Systems and methods for purifying solvents

The parallel filtration system addresses solvent contamination in semiconductor manufacturing by effectively reducing metallic and particulate impurities, enhancing solvent purity and productivity.

JP7719057B2Active Publication Date: 2025-08-05FUJIFILM ELECTRONIC MATERIALS U S A INC
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Patent Information

Application Number
JP2022514622
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2019-09-03
Filing Date
2020-08-27
Publication Date
2025-08-05
Estimated Expiration
2040-08-27

AI Technical Summary

Technical Problem

The semiconductor industry faces challenges in producing high-purity solvents for semiconductor manufacturing due to contamination from metallic impurities, particulates, and organic impurities, which can degrade circuit performance and reduce manufacturing yields.

Method used

A purification system and method using multiple filters with varying pore sizes arranged in parallel to achieve ultra-high purity solvents by controlling particle and metal impurity content, including a first filter unit with larger pore size and a second unit with smaller pore sizes arranged in parallel, along with optional additional filter units for further purification.

Benefits of technology

The system effectively reduces contaminants to predetermined levels, improving semiconductor wafer yield and productivity by maintaining high flow rates without increasing backpressure.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present disclosure relates to a method and system for purifying a solvent, which can be used to clean semiconductor substrates in a multi-step semiconductor manufacturing process.
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Description

[Technical Field]

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS This application claims priority to U.S. Provisional Application Serial No. 62 / 895,198, filed September 3, 2019, the contents of which are incorporated herein by reference in their entirety. The present disclosure relates to systems and methods for purifying solvents (e.g., organic solvents). In particular, the present disclosure relates to systems and methods that can be used to obtain organic solvents having high purity, low on-wafer particle counts, and / or low on-wafer metal counts. [Background technology]

[0002] The semiconductor industry has achieved rapid improvements in the integration density of electronic components. This results from the continuous reduction in component size, ultimately allowing more and more smaller components to be integrated into a given area. These improvements are primarily due to the development of new precision and fine-grained processing techniques.

[0003] During the manufacturing of high-precision integrated circuits (ICs), various process fluids come into contact with bare or film-coated wafers. For example, the fabrication of fine metal interconnects typically involves coating the base material with a prewetting fluid before it is coated with a composite fluid to form a resist film. These process fluids, which contain unique components and various additives, are known sources of contamination for IC wafers.

[0004] Even trace amounts of contaminants in chemical solutions, such as wafer prewetting solutions and developers, can cause defects in the resulting circuit patterns. Metallic impurities at levels as low as 1.0 ppt are known to hinder the performance and stability of semiconductor devices. Furthermore, certain types of metallic contaminants can degrade oxide properties, produce inaccurate patterns, and reduce the electrical performance of semiconductor circuits, ultimately negatively impacting manufacturing yields.

[0005] Contaminants, such as metallic impurities, particulates, organic impurities, and moisture, can be inadvertently introduced into chemical fluids during various stages of their manufacture. For example, impurities may be present in raw materials, by-products, or residual unreacted reactants during chemical fluid manufacture, or may be detached or extracted from manufacturing equipment surfaces or from vessels and reaction vessels used for transport, storage, or reaction. Therefore, the reduction or elimination of insoluble and soluble contaminants from these chemical fluids used in the manufacture of high-precision, ultra-fine semiconductor electronic circuits essentially ensures the production of defect-free ICs.

[0006] In this regard, in order to produce the high-purity chemical liquids that are essential for the manufacture of ultra-fine and highly precise semiconductor electronic circuits, it is necessary to significantly improve and strictly control the standards and quality of chemical liquid manufacturing processes and systems. Summary of the Invention

[0007] Therefore, the demand for ultra-high purity chemical fluids, and the quality improvement and control of these fluids, are crucial for the fabrication of precision integrated circuits. Specific key parameters targeted for quality improvement and control include reduction of metals in the fluids and on the wafers, reduction of particle counts in the fluids and on the wafers, reduction of defects on the wafers, and reduction of organic contaminants. All of these key parameters have been shown to be influenced by the necessary provision of a purification system and proper design of the purification process.

[0008] In view of the above, the present disclosure provides, among other things, a purification system and a method using the same for purifying a solvent (e.g., an organic solvent) to prepare a semiconductor manufacturing solvent, in which the system and method control the particle count and metal impurity content in the solvent within predetermined ranges to produce an ultra-high purity solvent without generating or introducing unknown unwanted substances. Therefore, the occurrence of residue and / or particle defects is suppressed, and semiconductor wafer yield is improved. Furthermore, the inventors have unexpectedly discovered that purifying a solvent using a relatively large number of filters with a relatively small average pore size arranged in parallel can result in a process with a relatively high flow rate (e.g., higher than conventional methods in which filters with a relatively small average pore size are arranged in series but not in parallel), thereby improving the productivity of the purification system.

[0009] In one aspect, the disclosure features a method for purifying an organic solvent, including passing the organic solvent through a first filter unit and a second filter unit downstream of the first filter unit to obtain a purified organic solvent. The first filter unit includes a first housing and at least one first filter within the first housing, the first filter including a filtration medium having a first average pore size. The second filter unit includes a second housing and at least two second filters within the second housing, the at least two second filters arranged in parallel within the second housing, each of the second filters independently including a filtration medium having a second average pore size. The number of first filters within the first filter unit is fewer than the number of second filters within the second filter unit, and the first average pore size is larger than the second average pore size.

[0010] In another aspect, the disclosure features a system including a first filter unit and a second filter unit downstream of and fluidly connected to the first filter unit. The first filter unit includes a first housing and at least one first filter within the first housing, the first filter including a filtration medium having a first average pore size. The second filter unit includes a second housing and at least two second filters within the second housing, the at least two second filters arranged in parallel within the second housing, each second filter independently including a filtration medium having a second average pore size. The number of first filters within the first filter unit is fewer than the number of second filters within the second filter unit, and the first average pore size is larger than the second average pore size.

[0011] Implementations may include one or more of the following features.

[0012] In some embodiments, the methods described herein can further include passing the organic solvent through a third filter unit disposed between the first filter unit and the second filter unit, the third filter unit including a third housing and at least one third filter within the third housing, the third filter including a filtration medium having a third average pore size, and the filtration medium within the third filter including an ion exchange membrane.

[0013] In some embodiments, the methods described herein may further include sending the organic solvent exiting the second filter unit to a storage tank. In some embodiments, the methods described herein may further include recirculating the organic solvent by transferring the organic solvent from the storage tank to the first filter unit and passing the organic solvent through the first filter unit and the second filter unit. In some embodiments, the methods described herein may further include passing the organic solvent through a fourth filter unit disposed downstream of the second filter unit. The fourth filter unit includes a fourth housing and at least two fourth filters within the fourth housing, the at least two fourth filters being disposed in parallel within the fourth housing. Each of the fourth filters independently contains a filtration medium having a fourth average pore size.

[0014] In some embodiments, the methods described herein may further include transferring the organic solvent exiting the fourth filter unit to a storage tank and subsequently passing the organic solvent through the fourth filter unit, thereby recycling the organic solvent. In some embodiments, the methods described herein may further include transferring the purified solvent to a packaging station located downstream of the fourth filter unit.

[0015] In some embodiments, the organic solvent is passed through at a flow rate of about 25 to about 170 L / min.

[0016] In some embodiments, the first filter unit includes one first filter. In some embodiments, the second filter unit includes two or three second filters. In some embodiments, the third filter unit includes one to three third filters. In some embodiments, the fourth filter unit includes four to fourteen fourth filters.

[0017] In some embodiments, the first average pore size is from about 50 nm to about 200 nm, in some embodiments, the second average pore size is from about 10 nm to about 50 nm, and in some embodiments, the fourth average pore size is about 10 nm or less.

[0018] In some embodiments, the filtration media in the first, second, third, or fourth filter comprises polypropylene, high density polyethylene, ultra-high molecular weight polyethylene, nylon, polytetrafluoroethylene, or a perfluoroalkoxyalkane polymer.

[0019] In some embodiments, the number of second filters in the second filter unit is less than the number of fourth filters in the fourth filter unit.

[0020] In some embodiments, the fourth average pore size is smaller than the second average pore size.

[0021] In some embodiments, the organic solvent comprises cyclohexanone, ethyl lactate, n-butyl acetate, propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, 4-methyl-2-pentanol, or propylene carbonate. [Brief explanation of the drawings]

[0022] [Figure 1] FIG. 1 is a schematic diagram illustrating an example of a purification system employed in a method for purifying an organic solvent according to some embodiments of the present disclosure. DETAILED DESCRIPTION OF THE INVENTION

[0023] As defined herein, unless otherwise specified, all percentages expressed should be understood to be weight percent based on the total weight of the composition. Ambient temperature is defined as about 16 degrees Celsius to about 27 degrees Celsius (°C) unless otherwise specified. The term "solvent" referred to herein refers to a single solvent or a combination of two or more (e.g., three or four) solvents unless otherwise specified. In this disclosure, "ppm" means "parts per million," "ppb" means "parts per billion," and "ppt" means "parts per trillion."

[0024] In general, the present disclosure features systems and methods for purifying solvents (e.g., organic solvents). The solvents described herein can be used as wafer processing fluids (such as prewetting fluids, developers, rinses, cleaning fluids, stripping fluids, etc.) or as solvents for semiconductor materials used in semiconductor manufacturing processes.

[0025] Before being subjected to the purification method of the present disclosure, the solvent may contain an undesirable amount of contaminants and impurities. After the solvent is treated by the purification method of the present disclosure, a significant amount of contaminants and impurities may be removed from the solvent. The solvent before treatment is also referred to as "unpurified solvent" in this disclosure. The solvent before treatment can be synthesized in a factory or purchased commercially from a supplier. The solvent after treatment is also referred to as "purified solvent" in this disclosure. The "purified solvent" may contain impurities limited within a predetermined range.

[0026] Generally, the solvent referred to herein may comprise at least one (e.g., two, three, or four) organic solvent. Examples of suitable organic solvents 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, 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, n-butyl acetate, γ-butyrolactone, diisoamyl ether, isoamyl acetate, chloroform, dichloromethane, 1,4-dioxane, hexyl alcohol, 2-heptanone, isoamyl acetate, propylene carbonate, and tetrahydrofuran.

[0027] In some embodiments, the solvent is a prewetting liquid. Examples of prewetting liquids include at least one of cyclopentanone (CyPe), cyclohexanone (CyH), monomethyl ether, 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 solvent can be a developer, such as n-butyl acetate, or a rinse, such as 4-methyl-2-pentanol (MIBC).

[0028] In some embodiments, the untreated or unpurified organic solvent may have a purity of about 95% or more (e.g., about 96% or more, about 97% or more, about 98% or more, or about 99% or more). In some embodiments, the treated or purified organic solvent obtained from the methods described herein may have a purity of about 99.5% or more (e.g., about 99.9% or more, about 99.95% or more, about 99.99% or more, about 99.995% or more, or about 99.999% or more). As used herein, "purity" refers to the weight percent of the solvent in the total weight of the liquid. The content of the organic solvent in the liquid may be measured using a gas chromatography-mass spectrometry (GCMS) device.

[0029] In some embodiments, the boiling point of the solvent described herein is about 200° C. or less (e.g., about 150° C. or less) or about 50° C. or more (e.g., about 100° C. or more) from the viewpoint of improving the manufacturing yield of semiconductor chips. In this disclosure, boiling point means the boiling point at 1 atmosphere.

[0030] Generally, impurities contained in the organic solvent before treatment may include metal impurities, particles, and others such as organic impurities and moisture.

[0031] As described herein, metal impurities can be in solid form (e.g., metal alone, particulate metal-containing compounds, etc.). Examples of common metal impurities include heavy metals such as iron (Fe), aluminum (Al), chromium (Cr), lead (Pb), and nickel (Ni), as well as ionic metals such as sodium (Na), potassium (K), and calcium (Ca). Depending on the type of metal, metal impurities can reduce oxide integrity, degrade MOS gate stacks, and shorten device lifetime. In organic solvents purified by the methods described herein, the total trace metal content is preferably within a predetermined range of 0 to 300 ppt by weight (e.g., 0 to 150 ppt).

[0032] In this disclosure, substances with a size of 0.03 μm or greater are referred to as "particles" or "particulate matter." Examples of particles include dust, dirt, organic solids, and inorganic solids. Particles may also contain colloidal metal atom impurities. The type of metal atom that can be easily colloidalized 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 organic solvents purified by the methods described herein, the total number of particles with a size of 0.03 μm or greater is preferably within a predetermined range of 100 or less (e.g., 80 or less, 60 or less, 50 or less, 40 or less, or 20 or less) per ml of solvent. The number of "particles" in a liquid medium can be counted using a light-scattering liquid particle counter, which is called the LPC (liquid particle count).

[0033] As used herein, organic impurities refer to organic substances, distinct from organic solvents, present in a concentration of 5,000 ppm by mass or less based on the total mass of the liquid containing the organic solvent and the organic impurities. Organic impurities can be volatile organic compounds present in the atmosphere, even in clean rooms. Some organic impurities originate from transportation and storage facilities, while others are originally present in the raw materials. Other examples of organic impurities include by-products and / or unreacted reactants produced when the organic solvent is synthesized.

[0034] The total content of organic impurities in the purified organic solvent is not particularly limited. From the viewpoint of improving the manufacturing yield of semiconductor devices, the total content of organic impurities in the purified organic solvent may be 0.1 to 5000 ppm by mass (e.g., 1 to 2000 ppm by mass, 1 to 1000 ppm by mass, 1 to 500 ppm by mass, or 1 to 100 ppm by mass). The content of organic impurities in the solvents described herein may be measured using a gas chromatography-mass spectrometry (GC-MS) device.

[0035] Figure 1 is a schematic diagram illustrating a purification system configuration according to some embodiments of the present disclosure. As shown in Figure 1, purification system 10 includes a supply unit 20, a first filtration system 110, a storage tank 130, a second filtration system 120, and a packaging station 140, all of which are fluidly connected to each other (e.g., via one or more conduits).

[0036] Generally, the supply unit 20 (e.g., a tank) is configured to hold or transport a starting material (e.g., an untreated or unpurified organic solvent). The starting material may be processed by the purification system 10 to generate or produce a purified organic solvent having a number of unwanted contaminants (e.g., particulate matter, organic impurities, metal impurities) limited within a predetermined range. The type of supply unit 20 is not particularly limited, as long as it continuously or intermittently supplies the starting material to other components of the purification system 10. In some embodiments, the supply unit 20 may include a material receiving tank, a sensor such as a level gauge (not shown), a pump (not shown), and / or a valve (not shown) for controlling the flow of the starting material. In FIG. 1 , the purification system 10 includes one supply unit 20. However, in some embodiments, multiple supply units 20 may be provided (e.g., in parallel or series) for various starting materials processed by the purification system 10.

[0037] Purification system 10 may include at least one first filtration system 110 and at least one second filtration system 120. Generally, first filtration system 110 performs an initial filtration of the starting material (e.g., crude organic solvent) to remove a majority of impurities and / or particles, and second filtration system 120 performs a subsequent filtration to remove remaining impurities and particulates to obtain an ultra-pure organic solvent.

[0038] In some embodiments, purification system 10 may optionally include a temperature control unit 100 for setting or maintaining the temperature of the organic solvent within a specific temperature range so that the organic solvent is maintained at a substantially constant temperature during the purification process. As described herein, the temperature control unit may include, for example, but is not limited to, a commercially available recirculating heating / cooling unit, a condenser, or a heat exchanger that may be installed in the conduits of purification system 10. Temperature control unit 100 may be configured, for example, between supply unit 20 and first filtration system 110. In some embodiments, temperature control unit 100 may set the temperature of the organic solvent to about 80°F or less (e.g., about 75°F or less, about 70°F or less, about 65°F or less, or about 60°F or less) and / or about 30°F or more (e.g., about 40°F or more, about 50°F or more, or about 60°F or more). In some embodiments, because the pumps used in purification system 10 may generate heat and increase the solvent temperature, purification system 10 may include additional temperature control units (e.g., units 170 and 180 described below) in appropriate locations to maintain the solvent temperature at a predetermined value.

[0039] Referring to FIG. 1, the first filtration system 110 may include an optional temperature control unit 100, a supply port 110a, one or more (e.g., 2, 3, 4, 5, or 10) filter units (e.g., units 112, 114, and 116), an outlet port 110b, an optional recirculation conduit 160h, and one or more optional temperature control units 170, all of which are fluidly connected to each other (e.g., via one or more conduits).

[0040] In some embodiments, each filter unit in the first filtration system 110 may include a filter housing and one or more (e.g., 2, 3, 4, 5, or 6) filters within the filter housing. Each filter may include a filtration medium having an average pore size. The filters may be arranged in parallel or in series within the filter housing. During use, if two filters are arranged in parallel, the solvent to be purified passes through the two filters in parallel (i.e., substantially simultaneously). Conversely, when two filters are arranged in series, the solvent to be purified passes through the two filters sequentially during use. In some embodiments, some filter units may include multiple filters in parallel within the filter housing to increase flow rate and improve productivity.

[0041] For example, the first filtration system 110 shown in Figure 1 includes three filter units (i.e., units 112, 114, and 116), each including a filter housing and one or more filters (e.g., filters 112a, 114a, and 116a) within the filter housing. In other embodiments, the first filtration system 110 may also include other purification modules (not shown) in addition to the three filter units shown in Figure 1.

[0042] Referring to FIG. 1 , filter unit 112 may include one or more filters 112a within a housing, filter unit 114 may include one or more filters 114a within a housing, and filter unit 116 may include one or more filters 116a within a housing. Filters 112a, 114a, and 116a may differ in function or characteristics and may provide different purification processes. In some embodiments, the specific filters (e.g., 112a, 114a, and 116a) housed within corresponding filter units (e.g., 112, 114, and 116) may have the same or similar purification function, physicochemical properties, pore size, and / or materials of construction. In some embodiments, each filter within a filter unit may be independently selected from the group consisting of particle removal filters, ion exchange filters, and ion absorption filters.

[0043] In some embodiments, filter unit 112 (also referred to herein as a first filter unit) may include a filter housing (also referred to herein as a first housing) and at least one (e.g., two or three) filter 112a (also referred to herein as a first filter) within the filter housing. In some embodiments, when filter unit 112 includes two or more filters 112a, the filters 112a may be arranged in parallel.

[0044] In some embodiments, filter 112a can be a particle removal filter for removing relatively large particles from the organic solvent. In some embodiments, filter 112a can include a filtration medium having an average pore size (also referred to herein as a first average pore size) of about 200 nm or less (e.g., about 180 nm or less, about 160 nm or less, about 150 nm or less, about 140 nm or less, about 120 nm or less, or about 100 nm or less) and / or about 50 nm or more (e.g., about 60 nm or more, about 70 nm or more, about 80 nm or more, about 90 nm or more, or about 100 nm or more). Within these ranges, foreign matter, such as impurities and aggregates, contained in the organic solvent can be reliably removed while minimizing clogging of filter 112a.

[0045] Examples of suitable filtering materials for the filter 112a include fluoropolymers (e.g., polytetrafluoroethylene (PTFE), perfluoroalkoxyalkane polymers (PFA), or modified polytetrafluoroethylene (MPTFE)), polyamide resins such as nylon (e.g., nylon 6 or nylon 66), and polyolefin resins (including high-density and ultra-high molecular weight resins) such as polyethylene (PE) and polypropylene (PP). For example, the filtering medium in the particle removal filter may be made of at least one polymer selected from the group consisting of polypropylene (e.g., high-density polypropylene), polyethylene (e.g., high-density polyethylene (HDPE) or ultra-high molecular weight polyethylene (UPE)), nylon, polytetrafluoroethylene, or perfluoroalkoxyalkane polymers. Filters made of the above materials may effectively remove foreign matter (e.g., highly polar) that tends to cause residue and / or particle defects and efficiently reduce the content of metal components in the chemical solution. In some embodiments, the filter unit 112 may include one filter 112a made of polypropylene having an average pore size of approximately 200 nm.

[0046] In some embodiments, filter unit 116 (also referred to herein as a second filter unit) may include a filter housing (also referred to herein as a second housing) and at least two (e.g., three or four) filters 116a (also referred to herein as second filters) within the filter housing. Filter 116a may be a particle removal filter for removing relatively small particles from the organic solvent. In some embodiments, filter 116a may include a filtration medium having an average pore size (also referred to herein as a second average pore size) of about 50 nm or less (e.g., about 45 nm or less, about 40 nm or less, about 35 nm or less, about 30 nm or less, about 25 nm or less, or about 20 nm or less) and / or about 10 nm or more (e.g., about 15 nm or more, about 20 nm or more, about 25 nm or more, or about 30 nm or more). In some embodiments, the average pore size of the filtration medium in filter 116a may be smaller than the average pore size of the filtration medium in filter 112a. In such an embodiment, filter 116a may be used to remove particles smaller than those removed by filter 112a.

[0047] In some embodiments, the filter 116a in the filter unit 116 may include an ion-absorbing membrane for removing relatively small particles and / or metal ions from an organic solvent. The ion-absorbing membrane may have a porous membrane material and may have ion exchange functionality. Examples of suitable materials that can be used to fabricate the ion-absorbing membrane include, but are not limited to, microfiltration membrane film materials such as cellulose, diatomaceous earth, polyamide resins such as nylon (e.g., nylon 6 or nylon 66), polyethylene (e.g., high-density polyethylene or ultra-high-molecular-weight polyethylene), polypropylene, polystyrene, resins having imide groups, resins having amide and imide groups, fluororesins (e.g., polytetrafluoroethylene (PTFE), perfluoroalkoxyalkane polymers (PFA), or modified polytetrafluoroethylene (MPTFE)), membrane materials with ion-exchange functional groups, and the like. For example, the filter 116a may include at least one polymer selected from the group consisting of polypropylene (e.g., high-density polypropylene), polyethylene (e.g., high-density polyethylene or ultra-high-molecular-weight polyethylene), nylon, polytetrafluoroethylene, or perfluoroalkoxyalkane polymers.

[0048] In some embodiments, at least some (e.g., all) of the filters 116a may be arranged in parallel within the filter unit 116, and the remaining filters 116a (if any) within the filter unit 116 may be arranged in series. When two filters are arranged in parallel, the organic solvent to be purified may pass through the two filters in parallel (e.g., simultaneously). In some embodiments, the number of filters 116a (e.g., arranged in parallel) within the filter unit 116 may be greater than the number of filters 112a within the filter unit 112. For example, if the filter unit 112 includes one filter 112a, the filter unit 116 may include two or three filters 116a arranged in parallel. Without wishing to be bound by theory, it is believed that an advantage of having more filters arranged in parallel within the filter unit 116 than within the filter unit 112 is that the system 10 may provide increased flow rates and have improved productivity, or the flow rate of the system 10 may be maintained without increasing the backpressure of the system. Without wishing to be bound by theory, it is believed that if the average pore size of the filtration medium in filter 116a is smaller than the average pore size of the filtration medium in filter 112a, the flow rate of the organic solvent through filter 116a may be reduced compared to the flow rate of the organic solvent through filter 112a. Therefore, it is believed that the flow rate and productivity of system 10 may be increased by arranging multiple filters 116a in parallel.

[0049] In some embodiments, the filter unit 116 may include three filters 116a arranged in parallel and having an average pore size of about 50 nm and made of ultra-high molecular weight polyethylene.

[0050] In some embodiments, purification system 10 may include an optional filter unit 114 (also referred to herein as a third filter unit). In some embodiments, filter unit 114 may include a filter housing (also referred to herein as a third housing) and at least one (e.g., two or three) filter 114a (also referred to herein as a third filter) within the filter housing. In some embodiments, at least some (e.g., all) of the filters 114a may be arranged in parallel within filter unit 114, and the remaining filters 114a (if any) may be arranged in series. In some embodiments, the number of filters 114a within filter unit 114 (e.g., arranged in parallel) may be greater than the number of filters 112a within filter unit 112. For example, if filter unit 112 includes one filter 112a, filter unit 114 may include two or three filters 114a (e.g., arranged in parallel). Without wishing to be bound by theory, it is believed that an advantage of having more filters arranged in parallel in filter unit 114 than in filter unit 112 is that system 10 may provide increased flow rates and have improved productivity, or the flow rates of system 10 may be maintained without increasing back pressure in the system.

[0051] In some embodiments, the filter 114a in the filter unit 114 may be an ion exchange filter. For example, the filter 114a may include one or more ion exchange resin membranes for removing charged particles and / or metal ions from organic solvents. The ion exchange resin membranes used in the present disclosure are not particularly limited, and filters containing ion exchange resins with appropriate ion exchange groups fixed to the resin membrane may be used. Examples of such ion exchange resin membranes include strongly acidic cation exchange resins with cation exchange groups (e.g., sulfonic acid groups) chemically modified on the resin membrane. Examples of suitable resin membranes include those containing cellulose, diatomaceous earth, nylon (a resin with amide groups), polyethylene (e.g., high-density polyethylene or ultra-high-molecular-weight polyethylene), polypropylene, polystyrene, resins with imide groups, resins with amide and imide groups, fluororesins (e.g., polytetrafluoroethylene or perfluoroalkoxyalkane polymers), or high-density polyethylene membranes. In some embodiments, the ion exchange resin membrane may have an integrated structure of a particle removal membrane and an ion exchange resin membrane. A polyalkylene (e.g., PE or PP) membrane with ion exchange groups chemically modified on the membrane is preferred. The ion exchange group is preferably a cation exchange group. The filter equipped with the ion exchange resin membrane used in the present disclosure may be a commercially available filter equipped with a metal ion removal function. These filters can be selected based on ion exchange efficiency and have an estimated pore size in the range of about 100 nm to about 500 nm.

[0052] Examples of membrane material shapes include pleated, flat, hollow fiber, and porous bodies as described in JP 2003-112060 A. To optimize the elution and selectivity of the components to be removed, it is preferable to use a combination of at least two of the cation-exchange groups, chelate-exchange groups, and anion-exchange groups as ion-exchange groups introduced into the membrane material. Because ion-adsorption membranes are porous, they can also remove some of the fine particles.

[0053] In some embodiments, the filter unit 114 may include three filters 114a arranged in parallel and which are ion exchange filters made from polytetrafluoroethylene.

[0054] In some embodiments, first filtration system 110 may optionally include a recirculation conduit 160h to form a recirculation loop for recirculating the partially purified organic solvent back to first filtration system 110 for processing again by a filter in first filtration system 110. In some embodiments, the partially purified organic solvent is recycled at least two times (e.g., at least three times, at least four times, or at least five times) before being transferred to storage tank 130.

[0055] Generally, storage tank 130 can be any suitable container for storing chemical liquid. In some embodiments, storage tank 130 can have a suitable capacity. For example, storage tank 130 can have a capacity of about 1000 liters or more (e.g., about 2000 liters or more, about 3000 liters or more, or about 5000 liters or more) and / or about 30,000 liters or less (e.g., about 25,000 liters or less, about 20,000 liters or less, about 15,000 liters or less, or about 10,000 liters or less). In some embodiments, storage tank 130 does not include any agitators or baffles.

[0056] In some embodiments, an optional temperature control unit 170 (e.g., a heat exchanger) may be configured along recirculation conduit 160h. In such embodiments, temperature control unit 170 may be configured for a temperature of about 80°F or less (e.g., about 75°F or less, about 70°F or less, or about 65°F or less) and / or about 30°F or more (e.g., about 40°F or more, about 50°F or more, or about 60°F or more), thereby maintaining the temperature of the partially purified organic solvent at about 80°F or less and recirculating it to first filtration system 110. In the example shown in FIG. 1 , recirculation conduit 160h is configured upstream of outlet port 110b of first filtration system 110. In some embodiments, recirculation conduit 160h may be configured downstream of outlet port 110b. It is understood that pumps and valves may be installed in the various conduits, outlet and supply ports of first filtration system 110, supply unit 20, and temperature control unit 100, as needed.

[0057] As an example shown in FIG. 1 , purification system 110 may optionally include a temperature control unit 170 (e.g., a heat exchanger) configured between filter unit 112 and filter unit 114 to control the temperature of the organic solvent to about 80°F or less (e.g., about 75°F or less, about 70°F or less, or about 65°F or less) and / or about 30°F or more (e.g., about 40°F or more, about 50°F or more, or about 60°F or more) before the organic solvent enters filter unit 114 for processing.

[0058] It should also be noted that the location of temperature control unit 170 is not limited to the above examples. In some embodiments, temperature control unit 170 may be configured upstream of filter unit 112, between filter units 114 and 116, or downstream of filter unit 116. In such embodiments, another temperature control unit may or may not be installed downstream of filter unit 112 and before entry into a subsequent filter unit (e.g., filter unit 114 and / or filter unit 116). Configuring another temperature control unit downstream of filter unit 112 is optional, as long as other means or devices (e.g., pumps) capable of reintroducing thermal energy into the organic solvent are not introduced or disposed between filter unit 112 and a subsequent filter (e.g., filter 114 or 116).

[0059] In some embodiments, filter units 112, 114, and 116 in first filtration system 110 may not include filter housings, and filters 112a, 114a, and 116a may be configured without compartmentalization within first filtration system 110. For example, first filtration system 110 may be a multi-stage system including interchangeable filters (e.g., 112a, 114a, and 116a) linked together within first filtration system 110, and the organic solvent may be passed through these filters in series. In such embodiments, temperature control unit 170 may be configured anywhere upstream of the first ion exchange filter or ion adsorption filter through which the organic solvent passes or passes in series. For example, if the first filtration system 110 contains, in sequence and downstream of the supply port 110a, a particle removal filter A, a particle removal filter B, an ion exchange membrane A, an ion exchange membrane B, and an ion adsorption membrane A, a temperature control unit 170 may be configured between the particle removal filter B and the ion exchange membrane A to adjust and control the temperature of the organic solvent to about 80° F. or less before the organic solvent is processed through the ion exchange membrane A and the subsequent ion exchange membrane B and ion adsorption membrane A. It should be noted that the above example is for illustrative purposes and is not intended to be limiting.

[0060] 1, purification system 10 also includes a second filtration system 120 in fluid communication between storage tank 130 and packaging station 140. Second filtration system 120 may include a supply port 120a, one or more (e.g., two, three, four, five, or ten) filter units 122, an outlet port 120b, an optional recirculation conduit 160f, and one or more optional temperature control units 180, all in fluid communication with each other (via one or more conduits). It is understood that pumps and valves may be installed in the various conduits, outlet and supply ports, and temperature control units in second filtration system 120, as needed.

[0061] In some embodiments, filter unit 122 (also referred to herein as the fourth filter unit) may include a filter housing (also referred to herein as the fourth housing) and at least two filters 122a (also referred to herein as fourth filters) within the filter housing. For example, filter unit 122 may include 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, or 14 filters 122a within the filter housing. The second filtration system 120 shown in FIG. 1 includes one filter unit 122. In some embodiments, second filtration system 120 may include two or more (e.g., three or four) filter units 122. In such embodiments, filter unit 122 may not have a separate housing, and filters 122a may be configured without compartmentalization within second filtration system 110. In other embodiments, second filtration system 120 may also include other purification modules (not shown) in addition to filter unit 122.

[0062] In some embodiments, filters 122a may have different functionality or characteristics and provide different purification processes. In some embodiments, filters 122a housed within filter unit 122 may have the same or similar purification function, physicochemical properties, pore size, and / or materials of construction. In some embodiments, each filter 122a may be independently selected from the group consisting of a particle removal filter, an ion exchange filter, and an ion absorption filter.

[0063] In some embodiments, filter 122a may include an ion-absorbing membrane (such as that described above with respect to filter 116a) for removing fine charged particles and / or metal ions in the organic solvent being purified. In some embodiments, filter 122a may include a filtration medium having an average pore size (also referred to herein as a fourth average pore size) of about 10 nm or less (e.g., about 7 nm or less, about 5 nm or less, about 3 nm or less, or about 1 nm or less) and / or about 1 nm or more (e.g., about 3 nm or more, or about 5 nm or more). In some embodiments, filter 122a may perform both a sieving function (e.g., to remove particulates) and an ion exchange function (e.g., to remove charged particles and / or metal ions). In some embodiments, the average pore size of the filtration medium in filter 122a may be smaller than the average pore size of the filtration medium in filter 116a. In such embodiments, filter 122a may be used to remove particles smaller than those removed by filter 116a.

[0064] Examples of suitable materials that can be used in filter 122a include polypropylene (e.g., high density polypropylene), polyethylene (e.g., high density polyethylene or ultra-high molecular weight polyethylene), nylon (e.g., nylon 6 or nylon 66), polytetrafluoroethylene, or perfluoroalkoxyalkane polymers. In some embodiments, filter 122a, as well as filters 112a, 114a, and 116a described above, can be made from non-fluoropolymers.

[0065] In some embodiments, the filters 122a (e.g., ion absorption filters) may have the same characteristics (e.g., the same pore size) except that they are made from different materials. For example, in some embodiments, if one filter 122a is made from ultra-high molecular weight polyethylene, another filter 122a may be made from a fluoropolymer (e.g., PTFE). Without wishing to be bound by theory, it is believed that using a combination of filters 122a whose filtration media are made from different materials can maximize the reduction of impurities, particles, and metal ions to obtain ultra-high purity organic solvents.

[0066] In some embodiments, at least some (e.g., all) of the filters 122a may be arranged in parallel within the filter unit 122, and the remaining filters 122a (if any) within the filter unit 122 may be arranged in series. In some embodiments, the number of filters 122a (e.g., arranged in parallel) within the filter unit 122 may be greater than the number of filters 116a within the filter unit 116. For example, if the filter unit 116 includes three filters 116a, the filter unit 122 may have four or more (e.g., six) filters 122a arranged in parallel. Without wishing to be bound by theory, it is believed that an advantage of having more filters arranged in parallel within the filter unit 122 than within the filter unit 116 is that the system 10 may provide increased flow rates and have improved productivity. Without wishing to be bound by theory, it is believed that if the average pore size of the filtration medium in filter 122a is smaller than the average pore size of the filtration medium in filter 116a, the flow rate of the organic solvent through filter 112a may be reduced compared to the flow rate of the organic solvent through filter 116a. Therefore, it is believed that arranging multiple filters 122a in parallel may increase the flow rate and productivity of system 10.

[0067] In some embodiments, the filter unit 122 may include six filters 122a arranged in parallel and having an average pore size of about 3 nm and made from ultra-high molecular weight polyethylene.

[0068] 1 , the second filtration system 120 includes an optional recirculation conduit 160 f for recirculating the partially purified organic solvent to the storage tank 130 to form a recirculation loop for reprocessing by the filter unit 122 in the second filtration system 120. In some embodiments, the partially purified organic solvent is recirculated at least two times (e.g., at least three times, at least four times, or at least five times) before the purification process is completed and the organic solvent is transferred to the packaging station 140. In some embodiments, without wishing to be bound by theory, it is believed that recirculating the partially purified solvent more than two times within the second filtration system 120 may not achieve further improvement in impurity removal. In the example shown in FIG. 1 , the recirculation conduit 160 f is configured downstream of the outlet port 120 b of the second filtration system 120. In other examples, the recirculation conduit 160 f may be configured upstream of the outlet port 120 b.

[0069] In some embodiments, second filtration system 120 may include one or more optional temperature control units 180 (e.g., heat exchangers) in any suitable location. For example, temperature control unit 180 may be configured along recirculation conduit 160f. In some embodiments, temperature control unit 180 may be configured between inlet port 120a and filter unit 122, and between filter unit 122 and outlet port 120b. In some embodiments, temperature control unit 180 may be configured for a temperature of about 80°F or less (e.g., about 75°F or less, about 70°F or less, or about 65°F or less) and / or about 30°F or more (e.g., about 40°F or more, about 50°F or more, or about 60°F or more), thereby maintaining the temperature of the organic solvent in second filtration system 120 at about 80°F or less.

[0070] In some embodiments, packaging station 140 may be a mobile storage tank (e.g., a tank on a tanker) or a fixed storage tank. In some embodiments, packaging station 140 may be a fluoropolymer-lined device (e.g., the interior surface may include a fluoropolymer such as PTFE).

[0071] The present disclosure also features methods for purifying a solvent (e.g., an organic solvent). Generally, the purification method can include passing the solvent through two or more (e.g., three or four) filter units in first and second filtration systems 110 and 120. For example, referring to FIG. 1 , the raw or unprocessed solvent (i.e., starting material) can be purified by purification system 10 by passing the solvent from supply unit 20 through filter unit 112, optional filter unit 114, and filter unit 116 in first filtration system 110 to collect it in storage tank 130, and passing the solvent from storage tank 130 through filter unit 122 in second filtration system 120 to packaging station 140 (e.g., having a capacity of about 100-1000 liters). In some embodiments, the purification methods described herein may include recirculating the solvent at least once (e.g., two or three times) through a recirculation loop in the second filtration system 120 (e.g., via the storage tank 130, the filter unit 122, and the recirculation conduit 116h) before transferring the purified solvent to the packaging station 140. In some embodiments, the purification methods described herein may include recirculating the solvent at least once (e.g., two or three times) through a recirculation loop in the first filtration system 110 (e.g., via the filter units 112, 114, and 116 and the recirculation conduit 160h) before transferring the partially purified solvent to the storage tank 130.

[0072] In some embodiments, the crude or pre-processed solvent may comprise an organic solvent containing a metal element selected from the group consisting of sodium (Na), potassium (K), aluminum (Al), calcium (Ca), copper (Cu), iron (Fe), chromium (Cr), nickel (Ni), and lead (Pb). In some embodiments, the content of each metal component in the pre-processed solvent is in the range of about 0.1 to 1000 ppt by weight (e.g., 200 to 1000 ppt by weight or 500 to 1000 ppt by weight).

[0073] 1, when the raw solvent reaches a temperature control unit (e.g., unit 100, or a subsequent temperature control unit such as units 170 and 180), the temperature of the solvent can be adjusted to a predetermined optimal temperature range (e.g., 30°F to 80°F, 30°F to 70°F, 41°F to 67°F, or 50°F to 65°F). For example, the solvent temperature can be adjusted to 70°F, 68.5°F, or 67.5°F. Generally, the temperature control unit can maintain or adjust the temperature of the solvent at a specific location within purification system 10 (e.g., before entering a filter) or throughout purification system 10.

[0074] At the end of processing by the first and second filtration systems 110 and 120, if the number of particles and the amount of impurities detected in the purified solvent are controlled within a predetermined range, an ultra-high purity solvent (e.g., containing 0.1 to 100 parts per trillion by mass of metal components, such as those selected from the group of metal elements consisting of iron (Fe), chromium (Cr), nickel (Ni), and lead (Pb)) is produced. The ultra-high purity solvent can then be transferred to either the packaging station 140 or a manufacturing process for producing semiconductor products.

[0075] In some embodiments, solvents purified by the methods and systems described herein may have a purity of about 99.5% or greater (e.g., about 99.9% or greater, about 99.95% or greater, about 99.99% or greater, about 99.995% or greater, or about 99.999% or greater). In some embodiments, solvents purified by the methods and systems described herein may form a film or coating on an entire wafer (e.g., a 12-inch wafer) that has an on-wafer particle count of about 500 or less (e.g., about 450 or less, about 400 or less, about 350 or less, about 300 or less, about 250 or less, about 200 or less, about 150 or less, about 100 or less, about 50 or less, or about 25 or less) or zero. In some embodiments, solvents purified by the methods and systems described herein may form films or coatings on an entire wafer (e.g., a 12-inch wafer) having an on-wafer metal count of about 100 or less (e.g., about 90 or less, about 80 or less, about 70 or less, about 60 or less, about 50 or less, about 40 or less, about 30 or less, about 20 or less, or about 10 or less) or 0 (e.g., either the total on-wafer metal count or the on-wafer metal count of a specific metal, such as Fe or Ni). In some embodiments, solvents purified by the methods and systems described herein may form films or coatings having a defect density (i.e., based on the total number of metals and particles on the wafer) of about 1.5 or less (e.g., about 1.4 or less, about 1.2 or less, about 1 or less, about 0.8 or less, about 0.6 or less, about 0.5 or less, about 0.4 or less, about 0.2 or less, about 0.1 or less, about 0.07 or less, about 0.05 or less, about 0.03 or less, about 0.02 or less, about 0.01 or less, about 0.007 or less, about 0.005 or less, about 0.004 or less, about 0.003 or less) or zero per square centimeter on an entire wafer (e.g., a 12-inch wafer).

[0076] In some embodiments, solvents can be purified by the methods and systems described herein at relatively high flow rates (e.g., through the first filtration system 110 or the second filtration system 120) of about 25 L / min or more (e.g., about 30 L / min or more, about 40 L / min or more, about 50 L / min or more, about 60 L / min or more, about 80 L / min or more, about 100 L / min or more, or about 120 L / min or more) and / or about 170 L / min or less (e.g., about 160 L / min or less, about 150 L / min or less, about 140 L / min or less, about 130 L / min or less, about 120 L / min or less, about 110 L / min or less, or about 100 L / min or less). In general, the flow rate of the purifying solvent can vary depending on many factors, including the nature and viscosity of the solvent being purified, the temperature, the number of filters (e.g., arranged in parallel), and the type and number of other equipment used in the purification process. Without wishing to be bound by theory, it is believed that the flow rate of the solvent being purified should not be too high to minimize defects on the wafer and to minimize static charge buildup on the interior surfaces of conduits or vessels (which can erode the conduits or vessels).

[0077] The present disclosure is illustrated in more detail with reference to the following examples, which are for illustrative purposes and should not be construed as limiting the scope of the disclosure. [Example]

[0078] Overview of OWPC and OWMC Measurements

[0079] A solvent sample was collected and inserted into a wafer coating tool. After the bare wafer was coated with the sample, the wafer was transferred to a laser-based inspection system and inspected. Using laser light, the laser-based inspection system detected, counted, and recorded the location and size of each particle on the wafer with a detection limit of 19 nm. More specifically, the count included particles 19 nm or larger in size. This data was used to create a wafer map and provide a total particle count (OWPC).

[0080] The wafer was then transferred and inspected by EDX (Energy Dispersive X-ray). Each particle reported by the laser-based inspection system was inspected by EDX (Energy Dispersive X-ray) to provide elemental information. Particles that were found to produce a metal signal were counted as metal particles. The total number of particles with a metal signal was summed and reported as OWMP (On Wafer Metal Particles).

[0081] Total and Trace Metals Measurement Overview

[0082] The total trace metal concentration of each solvent sample was tested using inductively coupled plasma mass spectrometry (ICP-MS). Using a method developed by Fujifilm, each sample was tested for the presence of 26 metal species. Detection limits were metal-specific, but typical detection limits ranged from 0.00010 to 0.030 ppb. The concentrations of each metal species were then summed to calculate a value expressed as total trace metals (ppb).

[0083] Example 1

[0084] n-Butyl acetate was the solvent purified in this example. Referring to FIG. 1 , n-butyl acetate was purified using a purification system including a supply unit 20, a first filtration system 110, a storage tank 130, and a second filtration system 120. The first filtration system 110 included filter unit 112, filter unit 114, and filter unit 116. Filter unit 112 included one filter 112a, which was a 200 nm polypropylene filter. Filter unit 114 included three ion exchange filters 114a arranged in parallel and made from ultra-high molecular weight polyethylene (UPE). Filter unit 116 included three filters 116a arranged in parallel and made from 50 nm PTFE filters. The second filtration system 120 included filter unit 122, which included six filters 122a arranged in parallel and made from UPE. A temperature control unit was not used. Recirculation conduit 160f was used, but recirculation conduit 160h was not.

[0085] The test results are summarized in Table 1 below.

[0086] [Table 1]

[0087] As shown in Table 1, the amounts of trace metals, particles, and nonvolatile organic residues in the feedstock (before purification) were all significantly reduced by using the above purification system.

[0088] Although the invention has been described in detail with reference to specific embodiments thereof, it will be understood that modifications and variations are encompassed within the spirit and scope of what is described and claimed. The present disclosure includes the following embodiments. <1> 1. A method for purifying an organic solvent, comprising: passing the organic solvent through a first filter unit and a second filter unit downstream of the first filter unit to obtain a purified organic solvent, the first filter unit includes a first housing and at least one first filter within the first housing, the first filter including a filtration medium having a first average pore size; the second filter unit includes a second housing and at least two second filters within the second housing, the at least two second filters being arranged in parallel within the second housing, each of the second filters independently including a filtration medium having a second average pore size; the number of the first filters in the first filter unit is less than the number of the second filters in the second filter unit, and the first average pore size is greater than the second average pore size; method. <2> the first filter unit includes one first filter; <1> The method described below. <3> the filtration media in the first filter comprises polypropylene, high density polyethylene, ultra-high molecular weight polyethylene, nylon, polytetrafluoroethylene, or a perfluoroalkoxyalkane polymer; <1> The method described below. <4> The first average pore size is about 50 nm to about 200 nm. <1> The method described below. <5> the second filter unit includes two or three second filters; <1> The method described below. <6> the filtration media in the second filter comprises polypropylene, high density polyethylene, ultra-high molecular weight polyethylene, nylon, polytetrafluoroethylene, or a perfluoroalkoxyalkane polymer; <1> The method described below. <7> The second average pore size is about 10 nm to about 50 nm. <1> The method described below. <8> further comprising passing the organic solvent through a third filter unit disposed between the first filter unit and the second filter unit; the third filter unit includes a third housing and at least one third filter within the third housing, the third filter including a filtration medium having a third average pore size, and the filtration medium within the third filter including an ion exchange membrane; The aforementioned <1> The method described below. <9> The third filter unit includes one to three third filters. <8> The method described below. <10> the ion exchange membrane in the third filter comprises polypropylene, high density polyethylene, ultra-high molecular weight polyethylene, nylon, polytetrafluoroethylene, or a perfluoroalkoxyalkane polymer; <8> The method described below. <11> and further comprising sending the organic solvent exiting the second filter unit to a storage tank. <1> The method described below. <12> transferring the organic solvent from the storage tank to the first filter unit and passing the organic solvent through the first filter unit and the second filter unit, thereby recirculating the organic solvent. <11> The method described below. <13> further comprising passing the organic solvent through a fourth filter unit disposed downstream of the second filter unit; The fourth filter unit includes a fourth housing and at least two fourth filters within the fourth housing, the at least two fourth filters being arranged in parallel within the fourth housing, and each of the fourth filters independently comprising a filtration medium having a fourth average pore size. The aforementioned <1> The method described below. <14> the number of the second filters in the second filter unit is less than the number of the fourth filters in the fourth filter unit; <13> The method described below. <15> The fourth filter unit includes 4 to 14 fourth filters. <13> The method described below. <16> the fourth average pore size is smaller than the second average pore size; <13> The method described below. <17> the fourth average pore size is about 10 nm or less, <13> The method described below. <18> the filtration media in the fourth filter comprises polypropylene, high density polyethylene, ultra-high molecular weight polyethylene, nylon, polytetrafluoroethylene, or a perfluoroalkoxyalkane polymer; <13> The method described below. <19> transferring the organic solvent exiting the fourth filter unit to a storage tank and subsequently passing the organic solvent through the fourth filter unit, thereby recirculating the organic solvent. <13> The method described below. <20> and transferring the purified solvent to a packaging station located downstream of the fourth filter unit. <13> The method described below. <21> The organic solvent comprises cyclohexanone, ethyl lactate, n-butyl acetate, propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, 4-methyl-2-pentanol, or propylene carbonate. <1> The method described below. <22> The organic solvent is passed through at a flow rate of about 25 L / min to about 170 L / min. <1> The method described below. <23> a first filter unit including a first housing and at least one first filter within the first housing, the first filter including a filtration medium having a first average pore size; a second filter unit downstream of and in fluid communication with the first filter unit, the second filter unit including a second housing and at least two second filters within the second housing, the at least two second filters being arranged in parallel within the second housing, each second filter independently comprising a filtration medium having a second average pore size; A system comprising: the number of the first filters in the first filter unit is less than the number of the second filters in the second filter unit, and the first average pore size is greater than the second average pore size; system.

Claims

1. 1. A method for purifying an organic solvent, comprising: passing an organic solvent through a first filter unit, a second filter unit, a third filter unit, and a fourth filter unit to obtain a purified organic solvent, wherein the second filter unit is downstream of the first filter unit, the third filter unit is disposed between the first filter unit and the second filter unit, and the fourth filter unit is downstream of the second filter unit, the first filter unit includes a first housing and at least one first filter within the first housing, the first filter including a filtration medium having a first average pore size; the second filter unit includes a second housing and at least two second filters within the second housing, the at least two second filters being arranged in parallel within the second housing, each of the second filters independently including a filtration medium having a second average pore size; the third filter unit includes a third housing and at least one third filter within the third housing, the at least one third filter including a filtration medium having a third average pore size, and the filtration medium within the at least one third filter including an ion exchange membrane; the fourth filter unit includes a fourth housing and at least two fourth filters within the fourth housing, the at least two fourth filters being arranged in parallel within the fourth housing, each of the fourth filters independently including a filtration medium having a fourth average pore size; the number of the first filters in the first filter unit is less than the number of the second filters in the second filter unit, the first average pore size is greater than the second average pore size, the number of the first filters in the first filter unit is less than the number of the third filters in the third filter unit, the number of the second filters in the second filter unit is less than the number of the fourth filters in the fourth filter unit, and the fourth average pore size is less than the second average pore size; method.

2. The method of claim 1 , wherein the first filter unit comprises one first filter.

3. 10. The method of claim 1, wherein the filtration media in the first filter comprises polypropylene, high density polyethylene, ultra-high molecular weight polyethylene, nylon, polytetrafluoroethylene, or a perfluoroalkoxyalkane polymer.

4. The method of claim 1, wherein the first average pore size is from 50 nm to 200 nm.

5. 10. The method of claim 1, wherein the second filter unit comprises two or three second filters.

6. 10. The method of claim 1, wherein the filtration media in the second filter comprises polypropylene, high density polyethylene, ultra-high molecular weight polyethylene, nylon, polytetrafluoroethylene, or a perfluoroalkoxyalkane polymer.

7. The method of claim 1, wherein the second average pore size is from 10 nm to 50 nm.

8. 10. The method of claim 1, wherein the third filter unit comprises two or three third filters.

9. 10. The method of claim 1, wherein the ion exchange membrane in the third filter comprises polypropylene, high density polyethylene, ultra-high molecular weight polyethylene, nylon, polytetrafluoroethylene, or a perfluoroalkoxyalkane polymer.

10. 10. The method of claim 1, further comprising sending the organic solvent exiting the second filter unit to a storage tank.

11. 11. The method of claim 10, further comprising recirculating the organic solvent by transferring the organic solvent from the storage tank to the first filter unit and passing the organic solvent through the first filter unit and the second filter unit.

12. 10. The method of claim 1, wherein the fourth filter unit comprises 4 to 14 fourth filters.

13. The method of claim 1 , wherein the fourth average pore size is 10 nm or less.

14. 10. The method of claim 1, wherein the filtration media in the fourth filter comprises polypropylene, high density polyethylene, ultra-high molecular weight polyethylene, nylon, polytetrafluoroethylene, or a perfluoroalkoxyalkane polymer.

15. 10. The method of claim 1, further comprising recirculating the organic solvent by transferring the organic solvent exiting the fourth filter unit to a storage tank and subsequently passing the organic solvent through the fourth filter unit.

16. 10. The method of claim 1, further comprising transferring the purified solvent to a packaging station located downstream of the fourth filter unit.

17. 10. The method of claim 1, wherein the organic solvent comprises cyclohexanone, ethyl lactate, n-butyl acetate, propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, 4-methyl-2-pentanol, or propylene carbonate.

18. 2. The method of claim 1, wherein the passing of the organic solvent is carried out at a flow rate of 25 L / min to 170 L / min.

19. a first filter unit including a first housing and at least one first filter within the first housing, the first filter including a filtration medium having a first average pore size; a second filter unit downstream of and in fluid communication with the first filter unit, the second filter unit including a second housing and at least two second filters within the second housing, the at least two second filters being arranged in parallel within the second housing, each second filter independently comprising a filtration medium having a second average pore size; a third filter unit disposed between the first filter unit and the second filter unit, the third filter unit including a third housing and at least one third filter within the third housing, the at least one third filter including a filtration medium having a third average pore size, and the filtration medium within the at least one third filter including an ion exchange membrane; a fourth filter unit downstream of the second filter unit, the fourth filter unit including a fourth housing and at least two fourth filters within the fourth housing, the at least two fourth filters being arranged in parallel within the fourth housing, each fourth filter independently including a filtration medium having a fourth average pore size; A system comprising: the number of the first filters in the first filter unit is less than the number of the second filters in the second filter unit, the first average pore size is greater than the second average pore size, the number of the first filters in the first filter unit is less than the number of the third filters in the third filter unit, the number of the second filters in the second filter unit is less than the number of the fourth filters in the fourth filter unit, and the fourth average pore size is less than the second average pore size; system.

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