flow path of the wash water based on a signal sent from the control device or manually, thereby transferring the wash water to the use point.

[0076] <Example of Manufacturing Device> 1 to 3 are block diagrams that schematically show a manufacturing apparatus according to the present disclosure. The manufacturing apparatus 1 in Figure 1 includes a transfer line L1 for ultrapure water W, pH-adjusted water W1, or cleaning water W2, a pH adjuster 12, a degassing device 14, and a gas-dissolved film type device 16. The transfer line L1 connects the pH adjuster 12 and the degassing device 14, and connects the degassing device 14 and the gas-dissolved film type device 16. The manufacturing apparatus 1 in Figure 1 may further include a pump (not shown) on the transfer line L1 between the pH adjuster 12 and the degassing device 14.

[0077] The manufacturing apparatus 1 in Fig. 2 includes a transfer line L1, a pH adjusting device 12, a degassing device 14, a gas dissolved film type device 16, a water quality monitoring device 18, a cleaning water flow path switching device 20, a control device 22, a transfer line L2, and a drain line L3. The manufacturing apparatus 1 in Fig. 2 may further include a pump (not shown) on the transfer line L1 between the pH adjusting device 12 and the degassing device 14.

[0078] Transfer line L1 connects pH adjuster 12 and degasser 14, connects degasser 14 and gas dissolved film type device 16, connects gas dissolved film type device 16 and water quality monitor 18, and connects water quality monitor 18 and switching device 20. Transfer line L2 connects switching device 20 and the point of use (UP).

[0079] The control device 22 controls the supply rate of the pH adjuster in the pH adjuster 12 and the supply rate of the functional gas supplied to the gas dissolved film type device 16 based on the water quality obtained by the water quality monitor 18.

[0080] The manufacturing apparatus 1 in Fig. 3 includes a transfer line L1, a hydrogen peroxide remover 11, a pH adjuster 12, an ORP adjuster 13, a degasser 14, a gas dissolved film type device 16, a water quality monitor 18, a cleaning water flow path switching device 20, a control device 22, a transfer line L2, and a drain line L3. The manufacturing apparatus 1 in Fig. 3 may further include a pump (not shown) on the transfer line L1 between the ORP adjuster 13 and the degasser 14.

[0081] 1 to 3, pH adjuster 12 includes tank 12A containing a pH adjuster, supply line 12L connecting tank 12A to transfer line L1, and pump 12B located on supply line 12L. In FIG. 3, the ORP adjuster 13 includes a tank 13A containing an ORP adjuster, a supply line 13L connecting the tank 13A to a transfer line L1, and a pump 13B located on the supply line 13L. 1 to 3, a functional gas supply device 16A is connected to a gas dissolved film type device 16 via a supply line 16L.

[0082] 2 and 3, a circulation line (not shown) for circulating cleaning water for reuse may be provided. The circulation line merges with the transfer line L1 at a junction located upstream of the pH adjuster 12, for example.

[0083] The cleaning water manufacturing apparatus of the present disclosure has been described above based on the above embodiment with reference to the attached drawings, but the cleaning water manufacturing apparatus of the present disclosure is not limited to the above embodiment and various modifications can be made.

[0084] [Method of manufacturing cleaning water for electronic devices] The method for producing cleaning water for electronic devices according to the present disclosure (hereinafter also simply referred to as the "production method according to the present disclosure") comprises a pH adjustment step of adding a pH adjuster to ultrapure water to prepare pH-adjusted water, a degassing step of degassing the pH-adjusted water, and a gas dissolution step of dissolving a functional gas in the degassed pH-adjusted water via a gas-permeable membrane to prepare cleaning water. The manufacturing method of the present disclosure may further include at least one step selected from the group consisting of an oxidation-reduction potential (ORP) adjustment step of adjusting the ORP of ultrapure water or pH-adjusted water, and a hydrogen peroxide removal step of removing hydrogen peroxide. The manufacturing method of the present disclosure can be carried out using, for example, the above-described manufacturing apparatus.

[0085] In the above production method, the ultrapure water, pH-adjusted water, and cleaning water are each transferred at a flow rate of 25 L / min or more, preferably 25 to 700 L / min, more preferably 30 to 500 L / min, even more preferably 40 to 300 L / min, and particularly preferably 50 to 200 L / min.

[0086] The above production method preferably further comprises a step of adjusting the pressure of the ultrapure water, pH-adjusted water, or cleaning water to 0.1 MPa or higher. The pressure is preferably 0.1 MPa or higher, more preferably 0.2 to 1.0 MPa, even more preferably 0.3 to 0.8 MPa, and particularly preferably 0.4 to 0.6 MPa.

[0087] The above manufacturing method preferably includes a water quality monitoring step of measuring the quality of the cleaning water. For example, based on the concentration of the active ingredient of the pH adjuster or ORP adjuster in the cleaning water measured in the water quality monitoring process, in the initial stage of cleaning water production, the pH adjuster or ORP adjuster is supplied for a predetermined time in the pH adjustment process or ORP adjustment process at a flow rate greater than the flow rate of the pH adjuster or ORP adjuster calculated from the above-mentioned set concentration, etc. at the point of use of the cleaning water, and after the above-mentioned predetermined time has elapsed, the pH adjuster or ORP adjuster is supplied in the pH adjustment process or ORP adjustment process at the flow rate of the pH adjuster or ORP adjuster calculated from the above-mentioned set concentration, etc.

[0088] For example, based on the concentration of the functional gas in the cleaning water measured in the water quality monitoring process, in the initial stage of cleaning water production, the functional gas is supplied in the gas dissolution process for a predetermined time at a flow rate greater than the flow rate of the functional gas calculated from the above-mentioned set concentration, etc. at the point of use of the cleaning water, and after the above-mentioned predetermined time has elapsed, the functional gas is supplied in the gas dissolution process at the flow rate of the functional gas calculated from the above-mentioned set concentration, etc.

[0089] If the water quality of the cleaning water measured in the water quality monitoring process does not reach the set water quality at the use point, it is preferable not to transfer the cleaning water to the use point, and if the water quality of the cleaning water measured in the water quality monitoring process reaches the set water quality at the use point, it is preferable to transfer the cleaning water to the use point.

[0090] Regarding the details of the above manufacturing method and the conditions of each step, the conditions described in the above section [Apparatus for manufacturing cleaning water for electronic devices] can be applied, and description here will be omitted.

[0091] The cleaning water produced by the manufacturing apparatus or manufacturing method of the present disclosure is supplied to a cleaning apparatus provided in a process apparatus for manufacturing electronic devices such as semiconductor devices. Examples of the cleaning apparatus include a cleaning apparatus that immerses an object to be cleaned in cleaning water in a cleaning tank to clean it, and a cleaning apparatus that sprays cleaning water onto the object in a shower-like manner and washes it by letting it flow over the object.

[0092] [Example of situation] The present disclosure relates to, for example, the following [1] to

[14] . [1] A pH adjustment device that prepares pH-adjusted water by adding a pH adjuster to ultrapure water; a degassing device for degassing the pH-adjusted water; a gas-dissolving membrane type device that dissolves a functional gas in the degassed pH-adjusted water through a gas-permeable membrane to prepare cleaning water; transfer lines capable of transferring the ultrapure water, the pH-adjusted water, and the cleaning water at a flow rate of 25 L / min or more; An apparatus for producing cleaning water for electronic devices, comprising: [2] The apparatus for producing cleaning water for electronic devices according to [1] above, further comprising a pump for adjusting the pressure of the pH-adjusted water to 0.1 MPa or more. [3] The manufacturing apparatus further includes a water quality monitoring device for the cleaning water and a control device, The water quality monitoring device is located downstream of the gas dissolved film device, the water quality monitoring device is a device for measuring the quality of the cleaning water, The control device is a device that controls at least one selected from the group consisting of a supply rate of the pH adjuster in the pH adjuster device and a supply rate of the functional gas in the gas dissolved film type device based on the water quality measured by the water quality monitoring device. The apparatus for producing cleaning water for electronic devices according to [1] or [2] above. [4] The control device based on the concentration of the active ingredient of the pH adjuster in the cleaning water measured by the water quality monitoring device, in the initial stage of cleaning water production, controlling the pH adjuster to supply the pH adjuster for a predetermined time at a flow rate higher than the flow rate of the pH adjuster calculated from the set concentration at the point of use of the cleaning water, After the predetermined time has elapsed, the pH adjusting device is controlled to supply the pH adjusting agent at a flow rate of the pH adjusting agent calculated from the set concentration. The apparatus for producing cleaning water for electronic devices according to [3] above. [5] The control device Based on the concentration of the functional gas in the cleaning water measured by the water quality monitoring device, in the initial stage of cleaning water production, control is performed so that the functional gas is supplied to the gas dissolved film type device for a predetermined time at a flow rate higher than the flow rate of the functional gas calculated from the set concentration of the cleaning water at the point of use, After the predetermined time has elapsed, the functional gas is supplied to the gas dissolved film type device at a flow rate of the functional gas calculated from the set concentration. The apparatus for producing cleaning water for electronic devices according to [3] or [4] above. [6] The manufacturing apparatus further includes a switching device for switching the flow path of the cleaning water, The switching device is located downstream of the water quality monitoring device, the transfer line for the cleaning water is branched in the switching device into a transfer line connected to a use point for the cleaning water, and a drain line for draining the cleaning water, or a circulation line that joins at a junction located upstream on the transfer line; When the quality of the flush water measured by the water quality monitoring device does not reach the set water quality at the use point, the control device controls the switching device to transfer the flush water to the drain line or the circulation line; when the quality of the flush water measured by the water quality monitoring device reaches the set water quality at the use point, the control device sends a signal to the switching device to switch the flush water flow path and control the switching device to transfer the flush water to the use point. The apparatus for producing cleaning water for electronic devices according to any one of the above [3] to [5]. [7] The apparatus for producing cleaning water for electronic devices according to any one of [1] to [6] above, wherein the pH adjuster prepares pH-adjusted water having a pH of 8 to 11. [8] The apparatus for producing cleaning water for electronic devices according to any one of [1] to [7] above, wherein the pH adjuster adds an aqueous solution of at least one alkaline compound selected from the group consisting of ammonia, tetramethylammonium hydroxide, 2-hydroxyethyltrimethylammonium hydroxide, sodium hydroxide, and potassium hydroxide to the ultrapure water as the pH adjuster. [9] The apparatus for producing cleaning water for electronic devices according to any one of [1] to [8] above, wherein the functional gas is at least one selected from the group consisting of hydrogen gas, ozone gas, carbon dioxide gas, and rare gases.

[10] A pH adjustment step of adding a pH adjuster to ultrapure water to prepare pH-adjusted water; a degassing step of degassing the pH-adjusted water; a gas dissolving step of dissolving a functional gas in the degassed pH-adjusted water through a gas-permeable membrane to prepare cleaning water; and The ultrapure water, the pH-adjusted water, and the cleaning water are each transferred at a flow rate of 25 L / min or more. A method for producing cleaning water for electronic devices.

[11] The method for producing cleaning water for electronic devices according to

[10] above, further comprising a step of adjusting the pressure of the pH-adjusted water to 0.1 MPa or more.

[12] The manufacturing method further comprises a water quality monitoring step of measuring the water quality of the cleaning water, based on the concentration of the active ingredient of the pH adjuster in the cleaning water measured in the water quality monitoring step, in the initial stage of cleaning water production, the pH adjuster is supplied for a predetermined time in the pH adjustment step at a flow rate higher than the flow rate of the pH adjuster calculated from the set concentration of the cleaning water at the point of use, After the predetermined time has elapsed, in the pH adjustment step, the pH adjuster is supplied at a flow rate of the pH adjuster calculated from the set concentration. The method for producing cleaning water for electronic devices according to

[10] or

[11] above.

[13] The manufacturing method further comprises a water quality monitoring step of measuring the water quality of the cleaning water, based on the concentration of the functional gas in the cleaning water measured in the water quality monitoring step, in the initial stage of cleaning water production, supplying the functional gas for a predetermined time in the gas dissolving step at a flow rate higher than the flow rate of the functional gas calculated from a set concentration of the functional gas at the point of use of the cleaning water, After the predetermined time has elapsed, in the gas dissolving step, the functional gas is supplied at a flow rate of the functional gas calculated from the set concentration. The method for producing cleaning water for electronic devices according to any one of the above

[10] to

[12] .

[14] The method for producing cleaning water for electronic devices according to

[12] or

[13] , wherein if the water quality of the cleaning water measured in the water quality monitoring process does not reach the set water quality at the use point, the cleaning water is not transferred to the use point, and if the water quality of the cleaning water measured in the water quality monitoring process reaches the set water quality at the use point, the cleaning water is transferred to the use point. [Example]

[0093] The cleaning water producing device of the present disclosure will be described based on examples. The cleaning water producing device of the present disclosure is not limited to the following examples.

[0094] [Example 1] Using an apparatus for producing cleaning water for electronic devices similar to that shown in Figure 2 (which further includes a pump, not shown, between the pH adjuster 12 and the degasser 14), cleaning water was obtained by dissolving ammonia and hydrogen gas in ultrapure water, as described below. In the above-mentioned production apparatus, polyvinylidene fluoride (PVDF) piping with an outer diameter of approximately 105 mm and an inner diameter of approximately 100 mm was used as the piping constituting the transfer line and supply line.

[0095] The cleaning water was produced using the above manufacturing equipment, and the supply method was evaluated assuming that the cleaning water would be supplied to semiconductor device manufacturing process equipment that requires cleaning water at a flow rate of 5 L / min per chamber.

[0096] The concentration rise time of the active ingredient of the pH adjuster in the cleaning water and the concentration rise time of the functional gas in the cleaning water were evaluated from the start of the production operation of the obtained cleaning water. The concentration rise time means the time until the concentration of the target component in the cleaning water reaches the set concentration. In this evaluation, an aqueous ammonia solution (containing ammonia as an active ingredient) was used as the pH adjuster, and hydrogen gas was used as the functional gas. The ammonia in the cleaning water was evaluated by converting the measured value into an ammonia concentration using a conductivity meter, and the hydrogen gas was evaluated using a DH meter. ◎: The concentration of the target component increases within 5 minutes. ○: The rise time of the target component concentration is more than 5 minutes and less than 10 minutes. ×: The rise time of the target component concentration is more than 10 minutes.

[0097] The ammonia concentration in the final wash water was set to 30 mg / L, and the hydrogen gas (H2) concentration was set to 1.4 mg / L.

[0098] Ultrapure water was supplied to the manufacturing apparatus at a flow rate of 25 L / min. An aqueous ammonia solution (ammonia concentration: 28%) was prepared by dissolving ammonia in ultrapure water. The above aqueous ammonia solution was added to the ultrapure water flowing through the transfer line to obtain pH-adjusted water. The pH-adjusted water was pressurized to 0.3 MPa using a pump. The pH-adjusted water was supplied to a degassing device (water degassing / aeration module, model number: EF-020-A30, material: poly-4-methylpentene-1, manufactured by DIC) at a flow rate of 25 L / min. Hydrogen gas was supplied to the gas-dissolved membrane device (the above water degassing / aeration module) and the degassed pH-adjusted water was supplied at a flow rate of 25 L / min to dissolve the hydrogen gas in the pH-adjusted water, producing cleaning water.

[0099] In the initial stage of the manufacturing process, the aqueous ammonia solution (ammonia concentration: 28%) was added to the ultrapure water flowing through the transfer line at a flow rate of 5 mL / min for 1 minute. After 1 minute had elapsed, the flow rate of the aqueous ammonia solution was changed to the flow rate (3 mL / min, stable flow rate) required for the set ammonia concentration (30 mg / L) in the wash water.

[0100] In the initial stage of the manufacturing process, hydrogen gas was supplied to the gas dissolved film device at a flow rate of 500 sccm for 3 minutes. After 3 minutes, the hydrogen gas flow rate was changed to the flow rate (400 sccm, steady state flow rate) required for the set concentration of hydrogen gas in the wash water (1.4 mg / L).

[0101] The pressure of the water flowing through the transfer line was measured to be 0.3 MPa.

[0102] The rise time of the ammonia concentration in the wash water was 2 minutes. The rise time of the hydrogen gas concentration in the wash water was 3 minutes.

[0103] [Examples 2 to 4 and Comparative Example 1] Cleaning water was produced in the same manner as in Example 1, except that the conditions were changed as shown in Table 1. The evaluation results are shown in Table 1. In Comparative Example 1, the supply rates of the aqueous ammonia solution and hydrogen gas were maintained at the supply rates required for the set concentrations. In Comparative Example 1, a pipe capable of transporting ultrapure water at a flow rate of less than 25 L / min but not at a flow rate of 25 L / min or more was used.

[0104] [Table 1] [Explanation of symbols]

[0105] 1. Equipment for producing cleaning water for electronic devices 11...Hydrogen peroxide removal device 12...pH adjustment device 12A: Tank containing pH adjuster 12B...Pump 12L…pH adjuster supply line 13...ORP adjustment device 13A: Tank containing ORP adjuster 13B...Pump 13L...ORP adjuster supply line 14... Degassing device 16...Gas-dissolved film device 16A...Functional gas supply device 16L...Functional gas supply line 18…Water quality monitoring device 20...Flow path switching device 22...Control device W…Ultra pure water W1…pH adjusted water W2: Washing water L1: Ultrapure water, pH-adjusted water, or cleaning water transfer line L2: Transfer line L3...Drain line UP...Use points

Claims

1. a pH adjusting device that prepares pH-adjusted water by adding a pH adjuster to ultrapure water; a degassing device for degassing the pH-adjusted water; a gas-dissolving membrane type device that dissolves a functional gas in the degassed pH-adjusted water through a gas-permeable membrane to prepare cleaning water; transfer lines capable of transferring the ultrapure water, the pH-adjusted water, and the cleaning water at a flow rate of 25 L / min or more; An apparatus for producing cleaning water for electronic devices, comprising:

2. 2. The apparatus for producing cleaning water for electronic devices according to claim 1, further comprising a pump for adjusting the pressure of the pH-adjusted water to 0.1 MPa or more.

3. The manufacturing apparatus further includes a water quality monitoring device for the cleaning water and a control device, The water quality monitoring device is located downstream of the gas dissolved film device, the water quality monitoring device is a device for measuring the quality of the cleaning water, The control device is a device that controls at least one selected from the group consisting of a supply rate of the pH adjuster in the pH adjustment device and a supply rate of the functional gas in the gas dissolved film type device based on the water quality measured by the water quality monitoring device. The apparatus for producing cleaning water for electronic devices according to claim 1.

4. The control device Based on the concentration of the active ingredient of the pH adjuster in the cleaning water measured by the water quality monitoring device, in the initial stage of cleaning water production, the pH adjuster is controlled to be supplied for a predetermined time at a flow rate greater than the flow rate of the pH adjuster calculated from the set concentration at the point of use of the cleaning water, After the predetermined time has elapsed, the pH adjusting device is controlled to supply the pH adjusting agent at a flow rate of the pH adjusting agent calculated from the set concentration. The apparatus for producing cleaning water for electronic devices according to claim 3.

5. The control device Based on the concentration of the functional gas in the cleaning water measured by the water quality monitoring device, in the initial stage of cleaning water production, control is performed so that the functional gas is supplied to the gas dissolved film type device for a predetermined time at a flow rate higher than the flow rate of the functional gas calculated from the set concentration of the cleaning water at the point of use, After the predetermined time has elapsed, the functional gas is supplied to the gas dissolved film type device at a flow rate of the functional gas calculated from the set concentration. The apparatus for producing cleaning water for electronic devices according to claim 3.

6. the manufacturing apparatus further includes a switching device for switching the flow path of the cleaning water; The switching device is located downstream of the water quality monitoring device, the transfer line for the cleaning water is branched in the switching device into a transfer line connected to a use point for the cleaning water, and a drain line for draining the cleaning water, or a circulation line that joins at a junction located upstream on the transfer line; When the quality of the flush water measured by the water quality monitoring device does not reach the set water quality at the use point, the control device controls the switching device to transfer the flush water to the drain line or the circulation line; when the quality of the flush water measured by the water quality monitoring device reaches the set water quality at the use point, the control device sends a signal to the switching device to switch the flush water flow path and control the switching device to transfer the flush water to the use point. The apparatus for producing cleaning water for electronic devices according to any one of claims 3 to 5.

7. 2. The apparatus for producing cleaning water for electronic devices according to claim 1, wherein the pH adjuster prepares pH-adjusted water having a pH of 8 to 11.

8. 2. The apparatus for producing cleaning water for electronic devices according to claim 1, wherein the pH adjuster adds, to the ultrapure water, an aqueous solution of at least one alkaline compound selected from the group consisting of ammonia, tetramethylammonium hydroxide, 2-hydroxyethyltrimethylammonium hydroxide, sodium hydroxide, and potassium hydroxide as the pH adjuster.

9. 2. The apparatus for producing cleaning water for electronic devices according to claim 1, wherein the functional gas is at least one selected from the group consisting of hydrogen gas, ozone gas, carbon dioxide gas, and rare gases.

10. a pH adjustment step of adding a pH adjuster to ultrapure water to prepare pH-adjusted water; a degassing step of degassing the pH-adjusted water; a gas dissolving step of dissolving a functional gas in the degassed pH-adjusted water through a gas-permeable membrane to prepare cleaning water; and The ultrapure water, the pH-adjusted water, and the cleaning water are each transferred at a flow rate of 25 L / min or more. A method for producing cleaning water for electronic devices.

11. The method for producing cleaning water for electronic devices according to claim 10 , further comprising the step of adjusting the pressure of the pH-adjusted water to 0.1 MPa or more.

12. The manufacturing method further comprises a water quality monitoring step of measuring the quality of the cleaning water, based on the concentration of the active ingredient of the pH adjuster in the cleaning water measured in the water quality monitoring step, in the initial stage of cleaning water production, supplying the pH adjuster for a predetermined time in the pH adjustment step at a flow rate higher than the flow rate of the pH adjuster calculated from the set concentration of the cleaning water at the point of use, After the predetermined time has elapsed, in the pH adjustment step, the pH adjuster is supplied at a flow rate of the pH adjuster calculated from the set concentration. The method for producing cleaning water for electronic devices according to claim 10.

13. The manufacturing method further comprises a water quality monitoring step of measuring the quality of the cleaning water, based on the concentration of the functional gas in the cleaning water measured in the water quality monitoring step, in the initial stage of cleaning water production, supplying the functional gas for a predetermined time in the gas dissolving step at a flow rate higher than the flow rate of the functional gas calculated from a set concentration of the functional gas at the point of use of the cleaning water, After the predetermined time has elapsed, in the gas dissolving step, the functional gas is supplied at a flow rate of the functional gas calculated from the set concentration. The method for producing cleaning water for electronic devices according to claim 10.

14. 14. The method for producing cleaning water for electronic devices according to claim 12 or 13, wherein if the water quality of the cleaning water measured in the water quality monitoring process does not reach the set water quality at the use point, the cleaning water is not transferred to the use point, and if the water quality of the cleaning water measured in the water quality monitoring process reaches the set water quality at the use point, the cleaning water is transferred to the use point.

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