Chemical liquid manufacturing equipment

Abstract

To provide a chemical liquid manufacturing apparatus for preparing chemical liquid for semiconductor manufacture.SOLUTION: A chemical liquid manufacturing apparatus, including a first system and a second system, is provided. 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, where the first system is configured to process a material at least once. 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, where the second system is configured for recirculation and to process the material at least twice. A route forming the first system and a route forming the second system are present independently of each other.SELECTED DRAWING: Figure 1

Description

Technical Field

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

[0002] This disclosure relates to a chemical liquid manufacturing apparatus and a method for manufacturing a chemical liquid using the same.

Background Art

[0003] The semiconductor industry is rapidly improving the integration density of electronic components, which is due to the continuous reduction of component size. Ultimately, many smaller components will be integrated into a specific area. These improvements are mainly due to the development of new precision and high-resolution processing technologies.

[0004] In the manufacture of high-resolution integrated circuits, various processing liquids come into contact with bare wafers or wafers coated with a film coating. For example, the manufacture of fine metal interconnects typically involves a procedure of coating a substrate with a prewetting liquid before the substrate is coated with a composite liquid to form a resist film. These processing liquids containing appropriate components and various additives are known to be sources of contamination for IC wafers.

[0005] It is presumed that even if trace amounts of contaminants are mixed into these chemical liquids, such as the prewetting liquid or developing solution for wafers, defects may occur in the circuit pattern. The presence of a very low level of metal impurities at 1.0 ppt is known to interfere with the performance and stability of semiconductor devices. <000​​​​Furthermore, depending on the type of metal contaminant, the oxidation properties may deteriorate, and The formation of precise patterns degrades the electrical performance of the semiconductor circuit, ultimately affecting the manufacturing yield. It has a negative impact.

[0006] Contamination by impurities such as metallic impurities, coarse particles, organic impurities, and moisture can affect various aspects of chemical liquid production. During the process, impurities may be inadvertently introduced into the chemical liquid. For example, impurities in the raw materials If present, containers, equipment, or reaction containers used for transporting, storing, or reacting raw materials or chemical liquids. The container, the by-products generated during the manufacture of chemical liquids, or the unreacted residues of the reaction There is a match.

[0007] Therefore, in order to form high-precision, ultra-fine semiconductor electronic circuits, pre-wetting liquid, Semiconductor processing solutions such as resist solutions, developer solutions, stripping solutions, rinsing solutions, and coating solutions. The chemical liquids used in various stages of the process require significant quality improvements, and as a result... In order to prevent defects from occurring in the circuit patterns, strict quality control must be maintained. No. [Overview of the project] [Problems that the invention aims to solve]

[0008] Therefore, in order to form high-precision integrated circuits, there is a requirement for ultra-high-purity chemical liquids, and Improving and controlling the quality of these liquids is extremely important. Specific important parameters include reducing trace metals, reducing the number of liquid particles, and on the wafer (on- This includes reducing defects in wafers, reducing organic contaminants, etc. Everything depends on the purification medium, medium preparation, filter sequence, filter contact time, structural materials, and the physicochemical properties of the purification medium. It has been shown that this is affected by the settings of the processing unit and processing parameters, including those mentioned above. [Means for solving the problem]

[0009] In consideration of the foregoing, this disclosure relates to a chemical liquid manufacturing apparatus for preparing chemical liquids, particularly for semiconductor manufacturing. This provides high-purity chemical liquids, which are controlled within a predetermined range. It is generated by the number of unwanted fine particles and the amount of metallic impurities. Therefore, residue and / or particle defects This suppresses the occurrence of defects and improves the yield of semiconductor wafers.

[0010] According to some embodiments of this disclosure, the chemical liquid manufacturing apparatus is at least a first system The system includes a first system and a second system, each of which is configured to process a material. The first system consists of a first filter, a first ion exchange membrane, and a first ion adsorption membrane. It includes at least one first filter medium selected from, and the at least one first filter medium is The second purification system is configured to process the material at least once, and the second purification system is configured to process the material at least twice. At least one selected from filters, second ion exchange membranes, and second ion adsorption membranes The system includes two filtration media, with at least one second filtration medium being recirculated, and the material being filtered at least twice. It is configured to process.

[0011] According to a particular exemplary embodiment, the first system is a single-pass (single p Configured for use ass)

[0012] According to alternative embodiments of the present disclosure, the chemical liquid manufacturing apparatus for processing materials includes at least one 1 system and a second system are included. The first system includes at least one first filter, at least one first filtration medium selected from a first ion exchange membrane and a first ion adsorption membrane and is configured to process a material at least once. The second system includes at least one second filter, a second ion exchange membrane, and at least one second filtration medium selected from a second ion adsorption membrane and is configured for recirculation and to process a material at least twice.

[0013] According to a specific exemplary embodiment, there are two or more first filters, and the two or more first filters preferably have different characteristics. According to a further specific 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 the first system and the 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 are different 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 are different in function, pore size or material . The first system is configured to process a material at least once, and the second system is for recirculation and is configured to process a material at least twice. [[Effect of the Invention]]

[0015] According to the present disclosure, a chemical having a multifunctional purification medium that combines adsorption, filtration, ion exchange, etc. Chemical liquid manufacturing equipment is used for preparing aqueous and high-purity chemical liquids applied in semiconductor manufacturing. It is used to effectively remove a wide range of organic and inorganic contaminants from solvent-based solutions. ru. [Brief explanation of the drawing]

[0016] The aspects of this disclosure will be best understood from the following detailed description, which will be read together with the accompanying drawings. It should be noted that, in accordance with standard industry practices, various features are depicted to scale. It is not. In fact, the dimensions of various features have been arbitrarily enlarged or modified to clarify the description. It may be scaled down.

[0017] [Figure 1] This is a schematic diagram showing the configuration of an exemplary chemical liquid manufacturing apparatus according to some embodiments of the present disclosure. [Figure 2] This is a schematic diagram showing the configuration of an exemplary chemical liquid manufacturing apparatus according to some embodiments of the present disclosure. [Modes for carrying out the invention]

[0018] The following disclosure provides different embodiments or examples for implementing various features of the subject matter. To simplify this disclosure, specific examples of components and arrangements are described below. These are This is merely an example and not intended to be limiting. For example, if the term "solvent" is used... Unless otherwise specified, it refers to a single solvent or a combination of two or more solvents. It is possible.

[0019] Furthermore, "beneath", "below", "lower", Spatially relative terms such as "above" and "upper" are used here. , for the convenience of explaining the relationship between features of one element or other elements, or the features that are illustrated. It is used for the purpose of. Spatially relative terms are used in the orientation shown in the diagram, as well as in use. It is intended to include different orientations of the device in operation. The device is distributed in other ways. It may be oriented (rotated by 90 degrees or other orientations), and the spatially relative description used here The child can be interpreted accordingly.

[0020] In this disclosure, the numerical range indicated by the term "~" is the same as the term "~". This refers to a range that includes the numbers listed before and after it as the lower and upper limits, respectively.

[0021] In this disclosure, "ppm" means "one part per million (10) ‐6 ) means "ppb" 1 in 1 billion (10 ‐9 ) means "ppt" means "1 in a trillion (10 ‐12 )" It tastes good.

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

[0023] <Items to be processed> Before being subjected to the purification process, the chemical liquid is treated to remove undesirable amounts of impurities and contaminants. It may contain. In this disclosure, the pre-purified chemical liquid is referred to as "processed". The term "target" or "material to be processed" is used. ...to remove a considerable amount of contaminants and impurities from the material to be treated, and to reduce impurities and contaminants to a predetermined range. It controls and restricts the generation of chemical liquids.

[0024] <Chemical liquid> In this disclosure, the chemical liquid comprises an organic solvent and a predetermined amount of impurities. Used in semiconductor manufacturing as a wetting solution, developing solution, rinsing solution, cleaning solution, stripping solution, etc. The treatment solution may include raw materials used in the synthesis of the treatment solution.

[0025] <organic solvents> In this disclosure, chemical liquids include organic solvents. The type of organic solvent is not particularly limited and includes known organic solvents. Organic solvents can be used. The content of organic solvents in the chemical liquid is not particularly limited, It mainly contains organic solvents. Specifically, the amount of organic solvent is equal to the total mass of the chemical liquid. It is 98% by mass or more relative to. In certain embodiments, the content of the organic solvent is the same as that of the chemical liquid. It is 99% by mass or more of the total mass. In other embodiments, the content of the organic solvent is a chemical solution The amount is 99.5% by mass or more of the total mass of the body. In other embodiments, the amount of organic solvent is also included. The amount is 99.8% by mass or more of the total mass of the chemical liquid. There is no particular upper limit. However, the upper limit is usually 99.99% by mass or less.

[0026] Organic solvents may be used individually or in combination of two or more. When using organic solvents in combination, it is preferable that their total content be within the above range.

[0027] The content of organic solvents in a chemical liquid is determined using a gas chromatography-mass spectrometry (GCMS) instrument. It can be measured.

[0028] The boiling point of the organic solvent is not particularly limited. However, considering the improvement of semiconductor chip manufacturing yield... From this perspective, it is preferable that the boiling point of the organic solvent is less than 200°C. In this disclosure, the boiling point This refers to the boiling point at 1 atmosphere.

[0029] The organic solvent is not particularly limited. Examples of organic solvents include methanol, ethanol, and 1-p Ropanol, isopropanol, n-propanol, 2-methyl-1-propanol, n -Butanol, 2-Butanol, tert-Butanol, 1-Pentanol, 2-Penta Nol, 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 Xanol, 5-methyl-1-hexanol, 5-methyl-2-hexanol, 2-ethyl Ru-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 Butyl ether, butyl methyl ether, butyl ethyl ether, butylpropyl ether , dibutyl ether, diisobutyl ether, tert-butylmethyl ether, tert-butylmethyl ether, tert rt-butylethyl ether, tert-butylpropyl ether, di-tert-butyl Lu ether, dipentyl ether, diisoamyl ether, cyclopentyl methyl ether , cyclohexyl methyl ether, bromomethyl methyl ether, α,α-dichloromethyl Chloromethyl ether, chloromethyl ethyl ether, 2-chloroethyl methyl ether, 2-bromoethylmethyl ether, 2,2-dichloroethylmethyl ether, 2-chloro Ethyl ethyl ether, 2-bromoethyl ethyl ether, (±)-1,2-dichloroethyl ether ethyl ether, 2,2,2-trifluoroethyl ether, ethyl vinyl ether butyl vinyl ether, allyl ethyl ether, allyl propyl ether, allyl buty Lu ether, diallyl ether, 2-methoxypropene, ethyl-1-propenyl ether Lu, cis-1-bromo-2-ethoxyethylene, 2-chloroethyl vinyl ether, ali Lu-1,1,2,2-tetrafluoroethyl ether, octane, isooctane, nonane Decane, methylcyclohexane, decalin, xylene, ethylbenzene, diethylbenzene Zene, cumene, sec-butylbenzene, cymene, dipentene, methyl pyruvate, pro Pyrene glycol monomethyl ether, propylene glycol monoethyl ether, pro Pyrene glycol monopropyl ether, propylene glycol monomethyl ether acetate Tate, ethyl lactate, methyl methoxypropionate, cyclopentanone, cyclohexano Butyl acetate, γ-butyrolactone, isoamyl acetate, chloroform, dichloromethane , 1,4-dioxane, hexyl alcohol, 2-heptanone, isoamyl acetate, and te Contains trahydrofuran.

[0030] In certain embodiments of this disclosure, the chemical liquid is a pre-wetting liquid. There are no particular restrictions on the type of pre-wetting solution. A specific example of a pre-wetting solution is cyclopene. Thanone (CyPe), cyclohexanone (CyH), propylene glycol monomethyl ester Propylene glycol monoethyl ether (PGME), propylene glycol monoethyl ether (PGEE), propylene Propylene glycol monomethyl ether acetate (PGMEA), propylene glycol mono It contains at least one of propyl ether (PGPE) and ethyl lactate (EL). Other implementations In terms of form, the chemical liquid is a developing solution such as butyl acetate, or 4-methyl-2-pentanol ( A rinse solution such as MIBC may also be used.

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

[0032] <Metallic impurities> The most common metal impurities are iron (Fe), aluminum (Al), chromium (Cr), Heavy metals such as nickel (Ni) and ions such as sodium (Na) and calcium (Ca) It contains metals. Depending on the type of metal, metal impurities can reduce the integrity of the oxide, The chemical liquid disclosed herein can degrade the MOS gate stack and shorten the lifespan of the device. In chemical liquids prepared by a body manufacturing device, the total trace metal content is 0-150p by mass. It is preferable that it be within a predetermined range called pt.

[0033] In this disclosure, metal impurities are in the form of a solid (elemental metal, particulate metal-containing compound, etc.) This refers to the metallic impurities provided.

[0034] In this disclosure, the total trace metals in the chemical liquid are defined as Fujifilm's method of development (Fujifilm Inductively coupled plasma mass spectrometry (ICP) using the m developed method Measured by -MS). OWMP (on-wafer metal particle) e) Laser-based inspection systems and EDX (energy dispersive Determined by inspecting the wafer using a combination of X-ray and ICP- Total trace metals using MS, on-wafer metal particles (OWMP) using laser and EDX The measurement method is as shown in the following example.

[0035] <particle> In this disclosure, objects to be counted having a size of 0.03 μm or larger are referred to as "particles." The number of "particles" in the body is counted using a light scattering type liquid particle counter, LPC(li This is called quid particle count.

[0036] Examples of particles include dust, dirt, organic solids, and inorganic solids. Particles are also It may contain impurities of colloidalized metal atoms. The type of metal atom is one that is easily colloidalized. Yes, without any particular limitations, Na, K, Ca, Fe, Cu, Mg, Mn, Li, Al, Cr, N It can contain at least one metal atom selected from the group consisting of i, Zn, and Pb. In the chemical liquid prepared by the chemical liquid manufacturing apparatus of this disclosure, saturates of 0.03 μm or larger The total content of ions particles must be within a specified range of 100 or less per 1 ml of chemical liquid. It is preferable.

[0037] <Organic impurities> Organic impurities refer to compounds different from the organic solvent, which is the main component of a chemical liquid. This refers to organic substances present in a concentration of 5000 ppm or less by mass relative to the total mass of a chemical liquid. It is considered an organic impurity and not an organic solvent.

[0038] Even inside a cleanroom, volatile organic compounds (VOCs) are present in the atmosphere. Some organic impurities The substances originate from shipping and storage equipment, and some are present in the raw materials from the beginning. Other organic impurities Examples include by-products and / or unreacted reactants generated during the synthesis of organic solvents. nothing.

[0039] The total content of organic impurities in the chemical liquid is not particularly limited. Manufacturing yield direction of semiconductor devices From the above perspective, the total content of organic impurities is 0.1 ppm relative to the total mass of the chemical liquid. ~5000 ppm by mass is preferred, 1 to 2000 ppm by mass is more preferred, and 1 to 100 0 ppm by mass is more preferred, 1 to 500 ppm by mass is particularly preferred, and 1 to 100 ppm by mass is preferred. PM is the most preferable option.

[0040] The content of organic impurities in a chemical liquid can be determined using a gas chromatography-mass spectrometry (GCMS) instrument. It can be measured.

[0041] <Moisture (water)> Moisture has the effect of destabilizing the chemical and physical state of semiconductor surfaces. It can originate from the surrounding air or residue from wet processes. Moisture is contained within the chemical liquid. It may be water that is inevitably included in the raw materials, or water that is inevitably included during the manufacture of chemical liquids. or water that is intentionally introduced.

[0042] The water content in a chemical liquid is not particularly limited. Generally, the water content is the total water content of the chemical liquid. It is preferable that the amount be 2.0% by mass or less, more preferably 1.0% by mass or less, and 0.5% by mass. A percentage of a certain amount is even more preferable. If the water content in the chemical liquid is 1.0% by mass or less, then the semiconductor The manufacturing yield of the chips will be further improved. There is no particular lower limit, but it should be around 0.01% by mass. It is often the case that the water content is below the above value. Due to manufacturing constraints, it is difficult to reduce the water content below the above value.

[0043] The water content is measured using an instrument that employs the Karl Fischer moisture metering method as its measurement principle. This refers to the amount of water that can be absorbed.

[0044] Hereinafter, embodiments of the present disclosure describe exemplary chemical liquid manufacturing apparatus and exemplary methods using the same. A method for producing chemical liquids is described. The chemical liquid production apparatus includes at least multiple material processing systems. Unwanted particulate matter (par) in chemical liquids containing Tem and prepared using a chemical liquid manufacturing apparatus. The number of particles and the amount of metallic impurities are predetermined. It is limited to the range. Therefore, the generation of residue and / or particle defects is suppressed, and semiconductor The yield of the wafers will be improved.

[0045] <Chemical liquid manufacturing equipment> Figure 1 shows an overview of the configuration of an exemplary chemical liquid manufacturing apparatus according to several embodiments of the present disclosure. This is a schematic diagram. As shown in Figure 1, the chemical liquid manufacturing apparatus 10 is connected to the processing target supply unit 20. The materials to be processed by the chemical liquid manufacturing apparatus 10, such as the object to be processed, are held or transported. The number of unwanted fine particles and the amount of metal impurities in the chemical liquid are controlled to stay within a predetermined range. The chemical liquid is produced. The processing target supply unit 20 is subjected to processing by the chemical liquid manufacturing apparatus 10. The processing target supply unit is not particularly limited as long as it supplies the material continuously or intermittently. 20 includes a material receiving tank, sensors such as a level gauge (not shown), and a pump (not shown). This may include valves, etc., for controlling the flow of the material to be processed (not shown). Figure 1 So, the chemical liquid manufacturing apparatus 10 is connected to one processing target supply unit 20. However, However, this disclosure is not limited in that way. In some exemplary embodiments, Multiple processing supply units for each type of material to be processed by the chemical liquid manufacturing apparatus 10 Knit 20 is provided in parallel.

[0046] The materials to be processed include, for example, pre-wetting solution, developing solution, rinsing solution, washing solution, and stripping solution. It may include raw materials used in the preparation of processing solutions applied to semiconductor manufacturing, such as synthesizers. In the following description, unless otherwise specified, the term “preparation” of specific materials is used in accordance with the foregoing disclosure. In most embodiments, the specific material or chemical liquid is, for example, used for the purification or reprocessing of the material to be processed. It is used to mean when the material to be processed is provided by the company or by mixing. You can synthesize it yourself, or you can use a commercially available product purchased from a supplier.

[0047] In certain embodiments of this disclosure, the material to be processed is used in the preparation of the pre-wetting solution. It is an unprocessed organic solvent. For example, the unprocessed organic solvent is processed by the chemical liquid manufacturing apparatus 10. It is processed to produce an ultra-high purity pre-wetting solution, such as high-purity grade cyclohexa Non (CyH), cyclopentanone (CyPe), ethyl lactate (EL), propylene glycol Polymethyl ether (PGME), propylene glycol monoethyl ether (P GEE), propylene glycol monomethyl ether acetate (PGMEA), propylene Lenglycol monopropyl ether (PGPE), etc., or combinations thereof, ru.

[0048] As shown in Figure 1, the chemical liquid manufacturing apparatus 10 optimizes the temperature of the material to be processed. A heat exchanger 100 for setting the processing range, and heat via the first transport conduit 160b The system includes a first material processing system 110 coupled to the exchanger 100, where the heat exchanger 1 00 is supplied directly to the processing target supply unit 20, or, for example, via the introduction conduit 160a. The first material processing system 110 is indirectly connected to one or more filtration media (reference numeral 110). The first transport conduit 160b includes the horizontal solid line shown in No. 114, and is connected to the heat exchanger 100, for example. For example, it is connected to the supply port 110a of the first material processing system 110.

[0049] In a particular exemplary embodiment, one or more filtration media 114 are each partitioned It may be converted and contained in one or more housings 112. For example, first material processing system 110 is the first housing 112a, the second housing 112b, and the third housing 112c It may include at least one housing 112 selected from, and at least one The housing 112 contains one or more filtration media 114 therein, To accommodate. In other words, according to the example above, the first material processing system 110 is one house Housing 112 (First housing 112a, second housing 112b, or third housing) Either of 112c, or two housings 112 (first housing 112a, second housing 112a, second housing 112a). Any combination of two of the wing 112b and the third housing 112c, or 3 The housings (first housing 112a, second housing 112b, and third housing) This may include (G112c). Note that the above example is for illustrative purposes only and does not include the number of housings. This is not limited to the illustrated examples. In other exemplary embodiments, the first material processing system 110 is: In addition to the first housing 112a, the second housing 112b, and the third housing 112c This includes more housings 112, for example, one, two, five, or ten or more. This is possible. Furthermore, there is no separate housing 112, and one or more filtration media 114 are 1. The material processing system 110 can also be configured without being partitioned. Further examples In this embodiment, the first material processing system 110, in addition to one or more filtration media 114, It may also include other material processing modules (not shown).

[0050] According to some embodiments of the present disclosure, the first material processing system 110 is a second transport conduit 1 The second transport conduit 160c may be connected to the collection tank 130 via 60c, for example Connected between the outflow port 110b of the first material processing system 110 and the collection tank 130. The pump and valves are installed as needed at the outlet port of the supply unit 20 to be processed and Various components such as supply ports, heat exchanger 100, first material processing system 110, collection tank 130, etc. It is understood that it will be installed in a conduit.

[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 directly connecting to a collection tank 130 or indirectly, for example, via a third transport conduit 160d; a fourth transport conduit 160e that connects the second material processing system 120 to a subsequent processing apparatus or packaging 140; a recirculation conduit 160f that branches off from the fourth transport conduit 160e and can be connected to the collection tank 130 for recirculating and supplying partially purified materials 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, where, 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 filtration media 124 and a fourth transport conduit 1 60 e may be connected to the outlet port 120b of the second material processing system 120. It is understood that the pump and valve may be installed in various conduits as needed, such as the outlet and supply ports of the second material processing system 120, the next processing unit or packaging 140, the sample detector 150, etc.

[0052] In certain exemplary embodiments of this disclosure, one or more filtration media 124 are each These are partitioned and may be contained within one or more housings 122. For example, second material processing System 120 includes the fourth housing 122a, the fifth housing 122b and the sixth housing It may include at least one housing 122 selected from g 122c, and less Each housing 122 contains one or more units of filtration medium 124. To accommodate. In other words, according to the example above, the second material processing system 120 is one, two , or it may include three housings 122. Note that the above example is for illustrative purposes only. Therefore, the number of housings is not limited to the illustrated example. In other exemplary embodiments, the second material The material processing system 120 includes a fourth housing 122a, a fifth housing 122b, and a sixth housing 122b. In addition to housing 122c, more housings 122, for example, one, two, five , or may include 10 or more. Furthermore, there is no separate housing 122, and one or more filters The superfluid medium 124 can also be configured without being partitioned within the second material processing system 120. In yet another exemplary embodiment, the second material processing system 120 includes one or more filtration media. In addition to body 124, other material processing modules not shown may be included.

[0053] In some exemplary embodiments, the first material processing system 110 also partially purifies The processed material is recirculated to the first material processing system 110, and the first material processing system 1 It may also include a recirculation conduit 160h that is processed again by 10. In the example shown in Figure 1, The recirculation conduit 160h is located upstream of the outlet port 110b of the first material processing system 110. It branches off from the configured fifth transport conduit 160i, but the above example is for illustrative purposes only. Yes, and not intended to be limiting. In other examples, the recirculation conduit 160h is in the collection tank 1 As long as it is configured upstream of 30 and / or the second material processing system 120, the outflow port 110 b may be configured downstream. Furthermore, the recirculation conduit 160h is located upstream of the heat exchanger 100. Into the introduction conduit 160a, or downstream of the heat exchanger 100 to the first transport conduit 160b, or It may be connected to the supply port 110a of the material processing system 110.

[0054] Also, referring to Figure 1, according to some embodiments, the chemical liquid manufacturing apparatus 10 is a first material The processing system 110 is configured to be located upstream of the second material processing system 120. The material to be processed first passes through the first material processing system 110, or the first material processing system 1 10 is processed by the first, and then the second material processing system 120 follows. However, alternative In this embodiment, the chemical liquid manufacturing apparatus 10 uses the second material processing system 120 to perform the first material processing It is placed upstream of system 110, and the object to be processed is first the second material processing system 120 first It passes through or is processed by the second material processing system 120, and then the first material processing System 110 can also be configured to follow.

[0055] In a particular embodiment, the first material processing system 110 is configured for inline single-pass processing. More specifically, the chemical liquid manufacturing apparatus 10 processes the first material processing system 110 into the second material. When configured to be located upstream of the material processing system 120, the material to be processed is the first material processing It is processed by system 110, or it passes through the first material processing system 110 once, and then the second Before proceeding to the material processing system 120, it is discharged into the collection tank 130, or the collection tank 130 It bypasses and is transported directly to the second material processing system 120. Specific exemplary cases of this disclosure According to one embodiment, in the case of an inline single pass, the first material processing system 110 is First filter medium 114a, second filter medium 114b, third filter medium 114c, and their respective It includes one unit of filtration medium 114 selected from the combination of intents. In other words, single The first material processing system 110 configured for the inline process is a first unit Filtration medium 114a, one unit of second filtration medium 114b, or one unit of third filtration medium 114c is included, or one unit of first filter medium 114a and one unit of second filter Including medium 114b, or one unit of first filter medium 114a and one unit of third It includes a filter medium 114c, or one unit of a second filter medium 114b and one unit of a second filter medium 114b. 3. Includes filtration medium 114c, or 1 unit of first filtration medium 114a, 1 unit The filter media may include a second filter medium 114b and one unit of a third filter medium 114c. 1. Material processing system 110 before the material to be processed is delivered to the second material processing system 120. , first filter medium 114a, second filter medium 114b, third filter medium 114c, and their One unit of filtration medium 114, selected from any combination, passes through and is processed. It is configured in such a way.

[0056] However, this disclosure is not limited in that way. In alternative embodiments, the first The material processing system 110 can also be configured for recirculation of multiple passes. The number of times an elephant is processed in the first material processing system 110 depends on the number of times the object to be processed is processed in the second material processing system Processing in the first material processing system 110 is completed before the material is handed over to 120 or the next processing stage. If so, it is not limited. In some exemplary embodiments, the first material processing system 11 0 is configured to recycle and process the material two or more times. First material processing system If 110 is configured for recirculation, processing the material two or more times, for example twice, then the first material The processing system 110 includes a first filtration medium 114a, a second filtration medium 114b, and a third filtration medium 1 Includes two units of filtration medium 114, selected from 14c and any combination thereof. In other words, the first material processing system 110 has two units of the first filter medium Body 114a, 2 units of second filter medium 114b, or 2 units of third filter medium 114 c is included, or two units of the first filter medium 114a and two units of the second filter medium 1 14b is included, or two units of the first filter medium 114a and two units of the third filter medium The body 114c is included, or two units of the third filter medium 114c and two units of the second filter It contains the perfusate 114b, or two units of the first filter medium 114a and two units of the second filter medium The first material may include a filtration medium 114b and two units of a third filtration medium 114c. The material processing system 110 includes a first filtration medium 114a, a second filtration medium 114b, and a third filtration medium 114c and two units of the second filter medium 11 selected from any combination thereof The processing target is set so that it passes through 4b, and the first filtration medium 114a and the second filtration medium 114b , a third filtration medium 114c, and another unit selected from any combination thereof The material is recirculated so that it passes through the filtration medium 114, and then proceeds to the second material processing system 120 or the next The process proceeds to the processing stage. Furthermore, the recirculation operated by the first material processing system 110 is continuous. For example, by the CPU (central processing unit) It can be controlled by the first material treatment. However, in some alternative embodiments, the first material treatment The filtration system 110 uses the same unit of filtration media 114 (114a, 114b, 114c, It may be configured to recirculate through (or any combination thereof)

[0057] According to the embodiment of the chemical liquid manufacturing apparatus shown in Figure 1, the second material processing system 120 is multiple This applies to the second continuous cycle. However, it should be noted that the second material processing system The M120 also allows the material to be processed to pass through, or to the second material processing system 120. Therefore, it may be configured to process only once. The second material processing system 120 is recirculated. There is no particular limit to the number of times the mixture is circulated, depending on the initial level of impurities and contamination, and the required purity of the chemical liquid, etc. It may vary depending on the conditions of the material being processed. In certain embodiments of this disclosure, the second material processing system The M120 is configured to recirculate and process the target at least twice. The elephant is processed two or more times by the second material processing system 120, for example, 2, 3, 4 or 10 times. If so, the material to be processed is returned to the second material processing system 120 via the recirculation conduit 160f. Then, additional processing is performed. In some embodiments, the processed material is recirculated to the collection tank 130. The material to be processed is then delivered to the second material processing system 120. In some examples, The material to be processed is, for example, the second material through the outlet port 120b of the second material processing system 120. The material exits the processing system 120 and, via the recirculation conduit 160f, goes to the collection tank 130 or the second material. It can be directly recycled to the processing system 120. In other examples not shown, The target of processing is the recirculation conduit 1 upstream of the outflow port 120b of the second material processing system 120. It is recirculated directly to the collection tank 130 or the second material processing system 120 via 60f. That's good too.

[0058] Similar to the first material processing system 110, the second material processing system 120 processes the material to be processed once. In the above case, if configured to treat or process, The filtration medium 124 of the unit (for example, the fourth filtration medium 124a, the fifth filtration medium 124b, A sixth filtration medium 124c, and a new unit of filtration medium selected from combinations thereof. Body 124) can be used in each pass. For example, the material to be processed can be used in the second material processing 120. When the material is recycled two or more times, the second material processing system 120 has two or more filter units. Filtration media 124 (fourth filtration media 124a, fifth filtration media 124b, sixth filtration media 124c, This includes (and any combination thereof). Also includes a fourth filtration medium 124a, a fifth filter Selected from the perfusate 124b, the sixth filtration medium 124c, and any combination thereof. Two or more filtration media 124 units are configured simultaneously within the second material processing system 120. Often, the processing target is controlled, for example, by the CPU, in order to achieve continuous recirculation. Each time, a new unit of filtration medium 124 (fourth filtration medium 124a, fifth filtration medium 124) is used. b) processed by a sixth filtration medium 124c, and any combination thereof. For example, 2, 3, or 4 units of filtration media 124 (4th filtration media 124a, 5th filtration) (Select from medium 124b, sixth filtration medium 124c, and any combination thereof) second material The processing system 120 is configured to simultaneously process two, three, or four consecutive items. Recirculation or processing is achieved. One point to note is the number of units of the above-mentioned filtration medium 124. (124a, 124b, 124c, or any combination thereof) and the number of recycles is These are merely examples and are not intended to be limiting. In some alternative embodiments, 1 or 2 The filtration medium 124 of the unit (124a, 124b, 124c, or any combination thereof) A combination of (1) and 1 or 2 units of the same filtration medium 124 (124a, 124b, 1) is provided. 24c (or any combination thereof) is used for multiple recirculations.

[0059] The second material processing system 120 processes the material processed by the second material processing system 120. At the end of each pass of the processing process, the sample detector 150 detects, for example, in-line particles. The system can also be configured to allow on-site testing of chemical liquid samples. In certain cases... The sample is collected and sent to the sample detector 150 via the sampling conduit 160g, there The number of unwanted fine particles remaining in the chemical liquid and the amount of metal impurities are explained below. The method used to measure the number of unwanted fine particles (parts) and the amount of metal impurities detected in the sample. However, if it is not within the desired range, the chemical liquid is recycled and processed by the second material processing system 12 It is processed again by 0. The number of particles and the amount of metal impurities in the chemical liquid are ensured to be within a predetermined range. Once the high-purity chemical liquid is produced, it is circulated or processed by the second material processing system 120. The process is terminated, and the chemical liquid is connected to the outlet port 120b of the second material processing system 120. The material is transported via the fourth transport conduit 160e to packaging or to the next processing stage 140.

[0060] According to some embodiments of this disclosure, the first material processing system 110 is a first housing Selected from housing 112a, second housing 112b, and third housing 112c Each can include one housing 112, and the selected housing(s) 112 Each contains one unit of filtration medium 114 (114a, 114b, 114c). To house or accommodate. More specifically, the first housing 112a is one or more units The first filtration medium 114a may be included, and the second housing 112b may be one or more units The second filtration medium 114b may be included, and the third housing 112c may contain one or more units The third filtration medium 114c of the nit can include, where the first, second and third filtration media 114a, 114b, and 114c differ in function or characteristics and offer different processing to the target object. It can be provided, but the selected housing 112 (112a, 112b, 112c) One or more filtration media units 114 (114a, 114b, 114c) corresponding to each of the above. ) each has the same or similar purification function, physicochemical properties, pore size and / or structural material, etc. It holds.

[0061] Furthermore, according to some embodiments of this disclosure, the second material processing system 120 is the fourth H A small number of housings selected from 122a, 5th housing 122b, and 6th housing 122c. It may include at least one housing 122, and the selected housing 122 Each contains one or more units of filtration medium 124 (124a, 124b, 124c ) includes or accommodates. More specifically, the fourth housing 122a contains one or more units The fourth filtration medium 124a may be included in the set, and the fifth housing 122b may be one or more The unit may include a fifth filtration medium 124b, and the sixth housing 122c may be 1 or It may include multiple units of the sixth filter medium 124c, where the fourth filter medium 124a The fifth filtration medium 124b and the sixth filtration medium 124c have different functions or characteristics, and are used for processing. Although different processing can be provided to the elephant, the selected housing 122 (122a, 1 1 or more units of filtration medium 124 (124a, 122c) corresponding to each of 22b, 122c) 124b, 124c) respectively have the same or similar purification function, physicochemical properties, pore size and It has / or structural materials, etc.

[0062] According to some exemplary embodiments of this disclosure, the first material processing system 110 together Through the interchangeable filter media 114 (114a, 114b, 114c) connected to the It is a multi-stage system configured to have a scalable material to be processed, and each stage is specific It has a purification function and provides specific processing. For example, the first material processing system 110 has a particle At least one filtration medium selected from a ion removal filter, an ion exchange membrane, and an ion adsorption membrane. This may include body 114 (114a, 114b, or 114c). Specific examples of this disclosure In a typical embodiment, there is at least one selected filter medium 114. The first material processing system 110 comprises, respectively, a first housing 112a and a second housing One particle removal filter housed in the third housing 112c, 1 It may include two ion exchange membranes and one ion adsorption membrane. In another example, the first material The processing system 110 comprises the second housing 112b and the third housing 112c, respectively. It includes two particle removal filters and two ion adsorption membranes housed within. It is possible to do so. In yet another example, the first material processing system 110 is the first how Ion exchange membrane of one unit housed in the 112a and second housing 112b And it may include an ion adsorption membrane of one unit. The examples are for illustrative purposes only and are not intended to be limiting.

[0063] Similarly, the second material processing system 120 includes a replaceable filtration medium 124 connected together. The material to be processed is configured to be cascaded via (124a, 124b, 124c). It is a multi-stage system, each with a specific purification function and providing a specific treatment, for example. For example, the second material processing system 120 uses a particle removal filter, an ion exchange membrane, and an adsorption membrane. This includes at least one selected filtration medium 124 (124a, 124b, 124c) This is possible. In certain embodiments of this disclosure, at least two selected filtration units A medium 124 exists. In some exemplary embodiments of this disclosure, there are three or more units, for example. For example, there are 3, 4, 5, or 10 selected filtration media 124. The second material processing system 120 is housed in the fourth filter housing 122a, and consists of three The particle removal filter and three ion exchangers housed in the fifth filter housing 122b It may include a film or three ion adsorption films. In another example, the second material processing system 1 20 is a fourth filter housing 122a containing two, three, or four particle removal filters The filter and two, three, or four additional particle removal devices housed in the fifth filter housing 122b Including the filter, here the particle removal filter in two housings 122a, 122b, They differ in terms of hole diameter and / or structural material, for example, two housings 122a, 122b Particle removal filters have pore sizes of 10 nm or less, but have completely different structural materials. Filters can be included. In some examples, two housings 122a and 122b The particle removal filters in each case are made of 3nm ultra-high molecular weight polyethylene (UPE) film. Luta and 1nm UPE filter, or 5nm MPTFE (modified p (Olytetrafluoroethylene) filter and 5nm nylon filter Includes. In some exemplary embodiments, the second material processing system 120 includes a filter housing. The Zing 122 currently houses two or more particle removal filters, continuous Enables recirculation or processing of items two or more times, and new unit particle removal fill The filter is used each time the system is recirculated. For example, two or more particle removal filters are used in the recirculation and 3 For the processing target of each processing, 3 units of 3nm UPE filters or 3 units of 5 It could be a nm nylon filter. Of course, the above example is for illustrative purposes only. It is not intended to be limiting.

[0064] It should be noted that the number of units of the filtration medium 114 shown and described is 124 and The numbers for housings 112 and 122 are representative and are not shown in the drawings or descriptions. The numbers are kept low for simplicity.

[0065] Furthermore, it should be noted that the filtration medium 114 (114a, 114b, 114c, or (combinations thereof) and filtration medium 124 (124a, 124b, 124c, or those) The number and arrangement order of combinations of the above filtration media 114 and 124, or the target of processing via the above filtration media 114 and 124. The flow order is not particularly limited and depends on the functionality of the filtration medium, the initial conditions of the material being processed, and This may vary depending on the purity requirements of the chemical liquid. In some exemplary embodiments of this disclosure, the material The material processing systems 110 and 120 are ion exchange filters located upstream of the ion adsorption membrane. It is configured to have a particle removal filter located upstream, through which the material to be processed passes, After being processed by the first particle removal filter, the material proceeds to an ion exchange membrane, and then to an ion adsorption membrane. However, in other exemplary embodiments, the filter medium 114 and the filter medium 124 are, respectively, In the processing systems 110 and 120, the processing is performed in a different order, and the target of processing is subjected to ion exchange. The membrane passes through the filtration media 114 and filtration media 124 in other orders, such as following the particle removal filter. To process or to have it processed. In some embodiments of this disclosure, the material processing system 110 is non More filtration with non-sieving properties The medium 114 may include, for example, more ion exchange membranes and / or ion absorption membranes. The material processing system 120 has pure sieving properties. Includes more filtration media 124 (e.g., coarser particle filters) having a certain perty. It is possible to see. Furthermore, the arrangement order of the filtration media 114 and filtration media 124 as exemplified above, or the processing target. The flow order is for illustrative purposes only and is not intended to be limiting.

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

[0067] In a particular exemplary embodiment, the first material processing system 110 includes a first filtration medium 11 4a, has the same function as the second filtration medium 114b or the third filtration medium 114c, but the first Filtration medium 114a, second filtration medium 114b, or third filtration medium 114c and pore size and / or The filtration media may differ in terms of structural materials, etc. Similarly, the second material processing system 1 20 is a fourth filter medium 124a, a fifth filter medium 124b, or a sixth filter medium 124c Although having similar functions, the fourth filtration medium 124a, the fifth filtration medium 124b, or the sixth filtration A filtration medium that differs from medium 124c in terms of pore size and / or structural material may be included. For example, as shown in Figure 2, the first housing 112a, the second housing 112b, the third housing In addition to the Zing 112c, the first material processing system 110 includes one or more units of the seventh filtration medium. It includes a seventh housing 112d corresponding to body 114d. The seventh filtration medium 114d removes particles This can be selected from defilters, ion exchange membranes, and ion adsorption membranes. Several examples So, the seventh filtration medium 114d is 0.2 PP (50 μm polyps) of the first filtration medium 114a. Particle removal filters (polypropylene film) and 3nm UP filters with different pore sizes and / or structural materials It can be an E particle removal filter. Note that the above example is just one example, and the 7th filtration medium 1 The type of 14d, and the pore size and material of the 7th filtration medium 114d are not limited to the illustrated examples. In addition to the 4th housing 122a, the 5th housing 122b, and the 6th housing 122c The second material processing system 120 then applies one or more units of the eighth filtration medium (not shown) to It may include an eighth housing (not shown) to accommodate the eighth filtration medium. These can be selected from particle removal filters, ion exchange membranes, and ion adsorption membranes. Note The above examples are for illustrative purposes only and are not intended to be limiting.

[0068] [Particle Removal Filter] The particle removal process uses a particle removal filter to remove particles and / or metal particles from the object being treated. This is a process for removing pure substances (solid metal impurities). Particle removal filters are particularly limited Alternatively, a known particle removal filter can be used.

[0069] The average pore size of the filter is not particularly limited, but is generally between 0.001 and 1.0 μm (1 nm). A suitable size is around 1000 nm, and approximately 0.01 to 0.5 μm (10 nm to 500 nm). This is preferable, and more preferably about 0.01 to 0.1 μm (10 nm to 100 nm). Within the specified range, it suppresses filter clogging while removing impurities and aggregates contained in the purified product. Foreign matter can be reliably removed. In certain embodiments of this disclosure, the first material processing system TEM110 is a particle removal filter with a small average pore size of about 2 nm (for example, 2 nm It can include a microfiltration membrane having a pore size of 0.002 μm (2 nm) or larger. It can be in the range of approximately 1.0 μm (1000 nm) or less. Gold such as iron and aluminum. In addition to colloidal impurities containing group atoms, if the object being processed contains fine particles, even finer particles may be required. To remove particles, filters with a small average pore size of 20 nm or 15 nm are used. Before the filtration to be performed is carried out, the material to be processed is filtered using a filter with an average pore size of approximately 50 nm. This process improves filtration efficiency and further enhances particle removal performance.

[0070] In some embodiments of this disclosure, a second filtration system (Second material processing system) 12 0) This may include a particle removal filter having a small pore size of about 0.001 μm (1 nm), and may be in the range of about 0.001 μm (1 nm) to about 0.015 μm (15 nm). In a particular embodiment, a second filtration system (Second material processing system) 120 ) This may include a UPE filter having a small pore size of about 3 nm. In yet another embodiment, a second filtration system (Second material processing system) 120 ) This may include nylon or MPTFE filters with a pore size of approximately 5 nm. Here, the average pore size can refer to the nominal value provided by the filter manufacturer.

[0071] Examples of filter materials used for particle removal include polytetrafluoroethylene (P Fluoropolymers such as TFE, polyamide resins such as nylon, polyethylene and polypropylene Polyolefin resins such as pyrene (PP) (including high-density and ultra-high molecular weight), purple Oroalkoxy (PFA) resin, etc., or modified polytetrafluoroethylene (MPTFE) This may include impurities and / or fine foreign matter such as aggregates contained in the chemical liquid. In terms of effective removal, the filter used for particle removal in this disclosure is made of nylon, poly Polypropylene (including high-density polypropylene), polyethylene, polytetrafluoroethylene Len, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, poly It consists of at least one selected from the group consisting of imides and polyamideimides. According to filters made of materials, highly polar alien particles can cause residual defects and / or particle defects. It can effectively remove substances and effectively reduce the content of metal components in chemical liquids. can.

[0072] Polyimides and / or polyamideimides contain carboxyl groups, salt-type carboxyl groups, and - It may have at least one selected from the group consisting of NH-bonds. Therefore, fluororesins, polyimides, and / or polyamide-imides are preferable.

[0073] [Ion exchange resin membrane (ion exchange membrane)] The ion exchange resin membrane used in this embodiment is not particularly limited, and any suitable ions fixed to the resin membrane can be used. A filter containing an ion exchange resin containing exchange groups can be used. As an exchange resin film, a strong acid is used, which is chemically modified on the resin film with cation exchange groups such as sulfonic acid groups. It contains a cation exchange resin, for example, cellulose, diatomaceous earth, nylon (a resin containing amide). Fat, polyethylene, polypropylene, polystyrene, resin having imide groups, amide groups A resin having an imide group, a fluororesin, or an integrated structure of a particle removal membrane and an ion exchange resin membrane. It includes a high-density polyethylene membrane and an ion exchange resin membrane having a particle removal membrane. A polyalkylene membrane having chemically modified ion exchange groups is preferred. This includes, for example, polyethylene and polypropylene, with polypropylene being preferred. As the ion exchange group, a cation exchange group is preferred. The lipid film can be any of the various commercially available filters that have metal ion removal capabilities. The filter was selected based on ion exchange efficiency, and the estimated pore size of the filter is approximately 0.2 μm (200 It is (nm).

[0074] [Ion adsorption membrane] Ion adsorption membranes are porous membrane materials that have ion exchange functions. Such ion adsorption membranes are There are no particular limitations as long as the pore size is 100 μm or less and it has ion exchange function. The material, type, etc., are not particularly limited. Examples of substrates constituting the ion adsorption film are limited. Although not made of cellulose, diatomaceous earth, nylon (a resin with amide groups), polyethylene Polypropylene, polystyrene, resin having imide groups, resin having amide groups and imide groups Film materials for precision filtration membranes such as resins, fluororesins, or high-density polyethylene resins, This includes film materials into which ON-exchange functional groups have been introduced. An example of the shape of the film material is Japanese Patent Publication No. 20 As described in No. 03-112060, pleated type, flat membrane type, hollow fiber type, porous type This includes the body, etc. The ion exchange groups introduced into the membrane material are optimized for the elution and selection of the components to be removed. To convert, at least two of the following are required: a cation exchange group, a chelate exchange group, and an anion exchange group. It is preferable to use a combination of these. Since the ion adsorption membrane is porous, fine particles It is also possible to remove a portion of it. In certain embodiments of this disclosure, the ion adsorption membrane is, for example, For example, it is a nylon film with a small pore size of 0.02 μm (20 nm).

[0075] In the chemical liquid preparation process of this embodiment, the ion exchange resin membrane or ion adsorption membrane is used beforehand. It is brought into contact with an organic solvent. Commercially available ion exchange resin membranes or ion adsorption membranes in a dry state are There are also hydrophilic materials that have a high affinity for aqueous solutions. In this embodiment, such Even when an ion-exchange resin film or an ion-adsorbent film is used, pre-contact with an organic solvent is performed on an untreated surface. To effectively remove metal impurities from the chemical liquid, and to pre-apply an ion exchange resin membrane or ion adsorption membrane Compared to cases where the material is not in contact with an organic solvent, the reducing effect is significantly superior.

[0076] [Methods for producing chemical liquids] An exemplary method for producing a chemical liquid includes providing a chemical liquid production 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, and if the first material processing system 110 includes multiple 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, and the second material processing system 1 2 If 0 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. A method for producing a chemical liquid also includes transporting the material to be processed to a first material processing system 110, processing the material once with one or more first filtration media 114 in the first material processing system 110, and, if necessary, recirculating the material to the first material processing system 110 for further processing. A production method also includes delivering the material to a second material processing system 120, processing the material with one or more second filtration media 124 in the second material processing system 120, and recirculating the material so that it is processed at least twice by the second material processing system 120. The manufacturing method further includes, at the end of each process in the second material processing system 120, collecting a sample of the chemical liquid in situ using a sample detector 150, such as an in-line particle counter 150, and measuring the number of particles and the amount of metal impurities remaining in the chemical liquid. If the number of particles and the amount of metal impurities detected in the sample exceed a desired predetermined range, the chemical liquid is recycled and processed again by the second material processing system 120. Once it is confirmed that the number of particles and the amount of metal impurities detected in the sample by the particle counter 150 are within the predetermined range and a high-purity chemical liquid is produced, the recycling or processing by the second material processing system 120 is immediately terminated, and the chemical liquid is transported to either packaging or the next processing stage 140.

[0077] According to some embodiments of this disclosure, a reverse osmosis membrane (RO) used in aqueous solvents It is preferable not to use a filter.

[0078] [Examples] The present disclosure will be described in more detail below based on the following examples. The materials used in the following examples are shown below. The dosage, proportion, processing content, processing procedure, etc. may be changed as appropriate without departing from the spirit of the present invention. This is possible. Therefore, the scope of this disclosure should not be interpreted restrictively by the following examples. Unless otherwise specified, "ppt," "ppb," and "ppm" are based on mass. ru.

[0079] <Preparation of chemical liquids> The chemical liquid in the example is cyclohexanone, and the raw material is cyclohexanone (pretreatment). By supplying the cyclohexanone (or the substance to be processed) to the chemical liquid manufacturing apparatus of this disclosure, It was made.

[0080] Arrangement, filtration medium 114 and second material in the first material processing system 110 (unit A) Selection of the filtration medium 124 in the material processing system 120 (unit B), for example, functionality, Pore ​​diameter, structural material and / or number of units of filter media 114 and filter media 124, and selection The number of times the raw material cyclohexanone passes through the filtration medium 114 and the selected filtration medium 124. The chemical liquids of the composition of each example were prepared by adjusting the parameters.

[0081] <Wafer mapping, OWPC, OWMC, defect assessment> Each chemical liquid sample was collected and inserted into a wafer coating tool. A test was then performed on a bare wafer. After coating the wafer with the material, it was moved to a laser-based inspection system for inspection. The laser-based inspection system uses laser light to detect wafers with a detection limit of 19 nm. The position and size of each particle were detected, counted, and recorded. More specifically, the particles to be counted were 19n This included particles with a size of m or larger. This data was used to create a wafer map. We created a dataset and provided the total number of particles on the wafer (OWPC).

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

[0083] <Total trace metals (ppb)> Each chemical liquid sample is analyzed using ICP-MS (inductively coupled plastic). Tested using SMA (Small Masometric Spectrometry). Fujifilm Using the developed method, each sample was tested for the presence of 26 metal species, and the detection limit was set for the metals. While specific to the specific type, the general detection limit was in the range of 0.00010–0.030 ppb. Next, the concentrations of each metal species are summed up to generate a value expressed as total trace metals (ppb). did.

[0084] <Liquid particle count LPC (>0.05um)> Each sample was tested using a liquid particle counter. This instrument detects particles in a liquid sample. Laser light was used to obtain the number and size, with a detection limit of 0.05 μm. The values ​​are expressed in units of "particles / ml".

[0085] <Evaluation Results> As shown in Table 1, each example was prepared using the chemical liquid manufacturing apparatus of this disclosure, but the chemical liquid manufacturing The manufacturing apparatus was configured differently to process the raw materials (objects to be processed) in each example. Various configurations of the chemical liquid manufacturing apparatus (raw cyclohexanone) are summarized in Table 1. As such, various processes W, X, Y, and Z were designed. Raw material (raw cyclo Hexanone was used as the baseline sample.

[0086] [Table 1]

[0087] In another embodiment, a filter having the smallest pore size (pore size less than 10 nm) is placed in unit A Example W-1 was manufactured in the same manner as Example W, except that it was placed on the upstream side. LPC, O WPC and OWMP are smaller than example W.

[0088] In another embodiment, a filter having the largest pore size (pore size greater than 50 nm) Except for being positioned at the uppermost upstream side of Unit A, Example W-2 was manufactured in the same manner as Example W. It was constructed. LPC, OWPC, and OWMP are smaller than example W.

[0089] Methanol, ethanol, 1-propanol, isopropanol, monomethyl ether propylene glycol monomethyl ether, propylene glycol monoethyl ether propylene glycol monopropyl ether, propylene glycol monomethyl ether Ethyl acetate, ethyl lactate, methyl methoxypropionate, cyclopentanone, cyclo Xanone, γ-butyrolactone, diisoamyl ether, butyl acetate, 4-methyl-2- Even if it is changed to a solvent selected from the group consisting of pentanol, and combinations thereof, the same tendency is obtained. Among them, cyclohexanone, PGMEA, butyl acetate, propylene glycol monomethyl ether acetate, and isopropanol are used to obtain better performance is obtained, and when cyclohexanone is used, even better performance is obtained.

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

Table 2

[0091]

Table 3

[0092]

Table 4

[0094] According to the results summarized in Table 3, the chemical liquid prepared by the chemical liquid manufacturing apparatus 10 of the present disclosure ​​​​In the liquid, it was also confirmed that the total liquid particle count (LPC) decreased significantly. The LPC of the X and W samples was less than 100 compared to the baseline sample with a value of 1 22556, and was 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, the chemical liquid prepared by the chemical liquid manufacturing apparatus 10 of the present disclosure has achieved the desired advantage of having very low counts in OWPC and OWMP as demonstrated. The OWPC of the X and W samples was 597 and 126 respectively , and the OWMP of the X and W samples was 43 and 1 respectively.

[0096] <00,00917>The above outlines the features of several embodiments so that those skilled in the art can better understand the aspects of the present disclosure. Those skilled in the art should understand that the present disclosure can be readily 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 do not depart from the spirit and scope of the present disclosure, and various changes, substitutions, and modifications can be made in the present specification without departing from the spirit and scope of the present disclosure.​​​​​​​​

Claims

1. A chemical liquid manufacturing apparatus for preparing chemical liquids for semiconductor manufacturing, A first system configured to process material from a supply unit to be processed, the first system comprising at least one first filtration medium selected from a first filter, a first ion exchange membrane, and a first ion adsorption membrane, and a first moisture removal device, the first moisture removal device selected from the group consisting of a dehydration membrane, a water absorbent, an aeration exchange device, and a heating device, and the first system configured to process the material at least once. A second system configured to process the aforementioned material, the second system comprising at least one second filtration medium selected from a second filter, a second ion exchange membrane, and a second ion adsorption membrane, and a second moisture removal device, the second moisture removal device being selected from the group consisting of a dehydration membrane, a water absorbent, an aeration exchange device, and a heating device, and the second system configured to process the aforementioned material at least twice for the purpose of recirculation. Includes, The routes constituting the first system and the routes constituting the second system do not overlap with each other. A chemical liquid manufacturing apparatus in which the first system is located upstream of the second system, and the material is processed by the first system before being processed by the second system.

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

3. The chemical liquid production apparatus according to claim 1, wherein the at least one second filtration medium includes the second filter, and the second filter is a particle size sieving filter having a pore size of about 10 nm or less.

4. The chemical liquid manufacturing apparatus according to claim 1, wherein the at least one first filtration medium includes the first filter, and the pore size of the first filter is about 50 nm or more.

5. The chemical liquid manufacturing apparatus according to claim 1, wherein the at least one first filtration medium includes the first filter, and the pore size of the first filter is about 15 nm or more.

6. The chemical liquid manufacturing apparatus according to claim 1, comprising the first ion exchange membrane or the first ion adsorption membrane.

7. The chemical liquid manufacturing apparatus according to claim 1, further comprising an online particle counter.

8. A chemical liquid manufacturing apparatus for processing materials from a processing target supply unit in order to prepare chemical liquids for semiconductor manufacturing, A first system comprising 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 a first moisture removal device, wherein the first moisture removal device is selected from the group consisting of a dehydration membrane, a water absorbent, an aeration exchange device, and a heating device, and the first system is configured to process the material at least once. A second system comprising 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 a second moisture removal device, wherein the second moisture removal device is selected from the group consisting of a dehydration membrane, a water absorbent, an aeration exchange device, and a heating device, and the second system is configured to process the material at least twice for the purpose of recirculation. Includes, The routes constituting the first system and the routes constituting the second system do not overlap with each other. A chemical liquid manufacturing apparatus in which the first system is located upstream of the second system, and the material is processed by the first system before being processed by the second system.

9. The chemical liquid manufacturing apparatus according to claim 8, wherein the at least one first filter comprises two first filters, the two first filters having different characteristics.

10. The chemical liquid manufacturing apparatus according to claim 9, wherein the two first filters differ in at least one of their pore size and structural material.

11. The chemical liquid manufacturing apparatus according to claim 10, wherein one of the two first filters has a pore size of approximately 50 nm or more.

12. The chemical liquid manufacturing apparatus according to claim 10, wherein one of the two first filters has a pore size of about 10 nm or less.

13. The chemical liquid manufacturing apparatus according to claim 8, wherein the at least one second filter comprises two second filters, the two second filters having different characteristics.

14. The chemical liquid manufacturing apparatus according to claim 13, wherein the two second filters differ in at least one of their pore size and structural material.

15. The chemical liquid manufacturing apparatus according to claim 13, wherein at least one of the two second filters is a particle size sieving filter having a pore size of about 10 nm or less.

16. The chemical liquid manufacturing apparatus according to claim 8, wherein the first system is configured such that the material passes through it once.

17. The chemical liquid manufacturing apparatus according to claim 8, comprising a first ion exchange membrane or a first ion adsorption membrane.

18. A chemical liquid manufacturing apparatus for preparing chemical liquids for semiconductor manufacturing, A first system comprising one or more first purification media and a first moisture removal device, wherein the first moisture removal device is selected from the group consisting of a dehydration membrane, a water absorbent, an aeration exchange device, and a heating device, and if the first system comprises multiple first purification media, at least two of the multiple first purification media are different in function, pore size, or material from the first system. A second system comprising one or more second purification media and a second moisture removal device, wherein the second moisture removal device is selected from the group consisting of a dehydration membrane, a water absorbent, an aeration exchange device, and a heating device, and if the second system comprises multiple second purification media, at least two of the multiple second purification media are second systems with different functions, pore sizes, or materials. Includes, The first system is configured to process material from a processing supply unit at least once. The second system is configured to process the material at least twice for the purpose of recirculation. The routes constituting the first system and the routes constituting the second system do not overlap with each other. A chemical liquid manufacturing apparatus in which the first system is located upstream of the second system, and the material is processed by the first system before being processed by the second system.

19. The chemical liquid production apparatus according to claim 18, wherein the one or more first purification media are selected from a filter, an ion exchange membrane, and an ion adsorption membrane.

20. The chemical liquid production apparatus according to claim 18, wherein the one or more second purification media are selected from a filter, an ion exchange membrane, and an ion adsorption membrane.

Images