Chemical liquid manufacturing apparatus

Abstract

A chemical liquid production apparatus is provided that includes a first system and a second system, wherein the first system includes at least one first filtration medium selected from a first filter, a first ion exchange membrane, and a first ion adsorption membrane, and the first system is configured to process a material at least once, and the second system includes at least one second filtration medium selected from a second filter, a second ion exchange membrane, and a second ion adsorption membrane, and the second system is configured to recirculate and process a material at least twice.

Description

[Technical field]

[0001] Related Application Data This application claims priority to U.S. Provisional Application No. 62 / 650,448, filed March 30, 2018, the entire contents of which are incorporated herein by reference.

[0002] The present disclosure relates to a chemical liquid manufacturing apparatus and a method for manufacturing a chemical liquid using the same. [Background technology]

[0003] The semiconductor industry is rapidly increasing the integration density of electronic components, which is due to the continuous reduction in component size. Eventually, more and more smaller components are integrated into a given area. These improvements are primarily due to the development of new precision and high-resolution processing techniques.

[0004] In the manufacture of high resolution integrated circuits, various process fluids come into contact with bare or film-coated wafers. For example, the manufacture of fine metal interconnects typically involves a procedure in which the substrate is coated with a pre-wetting fluid before the substrate is coated with a complex liquid to form a resist film. These process fluids, containing suitable components and various additives, are known to be a source of contamination of IC wafers.

[0005] It is speculated that even trace amounts of contaminants in these chemical liquids, such as wafer pre-wetting solutions and developer solutions, can cause defects in circuit patterns. The presence of metal impurities at very low levels, such as 1.0 ppt, is known to hinder the performance and stability of semiconductor devices. In addition, some types of metal contaminants can degrade the oxidation properties, resulting in inaccurate patterns and reduced electrical performance of semiconductor circuits, ultimately negatively impacting manufacturing yields.

[0006] Contamination by impurities such as metal impurities, coarse particles, organic impurities, and moisture may be inadvertently introduced into the chemical liquid during various stages of chemical liquid production. For example, it may be due to the presence of impurities in the raw materials, or from the transportation, storage of raw materials and chemical liquids, the container equipment and reaction vessels used in the reaction, by-products generated during the production of chemical liquids, or unreacted reactants left over.

[0007] Therefore, in order to form high-precision and ultra-fine semiconductor electronic circuits, chemical liquids used in various stages of semiconductor processes such as pre-wetting liquids, resist solutions, developing solutions, stripping solutions, rinsing solutions, and coating solutions require significant quality improvement and must maintain strict quality control to ensure that no defects occur in the resulting circuit patterns.

Summary of the Invention

Problems to be Solved by the Invention

[0008] Therefore, in order to form high-precision integrated circuits, the requirements for ultra-high-purity chemical liquids and the improvement and control of the quality of these liquids become very important. Specific important parameters for quality improvement and control include the reduction of trace metals, the reduction of the number of liquid particles, the reduction of on-wafer defects, the reduction of organic contaminants, etc. It has been shown that all of these important parameters are affected by the settings of processing equipment and processing parameters including purification media, media preparation, filter sequences, filter contact times, structural materials, and the physiochemical properties of the purification media.

Means for Solving the Problems

[0009] In view of the above, the present disclosure provides a chemical liquid production apparatus for preparing chemical liquids especially for semiconductor manufacturing, and high-purity chemical liquids are produced with the number of unwanted fine particles and the amount of metal impurities in the chemical liquid controlled within a predetermined range. Therefore, the generation of residues and / or particle defects is suppressed, and the yield of semiconductor wafers is improved.

[0010] According to some embodiments of the present disclosure, a chemical liquid manufacturing apparatus includes at least a first system and a second system, and each of the first and second systems is configured to process a material. The first system includes at least one first filtration medium selected from a first filter, a first ion exchange membrane, and a first ion adsorption membrane, and the at least one first filtration medium is configured to process the material at least once. The second purification system includes at least one second filtration medium selected from at least a second filter, a second ion exchange membrane, and a second ion adsorption membrane, and the at least one second filtration medium recirculates and is configured to process the material at least twice.

[0011] According to a particular exemplary embodiment, the first system is configured for single pass.

[0012] According to an alternative embodiment of the present disclosure, a chemical liquid manufacturing apparatus for processing a material includes at least a first system and a second system. The first system includes at least one first filtration medium selected from at least one first filter, a first ion exchange membrane, and a first ion adsorption membrane, and the first system is configured to process the material at least once. The second system includes at least one second filtration medium selected from at least one second filter, a second ion exchange membrane, and a second ion adsorption membrane, and the second system is configured for recirculation and to process the material at least twice.

[0013] According to a particular exemplary embodiment, there are two or more first filters, and the two or more first filters preferably have different characteristics. According to a further particular exemplary embodiment, there are two second filters, and the two second filters preferably have different characteristics.

[0014] According to yet another embodiment of the present disclosure, a chemical liquid manufacturing apparatus includes at least a first system and a second system. The first system includes one or more first purification media. When the first system includes a plurality of first purification media, at least two of the first purification media differ in function, pore size, or material. The second system includes one or more second purification media. When the second system includes a plurality of second purification media, at least two of the second purification media differ in function, pore size, or material. The first system is configured to process the material at least once, and the second system is configured to recirculate and process the material at least twice.

Effects of the Invention

[0015] According to the present disclosure, a chemical liquid manufacturing apparatus having a multifunctional purification medium that combines adsorption, filtration, ion exchange, etc. is used for effectively removing a wide range of organic and inorganic contaminants from aqueous and solvent-based solutions used for the preparation of high-purity chemical liquids applied to semiconductor manufacturing.

Brief Description of the Drawings

[0016] Aspects of the present disclosure are best understood from the following detailed description when read in conjunction with the accompanying drawings. It should be noted that, in accordance with standard industry practice, the various features are not drawn to scale. In fact, the dimensions of the various features may be arbitrarily enlarged or reduced for clarity of explanation.

[0017]

Fig. 1

Fig. 2

Modes for Carrying Out the Invention

[0018] The following disclosure provides different embodiments or examples for implementing various features of the present subject matter. For the sake of simplifying the present disclosure, specific examples of components and arrangements are described below. These are merely examples and are not intended to be limiting. For example, when the term "solvent" is used, unless otherwise specified, it can refer to a single solvent or a combination of two or more solvents.

[0019] Furthermore, spatially relative terms such as "beneath", "below", "lower", "above", "upper", etc. are used herein for the convenience of description to explain the relationship of features to one element or other elements or the features illustrated. Spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation shown in the figures. The device may be oriented in other ways (rotated by 90 degrees or other orientations), and the spatially relative descriptors used herein can be interpreted accordingly.

[0020] In the present disclosure, a numerical range indicated using the term "to" means a range that includes the numerical values described before and after the term "to" as the lower limit value and the upper limit value.

[0021] In the present disclosure, "ppm" means "one part per million (10 ‐6 )", "ppb" means "one part per billion (10 ‐9 )", and "ppt" means "one part per trillion (10 ‐12 )".

[0022] In the present disclosure, 1 Å (angstrom) corresponds to 0.1 nm (nanometer), and 1 μm (micron) corresponds to 1000 nm.

[0023] <Object to be processed> Before being subjected to the purification process, the chemical liquid may contain undesirable amounts of impurities and contaminants. In the present disclosure, here, the preliminarily purified chemical liquid is referred to as the "material to be treated" or "material to be processed". After treating the material to be treated with the chemical liquid manufacturing apparatus of the present disclosure, a significant amount of contaminants and impurities are removed from the material to be treated, and the impurities and contaminants are managed and restricted within a predetermined range to produce a chemical liquid.

[0024] <Chemical liquid> In the present disclosure, the chemical liquid contains an organic solvent and a predetermined amount of impurities. The chemical liquid may include processing liquids used in semiconductor manufacturing such as prewetting liquids, developing solutions, rinsing liquids, cleaning solutions, stripping solutions, etc., and raw materials used in the synthesis of the processing liquids.

[0025] <Organic solvent> In the present disclosure, the chemical liquid contains an organic solvent. The type of the organic solvent is not particularly limited, and known organic solvents can be applied. The content of the organic solvent in the chemical liquid is not particularly limited, but the organic solvent is contained as a main component. Specifically, the content of the organic solvent is 98% by mass or more based on the total mass of the chemical liquid. In a specific embodiment, the content of the organic solvent is 99% by mass or more based on the total mass of the chemical liquid. In other embodiments, the content of the organic solvent is 99.5% by mass or more based on the total mass of the chemical liquid. In still other embodiments, the content of the organic solvent is 99.8% by mass or more based on the total mass of the chemical liquid. The upper limit value is not particularly limited, but usually, the upper limit value is 99.99% by mass or less.

[0026] The organic solvent may be used alone or in combination of two or more. When two or more organic solvents are used in combination, it is preferable that the total content is within the above range.

[0027] The content of the organic solvent in the chemical liquid can be measured using a gas chromatograph mass spectrometry (GCMS) apparatus.

[0028] The boiling point of the organic solvent is not particularly limited. However, from the viewpoint of improving the manufacturing yield of the semiconductor chip, the boiling point of the organic solvent is preferably less than 200°C. In the present disclosure, the boiling point means the boiling point at 1 atm.

[0029] The organic solvent is not particularly limited. Examples of the organic solvent include methanol, ethanol, 1-propanol, isopropanol, n-propanol, 2-methyl-1-propanol, n-butanol, 2-butanol, tert-butanol, 1-pentanol, 2-pentanol, 3-pentanol, n-hexanol, cyclohexanol, 2-methyl-2-butanol, 3-methyl-2-butanol, 2-methyl-1-butanol, 3-methyl-1-butanol, 2-methyl-1-pentanol, 2-methyl-2-pentanol, 2-methyl-3-pentanol, 3-methyl-1-pentanol, 3-methyl-2-pentanol, 3-methyl-3-pentanol, 4-methyl-1-pentanol, 4-methyl-2-pentanol, 2-ethyl-1-butanol, 2,2-dimethyl-3-pentanol, 2,3-dimethyl-3-pentanol, 2,4-dimethyl-3-pentanol, 4,4-dimethyl-2-pentanol, 3-ethyl-3-heptanol, 1-heptanol, 2-heptanol, 3-heptanol, 2-methyl-2-hexanol, 2-methyl-3-hexanol, 5-methyl-1-hexanol, 5-methyl-2-hexanol, 2-ethyl-1-hexanol, methylcyclohexanol, trimethylcyclohexanol, 4-methyl-3-heptanol, 6-methyl-2-heptanol, 1-octanol, 2-octanol, 3-octanol, 2-propyl-1-pentanol, 2,6-dimethyl-4-heptanol, 2-nonanol, 3,7-dimethyl-3-octanol, ethylene glycol, propylene glycol, diethyl ether, dipropyl ether, diisopropyl ether, butyl methyl ether, butyl ethyl ether, butyl propyl ether, dibutyl ether, diisobutyl ether, tert-butyl methyl ether, tert-butyl ethyl ether, tert-butyl propyl ether, di-tert-butyl ether, dipentyl ether, diisoamyl ether, cyclopentyl methyl ether, cyclohexyl methyl ether, bromomethyl methyl ether, α,α-dichloromethyl methyl ether, chloromethyl ethyl ether, 2-chloroethyl methyl ether, 2-bromoethyl methyl ether, 2,2-dichloroethyl methyl ether, 2-chloroethyl ethyl ether, 2-bromoethyl ethyl ether, (±)-1,2-dichloroethyl ethyl ether, 2,2,2-trifluoroethyl ether, ethyl vinyl ether, butyl vinyl ether, allyl ethyl ether, allyl propyl ether, allyl butyl ether, diallyl ether, 2-methoxypropene, ethyl-1-propenyl ether, cis-1-bromo-2-ethoxyethylene, 2-chloroethyl vinyl ether, allyl-1,1,2,2-tetrafluoroethyl ether, octane, isooctane, nonane, decane, methylcyclohexane, decalin, xylene, ethylbenzene, diethylbenzene, cumene, sec-butylbenzene, cymene, dipentene, methyl pyruvate, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monomethyl ether acetate, ethyl lactate, methyl methoxypropionate, cyclopentanone, cyclohexanone, butyl acetate, γ-butyrolactone, isoamyl acetate, chloroform, dichloromethane, 1,4-dioxane, hexyl alcohol, 2-heptanone, isoamyl acetate, and tetrahydrofuran are included.,

[0030] In certain embodiments of the present disclosure, the chemical liquid is a prewetting liquid. The type of the prewetting liquid is not particularly limited. Specific examples of the prewetting liquid include at least one of cyclopentanone (CyPe), cyclohexanone (CyH), propylene glycol monomethyl ether (PGME), propylene glycol monoethyl ether (PGEE), propylene glycol monomethyl ether acetate (PGMEA), propylene glycol monopropyl ether (PGPE), and ethyl lactate (EL). In other embodiments, the chemical liquid may be a developing solution such as butyl acetate or a rinsing liquid such as 4-methyl-2-pentanol (MIBC).

[0031] <Impurities> Impurities contained in the object to be processed and / or the chemical liquid include metal impurities, particles, and other organic impurities, moisture, etc.

[0032] <Metal impurities> The most common metal impurities include heavy metals such as iron (Fe), aluminum (Al), chromium (Cr), nickel (Ni), etc., and ionic metals such as sodium (Na) and calcium (Ca). Depending on the type of metal, metal impurities can reduce the integrity of oxides, deteriorate the MOS gate stack, and shorten the life of the device. In the chemical liquid prepared by the chemical liquid manufacturing apparatus of the present disclosure, the total trace metal content is preferably within a predetermined range of 0 to 150 ppt by mass.

[0033] In the present disclosure, metal impurities refer to metal impurities provided in the form of solids (metallic elements, particulate metal-containing compounds, etc.).

[0034] In this disclosure, the total trace metals in the chemical liquid are measured by inductively coupled plasma mass spectrometry (ICP-MS) using the Fujifilm developed method. OWMP (on-wafer metal particle) is determined by inspecting the wafer by combining a laser-based inspection system and EDX (energy dispersive x-ray) inspection. The measurement methods for total trace metals using ICP-MS and on-wafer metal particles (OWMP) using a laser and EDX are as shown in the following examples.

[0035] <Particles> In the present disclosure, a counting target having a size of 0.03 μm or more is referred to as a "particle". The number of "particles" in the liquid medium is counted by a light scattering type in-liquid particle counter and is referred to as LPC (liquid particle count).

[0036] Examples of the particles include dust, dirt, organic solids, and inorganic solids. The particles may also contain impurities of colloidal metal atoms. The type of the metal atoms is easily colloidizable and is not particularly limited, and may include at least one metal atom selected from the group consisting of Na, K, Ca, Fe, Cu, Mg, Mn, Li, Al, Cr, Ni, Zn, and Pb. In the chemical liquid prepared by the chemical liquid production apparatus of the present disclosure, the total content of particles having a size of 0.03 μm or more is preferably within a predetermined range of 100 or less per 1 ml of the chemical liquid.

[0037] <Organic impurities> Organic impurities mean compounds different from the organic solvent which is the main component contained in the chemical liquid, and refer to organic substances contained in a content of 5000 mass ppm or less with respect to the total mass of the chemical liquid, and those which correspond to organic impurities and do not correspond to the organic solvent shall be used.

[0038] Even in a clean room, volatile organic compounds are present in the atmosphere. Some organic impurities are derived from shipping and storage equipment, and some are present in the raw materials from the beginning. Other examples of organic impurities include by-products and / or unreacted reactants generated when the organic solvent is synthesized.

[0039] The total content of organic impurities in the chemical liquid is not particularly limited. From the viewpoint of improving the manufacturing yield of semiconductor devices, the total content of organic impurities is preferably ppm, 0.1 to 5000 mass ppm, more preferably 1 to 2000 mass ppm, still more preferably 1 to 1000 mass ppm, particularly preferably 1 to 500 mass ppm, and most preferably 1 to 100 mass ppm with respect to the total mass of the chemical liquid.

[0040] The content of organic impurities in the chemical liquid can be measured by a gas chromatograph mass spectrometry (GCMS) apparatus.

[0041] <Moisture (water)> Moisture has the effect of destabilizing the chemical and physical states of the semiconductor surface. Moisture may be generated from ambient air or residues of wet processes. Moisture may be water inevitably contained in raw materials included in chemical liquids, water inevitably contained during the manufacture of chemical liquids, or water intentionally introduced.

[0042] The water content in the chemical liquid is not particularly limited. Generally, the water content is preferably 2.0% by mass or less, more preferably 1.0% by mass or less, and still more preferably 0.5% by mass or less with respect to the total mass of the chemical liquid. If the water content in the chemical liquid is 1.0% by mass or less, the manufacturing yield of semiconductor chips is further improved. The lower limit is not particularly limited, but is often about 0.01% by mass. In manufacturing, it is difficult to make the water content below the above value.

[0043] The water content means the water content that can be measured using an apparatus based on the Karl Fischer moisture measurement method as the measurement principle.

[0044] Hereinafter, embodiments of the present disclosure will describe an exemplary chemical liquid manufacturing apparatus and an exemplary method for manufacturing a chemical liquid using the same. The chemical liquid manufacturing apparatus includes at least a plurality of material processing systems, and the number of unnecessary particulates (particles) and the amount of metal impurities in the chemical liquid prepared using the chemical liquid manufacturing apparatus are limited within a predetermined range. Therefore, the generation of residues and / or particle defects is suppressed, and the yield of semiconductor wafers is improved.

[0045] <Chemical liquid manufacturing apparatus> FIG. 1 is a schematic diagram showing the configuration of an exemplary chemical liquid manufacturing apparatus according to some embodiments of the present disclosure. As shown in FIG. 1, the chemical liquid manufacturing apparatus 10 is connected to a processing target supply unit 20, holds or transports a material to be processed by the chemical liquid manufacturing apparatus 10, for example, a processing target, and generates a chemical liquid in which the number of unnecessary fine particles (particles) and the amount of metal impurities in the chemical liquid are controlled within a predetermined range. The processing target supply unit 20 is not particularly limited as long as it continuously or intermittently supplies an object to be processed to the chemical liquid manufacturing apparatus 10. The processing target supply unit 20 can include a material receiving tank, sensors such as a level gauge (not shown), a pump (not shown), a valve for controlling the flow of the processing target material (not shown), and the like. In FIG. 1, the chemical liquid manufacturing apparatus 10 is connected to one processing target supply unit 20. However, the present disclosure is not limited thereto. In some exemplary embodiments, a plurality of processing target supply units 20 are provided in parallel for each type of processing target material to be processed by the chemical liquid manufacturing apparatus 10.

[0046] The processing target material can include, for example, raw materials used for the preparation of processing liquids applied to semiconductor manufacturing, such as prewetting liquids, developing solutions, rinsing liquids, cleaning solutions, stripping solutions, and the like. In the following description, unless otherwise specified, the term "preparation" of a specific material is used to mean the case where a specific material or chemical liquid in most embodiments of the present disclosure is provided by, for example, purification, reaction, or mixing of the processing target material. The processing target material may be synthesized in-house or may be a commercially available product purchased from a vendor.

[0047] In certain embodiments of the present disclosure, the material to be processed is a raw organic solvent used in the preparation of a pre-wetting solution. For example, the raw organic solvent is processed by the chemical liquid manufacturing apparatus 10 to form an ultra-high purity pre-wetting solution, such as high purity grade cyclohexanone (CyH), cyclopentanone (CyPe), ethyl lactate (EL), propylene glycol monomethyl ether (PGME), propylene glycol monoethyl ether (PGEE), propylene glycol monomethyl ether acetate (PGMEA), propylene glycol monopropyl ether (PGPE), etc., or combinations thereof.

[0048] As shown in FIG. 1, the chemical liquid manufacturing apparatus 10 includes at least one heat exchanger 100 for setting the temperature of the material to be processed within an optimal processing range, and a first material processing system 110 coupled to the heat exchanger 100 via a first transport conduit 160b. Here, the heat exchanger 100 is directly or indirectly connected to the material supply unit 20 to be processed, for example, via an introduction conduit 160a. The first material processing system 110 includes one or more filter media (horizontal solid lines indicated by reference numeral 114), and the first transport conduit 160b is connected between the heat exchanger 100 and, for example, a supply port 110a of the first material processing system 110.

[0049] In certain exemplary embodiments, one or more filtration media 114 may each be compartmentalized and contained within one or more housings 112. For example, the first material processing system 110 can include at least one housing 112 selected from the first housing 112a, the second housing 112b, and the third housing 112c, and the at least one housing 112 contains and houses the filtration media 114 of one or more filtration media 114 therein. In other words, according to the above example, the first material processing system 110 can include one housing 112 (any one of the first housing 112a, the second housing 112b, or the third housing 112c), or two housings 112 (any combination of two of the first housing 112a, the second housing 112b, and the third housing 112c), or three housings (the first housing 112a, the second housing 112b, and the third housing 112c). Note that the above example is for illustrative purposes, and the number of housings is not limited to the illustrated example. In other exemplary embodiments, the first material processing system 110 can include more housings 112 in addition to the first housing 112a, the second housing 112b, and the third housing 112c, for example, one, two, five, or ten or more. Further, there may be no separate housing 112, and one or more filtration media 114 can be configured without being compartmentalized in the first material processing system 110. In still other exemplary embodiments, the first material processing system 110 can include other material processing modules (not shown) in addition to one or more filtration media 114.

[0050] According to some embodiments of the present disclosure, the first material processing system 110 may be connected to the collection tank 130 via the second transport conduit 160c, and the second transport conduit 160c is connected, for example, between the outflow port 110b of the first material processing system 110 and the collection tank 130. It is understood that pumps and valves are installed in various conduits such as the outflow port and supply port of the processing target supply unit 20, the heat exchanger 100, the first material processing system 110, the collection tank 130, etc. as required.

[0051] The chemical liquid manufacturing apparatus 10 further includes a second material processing system 120 that communicates with the first material processing system 110 by being directly connected to the collection tank 130 or indirectly connected, for example, via a third transport conduit 160d, a fourth transport conduit 160e that couples the second material processing system 120 to the next processing apparatus or packaging 140, a recirculation conduit 160f that branches from the fourth transport conduit 160e and can be connected to the collection tank 130 for recirculating and supplying a partially purified processing target to be processed again by the second material processing system 120, and a sample detector 150 that is coupled to the second material processing system 120 for monitoring the impurity content in the chemical liquid. Here, The third transport conduit 160d is connected between the collection tank 130 and the supply port 120a, the second material processing system 120 includes one or more filter media 124, and the fourth transport conduit 1 60 e may be connected to the outflow port 120b of the second material processing system 120. It is understood that pumps and valves are installed in various conduits such as the outflow port and supply port of the second material processing system 120, the next processing apparatus or packaging 140, and the sample detector 150 as necessary.

[0052] In certain exemplary embodiments of the present disclosure, one or more filtration media 124 may each be compartmentalized and contained within one or more housings 122. For example, the second material processing system 120 can include at least one housing 122 selected from the fourth housing 122a, the fifth housing 122b, and the sixth housing 122c, and the at least one housing 122 contains and houses one or more units of the filtration media 124 therein. In other words, according to the above example, the second material processing system 120 can include one, two, or three housings 122. Note that the above example is for illustrative purposes only, and the number of housings is not limited to the illustrated example. In other exemplary embodiments, the second material processing system 120 can include more housings 122, for example, one, two, five, or ten or more, in addition to the fourth housing 122a, the fifth housing 122b, and the sixth housing 122c. Further, there may be no separate housing 122, and one or more filtration media 124 can be configured without being compartmentalized in the second material processing system 120. In still other exemplary embodiments, the second material processing system 120 can include other material processing modules not shown in the figures in addition to one or more filtration media 124.

[0053] In some exemplary embodiments, the first material processing system 110 can also include a recirculation conduit 160h that recirculates a partially purified material to be processed into the first material processing system 110 for further processing by the first material processing system 110. In the example shown in FIG. 1, the recirculation conduit 160h branches from a fifth transport conduit 160i configured upstream of the outflow port 110b of the first material processing system 110, but the above example is for illustrative purposes only and is not intended to be limiting. In other examples, the recirculation conduit 160h may be configured downstream of the outflow port 110b as long as it is configured upstream of the collection tank 130 and / or the second material processing system 120. Further, the recirculation conduit 160h may be connected to the introduction conduit 160a upstream of the heat exchanger 100, or to the first transport conduit 160b downstream of the heat exchanger 100, or to the supply port 110a of the first material processing system 110.

[0054] Also, referring to FIG. 1, according to some embodiments, the chemical liquid manufacturing apparatus 10 is configured such that the first material processing system 110 is disposed upstream of the second material processing system 120, and the object to be processed first passes through the first material processing system 110 or is first processed by the first material processing system 110, and then the second material processing system 120 follows. However, in an alternative embodiment, the chemical liquid manufacturing apparatus 10 may be configured such that the second material processing system 120 is disposed upstream of the first material processing system 110, and the object to be processed first passes through the first second material processing system 120 or is processed by the second material processing system 120, and then the first material processing system 110 follows.

[0055] In certain embodiments, the first material processing system 110 is configured for in-line single pass. More specifically, when the chemical liquid manufacturing apparatus 10 is configured to dispose the first material processing system 110 upstream of the second material processing system 120, the material to be processed is either processed by the first material processing system 110, passes through the first material processing system 110 once, is discharged to the collection tank 130 before proceeding to the second material processing system 120, or bypasses the collection tank 130 and is directly conveyed to the second material processing system 120. According to a particular exemplary embodiment of the present disclosure, in the case of an in-line single pass, the first material processing system 110 includes one unit of filtration medium 114 selected from the first filtration medium 114a, the second filtration medium 114b, the third filtration medium 114c, and any combination thereof. In other words, the first material processing system 110 configured for a single in-line process can include one unit of the first filtration medium 114a, one unit of the second filtration medium 114b, or one unit of the third filtration medium 114c, or include one unit of the first filtration medium 114a and one unit of the second filtration medium 114b, or include one unit of the first filtration medium 114a and one unit of the third filtration medium 114c, or include one unit of the second filtration medium 114b and one unit of the third filtration medium 114c, or can include one unit of the first filtration medium 114a, one unit of the second filtration medium 114b, and one unit of the third filtration medium 114c. The first material processing system 110 is configured such that the material to be processed passes through and is processed by one unit of filtration medium 114 selected from the first filtration medium 114a, the second filtration medium 114b, the third filtration medium 114c, and any combination thereof before being delivered to the second material processing system 120.

[0056] However, the present disclosure is not so limited. In alternative embodiments, the first material processing system 110 can also be configured for multi-pass recirculation. Note that the number of times the material to be processed is processed by the first material processing system 110 is not limited as long as the processing by the first material processing system 110 is completed before the material to be processed is transferred to the second material processing system 120 or the next processing stage. In some exemplary embodiments, the first material processing system 110 is configured to recirculate and process the material to be processed more than once, e.g., twice. When the first material processing system 110 is configured for recirculation to process the material to be processed more than once, e.g., twice, the first material processing system 110 can include two-unit filtration media 114 selected from the first filtration media 114a, the second filtration media 114b, the third filtration media 114c, and any combination thereof. In other words, the first material processing system 110 can include two units of the first filtration media 114a, two units of the second filtration media 114b, or two units of the third filtration media 114c, or include two units of the first filtration media 114a and two units of the second filtration media 114b, or include two units of the first filtration media 114a and two units of the third filtration media 114c, or include two units of the third filtration media 114c and two units of the second filtration media 114b, or include two units of the first filtration media 114a, two units of the second filtration media 114b, and two units of the third filtration media 114c. The first material processing system 110 sets the material to be processed to pass through two units of the second filtration media 114b selected from the first filtration media 114a, the second filtration media 114b, the third filtration media 114c, and any combination thereof, recirculates it to pass through another unit of filtration media 114 selected from the first filtration media 114a, the second filtration media 114b, the third filtration media 114c, and any combination thereof, and then proceeds to the second material processing system 120 or the next processing stage. Further, the recirculation operated by the first material processing system 110 is continuous and can be controlled, for example, by a CPU (central processing unit).However, in some alternative embodiments, the first material processing system 110 may be configured to recirculate through the filtration media 114 (114a, 114b, 114c, or any combination thereof) of the same unit.

[0057] According to the embodiment of the chemical liquid manufacturing apparatus shown in FIG. 1, the second material processing system 120 is applied to multiple consecutive circulations. However, it should be noted that the second material processing system 120 may also be configured to pass the material to be processed or to be processed only once by the second material processing system 120. The number of times the second material processing system 120 is recirculated is not particularly limited and may vary according to the conditions of the material to be processed, such as the degree of initial impurities and contamination, and the purity requirements of the chemical liquid. In a specific embodiment of the present disclosure, the second material processing system 120 is configured to recirculate and process the material to be processed at least twice. When the material to be processed is processed by the second material processing system 120 two or more times, for example, 2, 3, 4, or 10 times, the material to be processed is returned to the second material processing system 120 via the recirculation conduit 160f and additional processing is performed. In some embodiments, the material to be processed is recirculated to the collection tank 130, and the material to be processed is further delivered to the second material processing system 120. In some examples, the material to be processed can exit the second material processing system 120 through, for example, the outlet port 120b of the second material processing system 120 and be directly recirculated to the collection tank 130 or the second material processing system 120 via the recirculation conduit 160f. In other non-illustrated examples, the material to be processed may be directly recirculated to the collection tank 130 or the second material processing system 120 via the recirculation conduit 160f upstream of the outlet port 120b of the second material processing system 120.

[0058] Similar to the first material processing system 110, when the second material processing system 120 is configured to treat or process the object to be processed one or more times, a new unit of the filtration medium 124 (e.g., a new unit of the filtration medium 124 selected from the fourth filtration medium 124a, the fifth filtration medium 124b, the sixth filtration medium 124c, and combinations thereof) can be used for each pass. For example, when the object to be processed is recirculated and processed more than twice in the second material processing 120, the second material processing system 120 includes two or more units of the filtration medium 124 (selected from the fourth filtration medium 124a, the fifth filtration medium 124b, the sixth filtration medium 124c, and any combination thereof). Also, two or more units of the filtration medium 124 selected from the fourth filtration medium 124a, the fifth filtration medium 124b, the sixth filtration medium 124c, and any combination thereof may be configured simultaneously within the second material processing system 120, and the object to be processed is processed, for example, by a CPU and, in order to achieve continuous recirculation, each time by a new unit of the filtration medium 124 (selected from the fourth filtration medium 124a, the fifth filtration medium 124b, the sixth filtration medium 124c, and any combination thereof). For example, two, three, or four units of the filtration medium 124 (selected from the fourth filtration medium 124a, the fifth filtration medium 124b, the sixth filtration medium 124c, and any combination thereof) are configured simultaneously in the second material processing system 120 to achieve two, three, or four consecutive recirculations or processes of the object to be processed. It should be noted that the number of units of the filtration medium 124 (124a, 124b, 124c, or any combination thereof) and the number of recirculations are merely examples and are not intended to be limiting. In some alternative embodiments, one or two units of the filtration medium 124 (124a, 124b, 124c, or any combination thereof) are provided, and the same one or two units of the filtration medium 124 (124a, 124b, 124c, or any combination thereof) are used for multiple recirculations.

[0059] The second material processing system 120 is also configured such that at the end of each pass of the material processing process executed by the second material processing system 120, a sample of the chemical liquid can be tested by a sample detector 150, for example, on-site by an in-line particle counter. In a specific example, the sample is collected and sent to the sample detector 150 via a sampling conduit 160g, where the number of unwanted fine particles (particles) remaining in the chemical liquid and the content of metal impurities are measured by the method described below. If the number of unwanted fine particles (particles) detected in the sample and the amount of metal impurities are not within the desired predetermined range, the chemical liquid is recycled and processed again by the second material processing system 120. When high-purity chemical liquid with the number of particles and the amount of metal impurities in the chemical liquid ensured within a predetermined range is produced, the circulation or processing by the second material processing system 120 is terminated, and the chemical liquid is transported to packaging or the next processing stage 140 via a fourth transport conduit 160e connected to the outflow port 120b of the second material processing system 120.

[0060] According to some embodiments of the present disclosure, the first material processing system 110 can include at least one housing 112 selected from the first housing 112a, the second housing 112b, and the third housing 112c, and each of the selected housing(s) 112 contains or houses one unit of a filtration medium 114 (114a, 114b, 114c) therein. More specifically, the first housing 112a can include one or more units of a first filtration medium 114a, the second housing 112b can include one or more units of a second filtration medium 114b, and the third housing 112c can include one or more units of a third filtration medium 114c, where the first, second, and third filtration media 114a, 114b, and 114c have different functions or characteristics and can provide different treatments for the object to be processed. However, each of the one or more units of the filtration medium 114 (114a, 114b, 114c) corresponding to each of the selected housing 112 (112a, 112b, 112c) has the same or similar purification functions, physicochemical properties, pore sizes, and / or structural materials, etc.

[0061] Also, according to some embodiments of the present disclosure, the second material processing system 120 can include at least one housing 122 selected from the fourth housing 122a, the fifth housing 122b, and the sixth housing 122c, and each of the selected housings 122 contains or houses one or more units of a filtration medium 124 (124a, 124b, 124c) therein. More specifically, the fourth housing 122a can include one or more units of the fourth filtration medium 124a, the fifth housing 122b can include one or more units of the fifth filtration medium 124b, and the sixth housing 122c can include one or more units of the sixth filtration medium 124c, where the fourth filtration medium 124a, the fifth filtration medium 124b, and the sixth filtration medium 124c have different functions or characteristics and can provide different treatments for the object to be treated, but one or more units of the filtration medium 124 (124a, 124b, 124c) corresponding to each of the selected housings 122 (122a, 122b, 122c) each have the same or similar purification functions, physicochemical properties, pore sizes, and / or structural materials, etc.

[0062] According to some exemplary embodiments of the present disclosure, the first material processing system 110 is a multi-stage system configured to have a material to be processed cascading through exchangeable filtration media 114 (114a, 114b, 114c) connected together, each having a specific purification function and providing a specific treatment. For example, the first material processing system 110 can include at least one filtration medium 114 (114a, 114b, or 114c) selected from a particle removal filter, an ion exchange membrane, and an ion adsorption membrane. In certain specific exemplary embodiments of the present disclosure, there is at least 1 unit of the selected filtration medium 114. As an example, the first material processing system 110 can include one particle removal filter, one ion exchange membrane, and one ion adsorption membrane, respectively housed in a first housing 112a, a second housing 112b, and a third housing 112c. In another example, the first material processing system 110 can include two units of particle removal filters and two units of ion adsorption membranes, respectively housed in the second housing 112b and the third housing 112c. In yet another example, the first material processing system 110 can include one unit of an ion exchange membrane and one unit of an ion adsorption membrane, respectively housed in the first housing 112a and the second housing 112b. It should be noted that the above examples are for illustrative purposes and are not intended to be limiting.

[0063] Similarly, the second material processing system 120 is a multi-stage system configured to cascade the material to be processed through interchangeable filtration media 124 (124a, 124b, 124c) connected together, each having a specific purification function and providing a specific treatment. For example, the second material processing system 120 can include at least one filtration media 124 (124a, 124b, 124c) selected from a particle removal filter, an ion exchange membrane, and an adsorption membrane. In certain embodiments of the present disclosure, there are at least two units of selected filtration media 124. In some exemplary embodiments of the present disclosure, there are three or more units, such as 3, 4, 5, or 10 units of selected filtration media 124. As an example, the second material processing system 120 can include three particle removal filters housed in the fourth filter housing 122a and three ion exchange membranes or three ion adsorption membranes housed in the fifth filter housing 122b. In another example, the second material processing system 120 includes two, three, or four particle removal filters housed in the fourth filter housing 122a and another two, three, or four particle removal filters housed in the fifth filter housing 122b, where the particle removal filters in the two housings 122a, 122b differ in terms of pore size and / or structural material. For example, the particle removal filters in the two housings 122a, 122b can include filters having a pore size of 10 nm or less but made of completely different structural materials. In some examples, the particle removal filters in the two housings 122a, 122b include a 3 nm ultra-high molecular weight polyethylene membrane (UPE) filter and a 1 nm UPE filter, respectively, or a 5 nm modified polytetrafluoroethylene (MPTFE) filter and a 5 nm nylon filter, respectively. In some exemplary embodiments, the second material processing system 120 includes two or more units of particle removal filters currently housed in the filter housing 122, enabling continuous recirculation or processing of the material to be processed more than once, with a new unit of particle removal filter being used each time of recirculation.For example, two or more particle removal filters can be three units of 3 nm UPE filters or three units of 5 nm nylon filters for recirculation and processing of the three objects to be processed. Of course, the above examples are for illustrative purposes and are not intended to be limiting.

[0064] It should be noted that the number 124 of units of the filtration medium 114 and the number of housings 112, 122 shown and described are representative and are kept low for simplicity in both the drawings and the description.

[0065] Also, it should be noted that the number and arrangement order of the filtration media 114 (114a, 114b, 114c, or a combination thereof) and the filtration media 124 (124a, 124b, 124c, or a combination thereof), or the flow order of the object to be processed through the filtration media 114 and 124 is not particularly limited and can vary depending on the functionality of the filtration media, the initial conditions of the object to be processed, and the purity requirements of the chemical liquid. In some exemplary embodiments of the present disclosure, the material processing systems 110 and 120 are configured to have a particle removal filter disposed upstream of an ion exchange filter upstream of the ion adsorption membrane, and after the object to be processed passes through or is processed by the first particle removal filter, it proceeds to the ion exchange membrane and further to the ion adsorption membrane. However, in other exemplary embodiments, the filtration media 114 and the filtration media 124 are each configured in a different order in the material processing systems 110 and 120, and the object to be processed is passed through or processed by the filtration media 114 and the filtration media 124 in another order such that the ion exchange membrane follows the particle removal filter. In some embodiments of the present disclosure, the material processing system 110 may include more filtration media 114 having non-sieving properties (e.g., more ion exchange membranes and / or ion absorption membranes), while the material processing system 120 may include more filtration media 124 having pure sieving properties (e.g., coarser particle filters). Note that the arrangement order of the filtration media 114 and the filtration media 124 or the flow order of the object to be processed exemplified above is for illustrative purposes and is not intended to be limiting.

[0066] Furthermore, in an alternative embodiment, the first material processing system 110 can include additional filtration media or material processing modules that differ from the first filtration media 114a, the second filtration media 114b, or the third filtration media 114c in terms of the type of processing and functionality. Similarly, the second material processing system 120 can include additional filtration media that differ from the fourth filtration media 124a, the fifth filtration media 124b, or the sixth filtration media 124c in terms of the type of processing and functionality. Further, the additional filtration media in the first material processing system 110 or the second material processing system can be housed in a housing. If the filtration media 114 (114a, 114b, 114c) includes, for example, a particle removal filter, an ion exchange membrane, or an ion adsorption membrane, the additional filtration media different from the first filtration media 114a, the second filtration media 114b, or the third filtration media 114c can include an organic impurity absorption filter for removing organic impurities, or a dehydration membrane, a water absorbent, an aeration exchange device, or a heating device for removing moisture. Similarly, if the filtration media 124 (124a, 124b, 124c) includes, for example, a particle removal filter, an ion exchange membrane, or an ion adsorption membrane, the additional filtration media different from the fourth filtration media 124a, the fifth filtration media 124b, or the sixth filtration media 12 4 c and different in terms of processing and functionality can include an organic impurity absorption filter for removing organic impurities, or a dehydration membrane, a water absorbent, an aeration exchange device, or a heating device for removing moisture.

[0067] In certain exemplary embodiments, the first material processing system 110 can include a filtration medium having a function similar to that of the first filtration medium 114a, the second filtration medium 114b, or the third filtration medium 114c, but different from the first filtration medium 114a, the second filtration medium 114b, or the third filtration medium 114c in terms of pore size and / or structural material, etc. Similarly, the second material processing system 120 can include a filtration medium having a function similar to that of the fourth filtration medium 124a, the fifth filtration medium 124b, or the sixth filtration medium 124c, but different from the fourth filtration medium 124a, the fifth filtration medium 124b, or the sixth filtration medium 124c in terms of pore size and / or structural material, etc. For example, as shown in FIG. 2, in addition to the first housing 112a, the second housing 112b, and the third housing 112c, the first material processing system 110 includes a seventh housing 112d corresponding to one or more units of the seventh filtration medium 114d. The seventh filtration medium 114d can be selected from a particle removal filter, an ion exchange membrane, and an ion adsorption membrane. In some examples, the seventh filtration medium 114d can be a 3 nm UPE particle removal filter having a pore size and / or structural material different from that of the 0.2 PP (50 μm polypropylene membrane) particle removal filter of the first filtration medium 114a. It should be noted that the above examples are for illustration purposes only, and the type of the seventh filtration medium 114d, as well as the pore size and material of the seventh filtration medium 114d, are not limited to the illustrated examples. Similarly, in addition to the fourth housing 122a, the fifth housing 122b, and the sixth housing 122c, the second material processing system 120 can include an eighth housing (not shown) corresponding to one or more units of an eighth filtration medium (not shown), where the eighth filtration medium can be selected from a particle removal filter, an ion exchange membrane, and an ion adsorption membrane. It should be noted that the above examples are for explanatory purposes only and are not intended to be limiting.

[0068] [Particle removal filter] The particle removal process is a process of removing particles and / or metal impurities (solid metal impurities) in the object to be processed using a particle removal filter. The particle removal filter is not particularly limited, and a known particle removal filter can be used.

[0069] The average pore size (pore diameter) of the filter is not particularly limited, but is preferably about 0.001 to 1.0 μm (1 nm to 1000 nm), more preferably about 0.01 to 0.5 μm (10 nm to 500 nm), and even more preferably about 0.01 to 0.1 μm (10 nm to 100 nm). Within this range, while suppressing clogging of the filter, foreign matters such as impurities and aggregates contained in the purified product can be surely removed. In a specific embodiment of the present disclosure, the first material processing system 110 can include a particle removal filter having an average pore size as small as about 2 nm (for example, a microfiltration membrane having a pore diameter of 2 nm or more), and can be in the range of 0.002 μm (2 nm) or more to about 1.0 μm (1000 nm) or less. In addition to colloidal impurities containing metal atoms such as iron and aluminum, when the object to be processed contains fine particles, before performing filtration using a filter having an average pore size as small as 20 nm or 15 nm to remove finer particles, the object to be processed is filtered using a filter having an average pore size of about 50 nm. Thereby, the filtration efficiency is improved and the particle removal performance is further improved.

[0070] In some embodiments of the present disclosure, the second filtration system (The second material processing system 12 0) can include a particle removal filter having a pore size as small as about 0.001 μm (1 nm), and can be in the range of about 0.001 μm (1 nm) or more to about 0.015 μm (15 nm) or less. In a specific embodiment, the second filtration system (The second material processing system 120 ) can include a UPE filter having a pore size as small as about 3 nm. In still other embodiments, the second filtration system (The second material processing system 120 ) can include a nylon or MPTFE filter having a pore diameter of about 5 nm. Here, the average pore size can refer to the nominal value of the filter manufacturer.

[0071] Examples of the filter materials used for particle removal may include fluororesins such as polytetrafluoroethylene (PTFE), polyamide resins such as nylon, polyolefin resins such as polyethylene and polypropylene (PP) (including high density and ultra-high molecular weight), perfluoroalkoxy (PFA) resins, etc., or modified polytetrafluoroethylene (MPTFE), etc. From the perspective of effectively removing fine foreign matters such as impurities and / or aggregates contained in the chemical liquid, the filter used for particle removal in the present disclosure is composed of at least one selected from the group consisting of nylon, polypropylene (including high density polypropylene), polyethylene, polytetrafluoroethylene, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, polyimide, and polyamideimide. According to the filter made of the above materials, foreign matters with high polarity that cause residual defects and / or particle defects can be effectively removed, and the content of metal components in the chemical liquid can be effectively reduced.

[0072] The polyimide and / or polyamideimide can have at least one selected from the group consisting of a carboxy group, a salt-type carboxy group, and an -NH- bond. Regarding solvent resistance, fluororesins, polyimide, and / or polyamideimide are excellent.

[0073] [Ion exchange resin membrane (ion exchange membrane)] The ion exchange resin membrane used in this embodiment is not particularly limited, and a filter containing an ion exchange resin containing an appropriate ion exchange group fixed to the resin membrane can be used. Such ion exchange resin membranes include strongly acidic cation exchange resins obtained by chemically modifying cation exchange groups such as sulfonic acid groups on the resin membrane. For example, cellulose, diatomaceous earth, nylon (resin having an amide group), polyethylene, polypropylene, polystyrene, resin having an imide group, resin having an amide group and an imide group, fluororesin, or an ion exchange resin membrane having an integrated structure of a particle removal membrane and an ion exchange resin membrane, such as a high-density polyethylene membrane having a particle removal membrane and an ion exchange resin membrane. A polyalkylene membrane having a chemically modified ion exchange group is preferred. Polyalkylene includes, for example, polyethylene and polypropylene, and polypropylene is preferred. As the ion exchange group, a cation exchange group is preferred. The ion exchange resin membrane used in this embodiment can be various commercially available filters having a metal ion removal function. These filters are selected based on the ion exchange efficiency, and the estimated pore diameter of the filter is about 0.2 μm (200 nm).

[0074] [Ion adsorption membrane] The ion adsorption membrane is a porous membrane material having an ion exchange function. Such an ion adsorption membrane is not particularly limited as long as it has a pore diameter of 100 μm or less and an ion exchange function. Its material, type, etc. are not particularly limited. Examples of the base material constituting the ion adsorption membrane include, but are not limited to, cellulose, diatomaceous earth, nylon (resin having an amide group), polyethylene, polypropylene, polystyrene, resin having an imide group, resin having an amide group and an imide group, fluororesin, or film materials of microfiltration membranes such as high-density polyethylene resin, and membrane materials into which an ion exchange functional group is introduced. Examples of the shape of the membrane material include, as described in JP-A-2003-112060, pleated type, flat membrane type, hollow fiber type, porous body, and the like. As the ion exchange groups introduced into the membrane material, in order to optimize the elution and selection of the components to be removed, it is preferable to use a combination of at least two of cation exchange groups, chelate exchange groups, and anion exchange groups. Since the ion adsorption membrane has porosity, it is also possible to remove a part of the fine particles. In a specific embodiment of the present disclosure, the ion adsorption membrane is, for example, a nylon membrane having a small pore diameter of 0.02 μm (20 nm).

[0075] In the chemical liquid preparation process of this embodiment, the ion exchange resin membrane or the ion adsorption membrane is brought into contact with an organic solvent in advance. There are commercially available products of the ion exchange resin membrane or the ion adsorption membrane in a dry state. Further, there are also hydrophilic materials having a high affinity for an aqueous solution. In this embodiment, even when such an ion exchange resin membrane or ion adsorption membrane is used, the preliminary contact with the organic solvent effectively removes metal impurities in the untreated chemical liquid, and the reduction effect is very excellent as compared with the case where the ion exchange resin membrane or the ion adsorption membrane has not been brought into contact with the organic solvent in advance.

[0076] [Method for manufacturing chemical liquid] An exemplary method of manufacturing a chemical liquid includes providing a chemical liquid manufacturing apparatus having at least a first material processing system 110 and a second material processing system 120. The first material processing system 110 includes one or more first filtration media 114. When the first material processing system 110 includes a plurality of first filtration media 114, at least two of the first filtration media 114 differ in function, pore size, and / or structural material. The second material processing system 120 includes one or more second filtration media 124. When the second material processing system 120 includes a plurality of second filtration media 124, at least two of the second filtration media 124 differ in functionality, pore size, and / or structural material. The method of manufacturing a chemical liquid also includes transporting a processing target to the first material processing system 110, processing the processing target once with one or more first filtration media 114 in the first material processing system 110, and, if necessary, recirculating the processing target to the first material processing system 110 for reprocessing. The manufacturing method also includes delivering the processing target to the second material processing system 120, processing the processing target with one or more second filtration media 124 in the second material processing system 120, and recirculating the processing target so that the processing target is processed at least twice by the second material processing system 120. The manufacturing method further includes, at the end of each processing of the second material processing system 120, collecting a sample of the chemical liquid on-site by a sample detector 150, e.g., an in-line particle counter 150, and measuring the number of particles remaining in the chemical liquid and the content of metal impurities. If the number of particles and the amount of metal impurities detected in the sample exceed a desired predetermined range, the chemical liquid is recirculated and processed again by the second material processing system 120. When it is confirmed that the number of particles and the amount of metal impurities in the sample detected by the particle counter 150 are within a predetermined range and a high-purity chemical liquid is generated, the recirculation or processing by the second material processing system 120 is immediately terminated, and the chemical liquid is transported either for packaging or to the next stage of processing 140. 2 When the second material processing system 120 includes a plurality of second filtration media 124, at least two of the second filtration media 124 differ in functionality, pore size, and / or structural material. The method of manufacturing a chemical liquid also includes transporting a processing target to the first material processing system 110, processing the processing target once with one or more first filtration media 114 in the first material processing system 110, and, if necessary, recirculating the processing target to the first material processing system 110 for reprocessing. The manufacturing method also includes delivering the processing target to the second material processing system 120, processing the processing target with one or more second filtration media 124 in the second material processing system 120, and recirculating the processing target so that the processing target is processed at least twice by the second material processing system 120. The manufacturing method further includes, at the end of each processing of the second material processing system 120, collecting a sample of the chemical liquid on-site by a sample detector 150, e.g., an in-line particle counter 150, and measuring the number of particles remaining in the chemical liquid and the content of metal impurities. If the number of particles and the amount of metal impurities detected in the sample exceed a desired predetermined range, the chemical liquid is recirculated and processed again by the second material processing system 120. When it is confirmed that the number of particles and the amount of metal impurities in the sample detected by the particle counter 150 are within a predetermined range and a high-purity chemical liquid is generated, the recirculation or processing by the second material processing system 120 is immediately terminated, and the chemical liquid is transported either for packaging or to the next stage of processing 140.

[0077] According to some embodiments of the present disclosure, it is preferred not to use a reverse osmosis membrane (RO filter) as used in an aqueous solvent.

[0078] [Examples] Hereinafter, the present disclosure will be described more specifically based on examples. The materials, amounts used, ratios, treatment details, treatment procedures, etc. shown in the following examples can be appropriately changed without departing from the spirit of the present invention. Therefore, the scope of the present disclosure should not be construed as being limited by the following examples. "ppt", "ppb", and "ppm" are based on mass unless otherwise specified.

[0079] <Preparation of Chemical Liquid> The chemical liquid in the examples was cyclohexanone, and the raw material cyclohexanone (pretreated cyclohexanone or the object to be treated) was used to prepare the chemical liquid by feeding it into the chemical liquid production apparatus of the present disclosure.

[0080] Arrangement, selection of the filter medium 114 in the first material processing system 110 (unit A) and the filter medium 124 in the second material processing system 120 (unit B), for example, functionality, pore size, structural material, and / or the number of units of the filter medium 114 and the filter medium 124, and adjusting the number of passes of the raw material cyclohexanone through the selected filter medium 114 and the selected filter medium 124 to prepare the chemical liquid of the composition of each example.

[0081] <Wafer Map, OWPC, OWMC, Defect Evaluation> Each chemical liquid sample was collected and inserted into a wafer coating tool. After coating the sample on a bare wafer, the wafer was transferred to a laser-based inspection system for inspection. The laser-based inspection system used a laser beam to detect, count, and record the position and size of each particle on the wafer with a detection limit of 19 nm. More specifically, the particles to be counted were those having a size of 19 nm or more. Using this data, a wafer map was created to provide the total number of particles (OWPC) on the wafer.

[0082] Next, the wafer was transferred to EDX (energy dispersive x-ray) for inspection. Each particle reported by the laser-based inspection system was inspected by EDX (energy dispersive x-ray) to provide elemental information. Particles found to generate a metal signal were counted as metal particles. Metal signal The total number of particles having is summed to be reported as the OWMC (on-wafer metal count).

[0083] <Total trace metals (ppb)> Each chemical liquid sample was tested using ICP-MS (inductively coupled plasma mass spectrometry). Using the Fuji Film development method, each sample was tested for the presence of 26 metal species, and the detection limit was specific to the metal, but the general detection limit was in the range of 0.00010 - 0.030 ppb. Next, the concentrations of each metal species were summed to generate a value shown as the total trace metals (ppb).

[0084] <Liquid particle count LPC (>0.05um)> Each sample was tested using a liquid particle counter. This instrument uses laser light to obtain the number and size of particles in a liquid sample, and the detection limit was set to 0.05um. The reported value has the unit of "particles / ml".

[0085] <Evaluation results> As shown in Table 1, each example was prepared by the chemical liquid manufacturing apparatus of the present disclosure, but the chemical liquid manufacturing apparatus was configured differently to process the raw material (object to be processed) of each example. Various configurations of the chemical liquid manufacturing apparatus for processing the raw material (unprocessed cyclohexanone) were designed as various processes W, X, Y, and Z, as summarized in Table 1. The raw material (unprocessed cyclohexanone) was used as the baseline sample.

[0086]

Table 1

[0087] In another embodiment, Example W-1 was produced in the same manner as Example W, except that a filter having a minimum pore diameter (pore diameter less than 10 nm) was disposed on the most upstream side of Unit A. LPC, OWPC, and OWMP are smaller than those in Example W.

[0088] In another embodiment, Example W-2 was produced in the same manner as Example W, except that a filter having a maximum pore diameter (pore diameter greater than 50 nm) was disposed on the most upstream side of Unit A. LPC, OWPC, and OWMP are smaller than those in Example W.

[0089] The same tendency can be obtained even when the solvent is changed to a solvent selected from the group consisting of methanol, ethanol, 1-propanol, isopropanol, monomethyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monomethyl ether acetate, ethyl lactate, methyl methoxypropionate, cyclopentanone, cyclohexanone, γ-butyrolactone, diisoamyl ether, butyl acetate, 4-methyl-2-pentanol, and combinations thereof. Among them, better performance can be obtained by using cyclohexanone, PGMEA, butyl acetate, propylene glycol monomethyl ether acetate, and isopropanol, and even better performance can be obtained by using cyclohexanone.

[0090] Various evaluations were conducted. Tables 2 to 4 summarize the results.

Table 2

[0091]

Table 3

[0092]

Table 4

[0093] Samples W, X, Y, and Z have been demonstrated to be more desirable in terms of the tested attributes such as reduction of metal traces, LPC, OWPC, and OWMP. Samples W, Y, and Z have been shown to have low total trace metals. As shown in Table 2, the chemical liquids prepared by the chemical liquid manufacturing apparatus 10 of the present application have achieved the desirable advantage of significantly reducing the total number of trace metals, as shown by the output of each process compared to the input of each process. More specifically, it has been shown that the total trace metals of Sample W is 0.1837.

[0094] From the results summarized in Table 3, it was also confirmed that in the chemical liquids prepared by the chemical liquid manufacturing apparatus 10 of the present disclosure, the total liquid particle count (LPC) was significantly reduced. Compared to the baseline sample with an LPC of 122556, the LPC of Samples X and W were less than 100, 76.4 and 60.9 respectively.

[0095] As shown in Table 4, the baseline sample was shown to be significantly higher in both OWPC (149,811) and OWMP (16,646). On the other hand, it has been demonstrated that the chemical liquids prepared by the chemical liquid manufacturing apparatus 10 of the present disclosure have achieved the desired advantage of having very low counts in OWPC and OWMP. The OWPC of Samples X and W were 597 and 126 respectively, and the OWMP of Samples X and W were 43 and 1 respectively.

[0096] The above outlines the features of several embodiments so that those skilled in the art can better understand aspects of the present disclosure. Those skilled in the art should understand that the present disclosure can be easily used as a basis for designing or modifying other processes and structures to achieve the same objectives and / or achieve the same advantages as the embodiments described herein. Those skilled in the art should also understand that such equivalent structures can make various changes, substitutions, and alterations herein without departing from the spirit and scope of the present disclosure.

Claims

1. A first system configured to process a material from a material supply unit to be processed, the first system including a first filtration medium including a first particle removal filter, a first ion exchange membrane, and a first ion adsorption membrane, the first system being configured to process the material at least once, the first system; A second system disposed downstream of the first system and configured to process the material processed by the first system, the second system including a second filtration medium including a second particle removal filter, a second ion exchange membrane, and a second ion adsorption membrane, the second system being configured to process the material at least twice for the purpose of recirculation, the second system; A chemical liquid manufacturing apparatus for semiconductor manufacturing, including.

2. The chemical liquid manufacturing apparatus for semiconductor manufacturing according to claim 1, wherein the first system is configured such that the material passes through once.

3. The chemical liquid manufacturing apparatus for semiconductor manufacturing according to claim 1, wherein the second particle removal filter is a particle size sieving filter having a pore size of 10 nm or less in the second particle removal filter.

4. The chemical liquid manufacturing apparatus for semiconductor manufacturing according to claim 1, wherein the pore size of the first particle removal filter is 50 nm or more.

5. The chemical liquid manufacturing apparatus for semiconductor manufacturing according to claim 1, wherein the pore size of the first particle removal filter is 15 nm or more.

6. The chemical liquid manufacturing apparatus for semiconductor manufacturing according to claim 1, further including an on-line particle counter.

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