WO2019181580A1 - ろ過装置、精製装置、薬液の製造方法 - Google Patents
ろ過装置、精製装置、薬液の製造方法 Download PDFInfo
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- WO2019181580A1 WO2019181580A1 PCT/JP2019/009500 JP2019009500W WO2019181580A1 WO 2019181580 A1 WO2019181580 A1 WO 2019181580A1 JP 2019009500 W JP2019009500 W JP 2019009500W WO 2019181580 A1 WO2019181580 A1 WO 2019181580A1
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- filter
- filtration device
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
- B01D2325/0283—Pore size
- B01D2325/02832—1-10 nm
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
- B01D2325/0283—Pore size
- B01D2325/02833—Pore size more than 10 and up to 100 nm
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/14—Membrane materials having negatively charged functional groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/16—Membrane materials having positively charged functional groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/42—Ion-exchange membranes
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
Definitions
- the present invention relates to a filtration device, a purification device, and a method for producing a chemical solution.
- a chemical solution containing water and / or an organic solvent is used as a cleaning solution after CMP, or as a diluted solution thereof.
- pattern miniaturization has progressed due to advances in photolithography technology.
- the chemical solution used in such a wiring formation process is required to further improve the defect suppression performance.
- Such a chemical solution is generally considered to be obtained by purifying a to-be-purified solution containing as a main component a component required for a chemical solution using a filter or the like to remove impurities and the like.
- Patent Document 1 discloses “a porous PTFE membrane including a porous polytetrafluoroethylene PTFE substrate having a non-crosslinked coating including a perfluorosulfonic acid polymer”.
- Patent document 2 describes “polytetrafluoroethylene blended with perfluorosulfonic acid polymer (porous membrane)”.
- the present inventors obtained a chemical solution by purifying the liquid to be purified using the filter and evaluated the defect suppression performance related to the chemical solution, and found that sufficient defect suppression performance may not be obtained. did. Then, this invention makes it a subject to provide the filtration apparatus which can manufacture the chemical
- Another object of the present invention is to provide a purification device and a method for producing a chemical solution.
- the “defect suppression performance” of a chemical means the performance of the chemical evaluated by the method described in the examples.
- Each chemical solution used for manufacturing a semiconductor substrate is required to have “defect suppression performance” corresponding to the type and role of the chemical solution.
- a chemical liquid that does not substantially contain a resin typically, a prewet liquid, a developer, a rinse liquid, etc.
- the residual defect suppression performance described in [Test Example 1] in Examples described later is referred to as “defect suppression performance”.
- the scum defect suppression performance described in [Test Example 3] in the example mentioned below be “defect suppression performance.”
- medical solution typically used as an etching liquid, resist stripping solution, a developing solution, etc.
- defect suppression performance it means each defect suppression performance (residue defect suppression performance, scum defect suppression performance, or metal defect ratio) according to the type of chemical.
- An inflow portion, an outflow portion, a filter A, and at least one filter B different from the filter A are provided, and the filter A and the filter B are arranged in series between the inflow portion and the outflow portion.
- a filtration device for purifying a liquid to be purified to obtain a chemical solution having a flow passage from the inflow portion to the outflow portion, wherein the filter A includes a porous substrate made of polytetrafluoroethylene, A first porous membrane having a non-crosslinked coating containing a perfluorosulfonic acid polymer formed over the substrate, and a second porous membrane containing polytetrafluoroethylene blended with the perfluorosulfonic acid polymer
- a filtration device comprising at least one selected from the group consisting of: [2] The filtration device according to [1], wherein the filter B includes at least one filter BD disposed on the downstream side of the filter A on the flow path.
- the filtration device according to [2], wherein at least one filter BD has a pore diameter of 20 nm or less.
- the filter BD disposed on the most downstream side has a pore diameter of 10 nm or less, and contains at least one selected from the group consisting of polytetrafluoroethylene, polyethylene, and nylon.
- the filtration device according to any one of [4].
- a filtration device for purifying a liquid to be purified to produce a chemical solution for producing a semiconductor substrate wherein the inflow portion, the outflow portion, the filter A, and the filter A are at least one filter B.
- the filter A and the filter B are arranged in series between the inflow portion and the outflow portion, and have a flow passage from the inflow portion to the outflow portion, and the filter A is made of polytetrafluoro
- a first porous membrane having a porous substrate made of ethylene, a non-crosslinked coating containing a perfluorosulfonic acid polymer formed to cover at least a portion of the substrate, and blended with the perfluorosulfonic acid polymer
- a filtration device comprising at least one selected from the group consisting of a second porous membrane containing polytetrafluoroethylene.
- a purification device comprising the filtration device according to any one of [1] to [20] and at least one distiller connected to an inflow portion of the filtration device.
- a method for producing a chemical solution wherein the liquid to be purified is obtained by purifying the solution to be purified by using the filtration device according to any one of [1] to [20].
- a method for producing a chemical solution comprising a filtration step.
- the method for producing a chemical solution according to [23] further including a filter cleaning step of cleaning the filter A and the filter B before the filtration step.
- a method for producing a chemical solution by purifying a solution to be purified to obtain a chemical solution wherein the solution to be purified is formed so as to cover a porous substrate made of polytetrafluoroethylene and at least a part of the substrate. Selected from the group consisting of a first porous membrane having a non-crosslinked coating containing a perfluorosulfonic acid polymer and a second porous membrane containing polytetrafluoroethylene blended with the perfluorosulfonic acid polymer.
- medical solution manufacturing method which has the process of obtaining the chemical
- the present invention it is possible to provide a filtration device capable of producing a chemical solution having excellent defect suppression performance.
- the present invention can also provide a purification device and a method for producing a chemical solution.
- a numerical range expressed using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.
- the filtration device includes an inflow portion, an outflow portion, a filter A, and at least one filter B different from the filter A, and the filter A and the filter B include the inflow portion and the outflow portion.
- at least one filter B different from the above filter A is a filtration device having a flow path from the inflow portion to the outflow portion, and the filter A includes a first porous membrane, which will be described later, and
- the filtration device is at least one selected from the group consisting of the second porous membranes.
- the filtration device has a flow path from the inflow portion to the outflow portion, and a filter A and at least one filter B different from the filter A are arranged in series between the inflow portion and the outflow portion. Since the filter A and the filter B according to the embodiment of the present invention are arranged in series on the flow path, the liquid to be purified is sequentially filtered by the filter A and the filter B (or the filter B and the filter A). Is done.
- the filtration apparatus which concerns on embodiment of this invention is demonstrated, in the following description, the filtration apparatus of the whole quantity filtration system (dead end system) which filters the whole quantity of the to-be-purified liquid introduce
- the filtration device is not limited to the above, and the introduced liquid to be purified is separated into a purified liquid to be purified and a concentrated liquid (further, the concentrated liquid is again introduced into the filter as a liquid to be purified). It may be a cross flow type filtration device, or a combination of these. Below, embodiment of the said filtration apparatus is described using drawing.
- Drawing 1 is a mimetic diagram showing the filtration device concerning a first embodiment of the present invention.
- the filter device 100 includes a filter 103 as a filter A and a filter 104 (filter BD) different from the filter 103 arranged in series via a pipe 105 between an inflow portion 101 and an outflow portion 102. It is.
- the inflow part 101, the filter 103, the pipe 105, the filter 104, and the outflow part 102 are configured so that the liquid to be purified can be circulated therein, and the flow path S ⁇ b> 1 (liquid to be purified) is connected to the above members. Is formed).
- the inflow part 101 and the outflow part 102 are not particularly limited as long as the liquid to be purified can be introduced into and discharged from the filtration device, but typically, a hollow cylinder having an inlet and an outlet. Shaped pipes (inflow pipe and outflow pipe) and the like. Hereinafter, a mode in which the outflow part and the inflow part are pipes will be described as an example.
- the forms of the inflow part 101, the pipe 105, and the outflow part 102 are not particularly limited, but typically, a hollow cylindrical form formed to allow the liquid to be purified to flow therethrough can be given. Although these material components are not particularly limited, it is preferable that the liquid contact portion (portion where the liquid to be purified may come into contact with when the liquid to be purified is filtered) is formed of a corrosion-resistant material described later. .
- the liquid to be purified introduced from the inflow portion 101 of the filtration device 100 flows through the filtration device 100 along the flow path S1, and is sequentially filtered by the filter 103 (filter A) and the filter 104 (filter BD). And discharged from the outflow portion 102 to the outside of the filtration device 100.
- the form of the liquid to be purified will be described later.
- the filtration device 100 is provided with a pump, a damper, a valve, etc. (not shown) on the flow passage S1 (for example, the inflow portion 101, the pipe 105, and the outflow portion 102) for the purpose of circulating the liquid to be purified. You may have.
- the form of the filter 103 (filter A) and the filter 104 (filter B) is not particularly limited.
- Examples of the form of the filter A and the filter B include a planar shape, a pleated shape, a spiral shape, and a hollow cylindrical shape.
- a core material that is typically formed of a material that allows the liquid to be purified to permeate and / or has a structure that allows the liquid to be purified to permeate, and the core material are wound.
- a cartridge filter having a filter disposed on the core in a rotated form is preferred.
- the core material is not particularly limited, but is preferably formed from a corrosion-resistant material described later.
- the method of arranging the filter is not particularly limited, but typically includes at least one inlet and at least one outlet, and is provided in a housing (not shown) in which at least one flow passage is formed between the inlet and the outlet. It is preferable to arrange
- the flow passage formed in the housing forms a part of the flow passage S1, and the liquid to be purified is filtered by a filter disposed across the flow passage S1 when flowing through the flow passage S1.
- the material of the housing is not particularly limited, and includes any suitable hard impermeable material including any impermeable thermoplastic material that is compatible with the liquid to be purified.
- the housing can be made of a metal such as stainless steel, or a polymer.
- the housing is a polymer such as polyacrylate, polypropylene, polystyrene, or polycarbonate.
- at least a part of the wetted part of the housing preferably 90% of the surface area of the wetted part, more preferably the surface area of the wetted part, in that a more excellent filtration device having the effect of the present invention is obtained.
- 99% is preferably made of a corrosion-resistant material described later.
- the liquid contact part means a part (excluding the filter itself) with which the liquid to be purified may come into contact, and means an inner wall of a unit such as a housing.
- the filter A has at least one film selected from the group consisting of a first porous film and a second porous film described later.
- the first porous membrane has a porous substrate made of polytetrafluoroethylene (PTFE) and a non-crosslinked coating containing a perfluorosulfonic acid (PFSA) acid polymer formed so as to cover the porous substrate.
- PTFE polytetrafluoroethylene
- PFSA perfluorosulfonic acid
- the porous substrate which the 1st porous film has may have the area
- the porous substrate made of polytetrafluoroethylene is not particularly limited, and those commercially available as PTFE porous substrates can be used as appropriate.
- the method for producing the first porous membrane is not particularly limited, but typically, a polymer dispersion containing a perfluorosulfonic acid (PFSA) polymer is applied to a PTFE porous substrate to form a non-crosslinked coating ( The method of forming the layer) is preferred.
- PFSA perfluorosulfonic acid
- the PFSA polymer dispersion for forming the coating (layer) is not particularly limited, but is available from Solvay Specialty Polymers (Borger, Texas) to AQUIVION® PFSA (eg, Aquivion PFSA D83-24B, Aquivion PFSA -06A, and Aquivion PFSA D79-20BS), which is a short side chain of tetrafluoroethylene and sulfonyl fluoride vinyl ether (SFVE) F 2 C ⁇ CF—O—CF 2 —CF 2 —SO 2 F (SSC) copolymer.
- the ionomer dispersion contains its sulfonic acid form.
- DuPont® Nafion® PFSA polymer dispersion is also preferred as the PFSA polymer dispersion.
- the content of PFSA in the coating solution can be adjusted as appropriate.
- the content is preferably in the range of 0.1 to 3% by mass, more preferably in the range of 0.12 to 2.2% by mass with respect to the total mass of the coating solution.
- the method for forming the coating on the substrate is not particularly limited, and examples thereof include a method of immersing the substrate in the coating solution and a method of spraying the coating solution on the substrate.
- the pore diameter of the first porous membrane is not particularly limited, but is generally preferably 1 to 200 nm and more preferably 10 to 20 nm.
- the pore size is determined by the bubble point of isopropanol (IPA) or HFE-7200 (“Novec 7200”, manufactured by 3M, hydrofluoroether, C 4 F 9 OC 2 H 5 ). Means the pore diameter.
- the thickness of the coating (layer) is not particularly limited, but is generally preferably 5 to 127 ⁇ m, more preferably 13 to 25 ⁇ m.
- the critical wet surface tension (for example, CWST; critical wetting surface tension defined in US Pat. No. 4,925,572) of the first porous membrane (filter A) is not particularly limited.
- CWST can be measured using a set of solutions of constant composition. Each solution has a specific surface tension. The surface tension of the solution ranges from 25 ⁇ 10 ⁇ 5 to 92 ⁇ 10 ⁇ 5 N / cm in small unequal increments.
- the first porous membrane is placed on a white light table, a drop of solution with a constant surface tension is applied to the surface of the membrane, and the droplet is in the first porous The time taken for the light to pass through the membrane and become bright white indicating that light has passed through the membrane is recorded.
- CWST is further known, for example, from US Pat. Nos. 5,152,905, 5,443,743, 5,472,621, and 6,074,869, as known in the art. Can be selected as disclosed in the issue.
- the critical wet surface tension of the first porous membrane is preferably 27 ⁇ 10 ⁇ 5 N / cm or more.
- the inventors have determined that the defect suppression performance of the obtained chemical solution may be affected by the correlation between the physical properties of the liquid to be purified and the critical wet surface tension of the first porous membrane. I caught it.
- the critical wet surface tension of the first porous membrane (filter A) according to the type of the liquid to be purified, a chemical solution having better defect suppression performance can be obtained.
- the critical wet surface tension is 27 ⁇ 10 ⁇ 5 N / cm or more, metal impurities and the like contained in the liquid to be purified can be more efficiently removed, resulting in more excellent defects. A chemical solution having inhibitory performance is obtained.
- the critical wet surface tension is more preferably 30 ⁇ 10 ⁇ 5 N / cm or more, and further preferably 33 ⁇ 10 ⁇ 5 N / cm or more.
- the first porous film has a smaller absolute value of the difference between the critical wet surface tension of the first porous film and the surface tension of the liquid to be purified.
- the surface tension of an organic solvent is generally 15 ⁇ 10 ⁇ 5 to 35 ⁇ 10 ⁇ 5 N / cm so that the surface tension of isopropyl alcohol is 20.8 (25 ° C.) ⁇ 10 ⁇ 5 N / cm.
- the critical wet surface tension of the first porous membrane is generally preferably 40 ⁇ 10 ⁇ 5 N / cm or less.
- the criticality of the first porous membrane is determined.
- a form in which the wet surface tension exceeds 40 ⁇ 10 ⁇ 5 N / cm is also preferable.
- the critical wet surface tension of the first porous membrane can be adjusted by the content of the perfluorosulfonic acid polymer in the non-crosslinked coating containing the perfluorosulfonic acid polymer. Specifically, if the content of the perfluorosulfonic acid polymer in the non-crosslinked coating is increased, a first porous membrane having a higher critical wet surface tension can be easily obtained. If the content is reduced, a first porous membrane having a lower critical wet surface tension can be easily obtained.
- the second porous membrane is a porous membrane containing polytetrafluoroethylene blended with a perfluorosulfonic acid polymer.
- PTFE is not particularly limited, and known PTFE can be used.
- the PFSA blended with PTFE is not particularly limited, but, for example, Solvay Specialty Polymers (Borger, Texas) to Aquivion (registered trademark) PFSA (eg, Aquivion PFSA D83-24B, Aquivion PFSA P83 AFP D79-20BS) which is a short side chain (SSC) copolymer of tetrafluoroethylene and sulfonyl fluoride vinyl ether (SFVE) F 2 C ⁇ CF—O—CF 2 —CF 2 —SO 2 F. Based on.
- the ionomer dispersion contains its sulfonic acid form.
- Another example of a suitable PFSA additive is DuPont® Nafion® PFSA polymer dispersion.
- the content of PFSA is not particularly limited.
- the content of PFSA is typically preferably 1 to 20% by weight, more preferably 1 to 4% by weight, based on the total weight of the blend.
- the method for producing the second porous membrane is not particularly limited, and a known method can be used.
- a lubricant it does not restrict
- PFSA can be sprayed onto the PTFE resin (eg, to improve distribution) prior to physical mixing with the lubricant.
- a required amount of PTFE powder is mixed with a solution of PFSA in an appropriate solvent, for example, an alcohol solvent such as methanol, ethanol, or isopropanol, to obtain a blend.
- an appropriate solvent for example, an alcohol solvent such as methanol, ethanol, or isopropanol
- the blend is then mixed with a odorless mineral spirit, such as a lubricant such as Isopar G, and the resulting paste is subjected to shearing, for example with a twin roller, at least twice, at 2 MPa or more pressure.
- shearing for example with a twin roller, at least twice, at 2 MPa or more pressure.
- each is molded into billets for about 55 seconds.
- the resulting billet is allowed to equilibrate for about 12 hours or longer at room temperature.
- the billet is then extruded into the desired shape.
- extrusion is performed at a die gap size of 26 mm, a maximum pressure, and a constant temperature of 55 ° C. to obtain a tube-shaped PTFE tape.
- the tube-shaped tape is cut open along the central axis and rewound around the pipette to obtain a new billet (uncompressed).
- This new billet is extruded again under the same conditions used in the initial extrusion process.
- This step is added to impart advantageous cross direction mechanical properties to the PTFE tape.
- the calendering is performed at 30 ° C. with a target tape thickness of 200-250 ⁇ m.
- the resulting tape is then dried at 125 ° C. for 1 hour to remove the lubricant from the extruded tape.
- the stretch ratio in the machine direction (MD) and the transverse direction (TD) is 3 at a stretch rate of 300% / second.
- the temperature in the drawing oven is set to 150 ° C.
- the stretched tape is annealed.
- Annealing is performed in an annealing oven, after which the tape is cooled.
- the porosity generated by the stretching is retained during cooling.
- IPA isopropyl alcohol
- the pore diameter of the second porous membrane is not particularly limited, but is preferably 1 to 200 nm, more preferably 10 to 20 nm.
- the thickness of the second porous membrane is not particularly limited, but is generally preferably 5 to 127 ⁇ m, more preferably 0.5 to 1.0 ⁇ m.
- the critical wet surface tension of the second porous membrane (filter A) is preferably 27 ⁇ 10 ⁇ 5 N / cm or more.
- the present inventors have determined that the defect suppression performance of the obtained chemical solution may be influenced by the correlation between the physical properties of the liquid to be purified and the critical wet surface tension of the second porous membrane. It was.
- the critical wet surface tension is 27 ⁇ 10 ⁇ 5 N / cm or more, it is possible to more efficiently remove metal impurities and the like contained in the liquid to be purified, and as a result, a chemical solution having better defect suppression performance. Is obtained.
- the critical wet surface tension is more preferably 30 ⁇ 10 ⁇ 5 N / cm or more, and further preferably 33 ⁇ 10 ⁇ 5 N / cm or more.
- the second porous membrane contains an organic solvent (when it is an “organic solvent-based liquid to be purified” described later) or the like, from the viewpoint of reducing the difference from the surface tension of the liquid to be purified, the second porous membrane
- the critical wet surface tension is preferably 40 ⁇ 10 ⁇ 5 N / cm or less.
- the second porous when the surface tension of the liquid to be purified is larger (for example, when the liquid to be purified contains water or the like, when the liquid to be purified is an “aqueous system liquid to be described later” or the like), the second porous It is also preferred that the critical wet surface tension of the membrane exceeds 40 ⁇ 10 ⁇ 5 N / cm.
- the critical wet surface tension of the second porous membrane can be adjusted by the content of the perfluorosulfonic acid polymer in polytetrafluoroethylene blended with the perfluorosulfonic acid polymer.
- a second porous membrane having a higher critical wetting surface tension can be obtained, and if the content of the perfluorosulfonic acid polymer is decreased, the lower critical wetting is achieved. It is easy to obtain a second porous film having surface tension.
- the filter BD is a filter different from the filter A, and is a filter arranged in series with the filter A on the downstream side of the filter A on the flow path.
- different filters mean that at least one selected from the group consisting of pore diameter, material, and pore structure is different.
- the filter A and the filter BD preferably have different pore diameters, and preferably have different pore diameters and materials, in that a more excellent filtration device having the effect of the present invention can be obtained.
- the different materials typically include forms having different constituent components (material components).
- the pore size of the filter BD is not particularly limited, and a filter having a pore size normally used for filtering the liquid to be purified can be used.
- the pore diameter of the filter is preferably 200 nm or less, more preferably 20 nm or less, still more preferably 10 nm or less, particularly preferably 7 nm or less, and most preferably 5 nm or less.
- limit especially as a lower limit Generally 1 nm or more is preferable from a viewpoint of productivity.
- the filtration device according to the present embodiment has the filter BD on the downstream side of the filter A on the flow path, the fine particles resulting from the filter A can be separated from the liquid to be purified, and more excellent defect suppression. It is easy to obtain chemicals with performance.
- the filtration apparatus of FIG. 1 has one filter BD, as a filtration apparatus which concerns on this embodiment, you may have several filter BD.
- the relationship between the pore diameters of the plurality of filters BD is not particularly limited, but a plurality of pore diameters of the filter BD arranged on the most downstream side on the flow passage are easy in that a chemical solution having better defect suppression performance can be obtained. It is preferable to be the smallest among the filters BD.
- the filter BD arranged on the most downstream side means the filter BD arranged on the most downstream side among all the filters arranged in the flow path.
- the filter BD arranged on the most downstream side contains at least one selected from the group consisting of polyethylene (particularly ultrahigh molecular weight polyethylene; UPE), polytetrafluoroethylene, and nylon as a material component.
- polyethylene particularly ultrahigh molecular weight polyethylene; UPE
- polytetrafluoroethylene particularly ultrahigh molecular weight polyethylene; UPE
- nylon as a material component.
- the filter BD is typically arranged for the purpose of filtering out impurities that may be mixed in the liquid to be purified unintentionally when the product to be purified is filtered by the filter A or the like arranged on the upstream side. Is done.
- the impurities to be removed often differ depending on the material components contained in the filter BD.
- a filter BD containing nylon is presumed that gel-like impurities are easily adsorbed and removed by a hydrophilic layer presumed to be formed on the membrane in the liquid to be purified, and contains ultrahigh molecular weight polyethylene. It is presumed that the filter BD that easily removes particulate impurities due to the sieving effect.
- the filter BD When the liquid to be purified is an organic solvent-based liquid to be purified which will be described later, when the liquid to be purified is passed through a filter BD containing nylon or a filter BD containing ultrahigh molecular weight polyethylene, the filter BD The present inventors have found that unintended impurities may be mixed into the liquid to be purified due to the material. In such a case, if a filter containing polytetrafluoroethylene (preferably made of polytetrafluoroethylene) is arranged as the filter BD arranged on the most downstream side on the flow path, these impurities and the like are also removed. Possible and preferred.
- the pore size of the filter BD is not particularly limited, but is preferably 1 to 20 nm, more preferably 1 to 10 nm, and further preferably 1 to 7 nm.
- the relationship between the hole diameter of the filter A and the hole diameter of the filter BD is not particularly limited, but the hole diameter of the filter BD is preferably smaller than the hole diameter of the filter A.
- the hole diameter of the filter BD is preferably smaller than the hole diameter of the filter A.
- the material of the filter BD is not particularly limited, and may be the same as or different from the filter A. Especially, it is preferable that it differs from the material of the filter A by the point from which the filtration apparatus which has the more excellent effect of this invention is obtained.
- the filter BD includes, as material components, polyamide such as 6-nylon and 6,6-nylon; polyolefin such as polyethylene and polypropylene; polystyrene; polyimide; polyamideimide; poly (meth) acrylate; Polyfluorocarbons such as fluoroalkoxyalkanes, perfluoroethylenepropene copolymers, ethylene-tetrafluoroethylene copolymers, ethylene-chlorotrifluoroethylene copolymers, polychlorotrifluoroethylene, polyvinylidene fluoride, and polyvinyl fluoride; polyvinyl alcohol; polyester Cellulose; preferably containing cellulose acetate and the like.
- polyamide such as 6-nylon and 6,6-nylon
- polyolefin such as polyethylene and polypropylene
- polystyrene polyimide
- polyamideimide poly (meth) acrylate
- Polyfluorocarbons such as fluoroalkoxyalkan
- nylon especially 6,6-nylon is preferred
- polyolefin especially polyethylene is preferred
- polyfluorocarbon in particular, polytetrafluoroethylene (PTFE) and perfluoroalkoxyalkane (PFA) are preferred.
- PTFE polytetrafluoroethylene
- PFA perfluoroalkoxyalkane
- the filter may be surface-treated.
- the surface treatment method is not particularly limited, and a known method can be used. Examples of the surface treatment method include chemical modification treatment, plasma treatment, hydrophobic treatment, coating, gas treatment, and sintering.
- Plasma treatment is preferable because the surface of the filter is hydrophilized.
- the water contact angle on the surface of the filter medium hydrophilized by plasma treatment is not particularly limited, but the static contact angle at 25 ° C. measured with a contact angle meter is preferably 60 ° or less, more preferably 50 ° or less. 30 ° or less is more preferable.
- the filter is preferably a filter in which the above-mentioned materials are used as base materials and ion exchange groups are introduced into the base materials.
- a filter including a layer containing a substrate having an ion exchange group on the surface of the substrate is preferable.
- the surface-modified base material is not particularly limited, and those in which an ion exchange group is introduced into the polymer are preferable in terms of easier production.
- the ion exchange group examples include a sulfonate group, a carboxy group, and a phosphate group as a cation exchange group, and a quaternary ammonium group as an anion exchange group.
- the method for introducing the ion exchange group into the polymer is not particularly limited, but a method of reacting a compound having an ion exchange group and a polymerizable group with the polymer and typically grafting is exemplified.
- the method for introducing the ion exchange group is not particularly limited, but the resin fibers are irradiated with ionizing radiation ( ⁇ ray, ⁇ ray, ⁇ ray, X ray, electron beam, etc.) and an active moiety ( Radical).
- ionizing radiation ⁇ ray, ⁇ ray, ⁇ ray, ⁇ ray, X ray, electron beam, etc.
- Radical an active moiety
- the resin having the produced polymer as a side chain is contact-reacted with a compound having an anion exchange group or a cation exchange group, whereby an ion exchange group is introduced into the graft-polymerized side chain polymer to obtain a final product. It is done.
- the filter may have a configuration in which a woven fabric or a non-woven fabric in which an ion exchange group is formed by a radiation graft polymerization method and a conventional glass wool, woven fabric, or a non-woven fabric filter material.
- the filter BD is at least one selected from the group consisting of polyolefin, polyamide, polyfluorocarbon, polystyrene, polysulfone, and polyethersulfone, in that a filtration device having a better effect of the present invention can be obtained. It is preferable that the filter BD is made of at least one material component selected from the group consisting of polyolefin, polyamide, polyfluorocarbon, polystyrene, polysulfone, and polyethersulfone.
- the polyolefin include polyethylene and polypropylene. Among them, ultrahigh molecular weight polyethylene is preferable.
- the polyamide include 6-nylon and 6,6-nylon.
- Polyfluorocarbons include polytetrafluoroethylene (PTFE), perfluoroalkoxyalkanes, perfluoroethylene propene copolymers, ethylene-tetrafluoroethylene copolymers, ethylene-chlorotrifluoroethylene copolymers, polychlorotrifluoroethylene, polyvinylidene fluoride, and And polyvinyl fluoride, and the like.
- PTFE polytetrafluoroethylene
- perfluoroalkoxyalkanes perfluoroethylene propene copolymers
- ethylene-tetrafluoroethylene copolymers ethylene-chlorotrifluoroethylene copolymers
- polychlorotrifluoroethylene polyvinylidene fluoride
- polyvinyl fluoride and the like.
- PTFE is preferable.
- the pore structure of the filter BD is not particularly limited, and may be appropriately selected according to the component of the liquid to be purified.
- the pore structure of the filter BD means a pore size distribution, a positional distribution of pores in the filter, a shape of the pores, and the like. It can be controlled.
- a porous film can be obtained by forming a powder of resin or the like by sintering, and a fiber film can be obtained by forming by a method such as electrospinning, electroblowing, or meltblowing. These have different pore structures.
- Porous membrane is a membrane that retains components in the liquid to be purified, such as gels, particles, colloids, cells, and polyoligomers, but components that are substantially smaller than the pores pass through the pores. Means. The retention of the components in the liquid to be purified by the porous membrane may depend on operating conditions such as surface speed, use of surfactant, pH, and combinations thereof, and the pore size of the porous membrane, It may depend on the structure and the size of the particles to be removed and the structure (such as hard particles or gel).
- UPE (ultra high molecular weight polyethylene) filters are typically sieving membranes.
- sieving membrane is meant a membrane that captures particles primarily through a sieving retention mechanism, or a membrane that is optimized to capture particles via a sieving retention mechanism.
- Typical examples of sieve membranes include, but are not limited to, polytetrafluoroethylene (PTFE) membranes and UPE membranes.
- PTFE polytetrafluoroethylene
- the “sieving holding mechanism” refers to holding the result due to the removal target particle being larger than the pore diameter of the porous membrane.
- Sieve retention can be improved by forming a filter cake (aggregation of particles to be removed on the surface of the membrane). The filter cake effectively functions as a secondary filter.
- the pore structure of the porous membrane is not particularly limited, but examples of the pore shape include a lace shape, a string shape, and a node shape. It is done.
- the distribution of the pore size in the porous membrane and the distribution of the positions in the membrane are not particularly limited. The size distribution may be smaller and the distribution position in the film may be symmetric. Further, the size distribution may be larger, and the distribution position in the film may be asymmetric (the above film is also referred to as “asymmetric porous film”). In an asymmetric porous membrane, the pore size varies in the membrane and typically the pore size increases from one surface of the membrane to the other surface of the membrane.
- the surface on the side having many pores with a large pore diameter is referred to as “open side”, and the surface on the side having many pores with a small pore diameter is also referred to as “tight side”.
- examples of the asymmetric porous membrane include those having the smallest pore size at a certain position within the thickness of the membrane (this is also referred to as “hourglass shape”).
- the primary side is a larger-sized hole, in other words, if the primary side is the open side, a prefiltration effect can be produced.
- the porous membrane may include a thermoplastic polymer such as PESU (polyethersulfone), PFA (perfluoroalkoxyalkane, copolymer of tetrafluoroethylene and perfluoroalkoxyalkane), polyamide, and polyolefin.
- PESU polyethersulfone
- PFA perfluoroalkoxyalkane, copolymer of tetrafluoroethylene and perfluoroalkoxyalkane
- polyamide polyolefin
- polytetrafluoroethylene may be included.
- a porous membrane contains ultra high molecular weight polyethylene as a material component.
- Ultra high molecular weight polyethylene means a thermoplastic polyethylene having an extremely long chain, and preferably has a molecular weight of 1 million or more, typically 2 to 6 million.
- non-sieving membranes include, but are not limited to, nylon membranes such as nylon-6 membrane and nylon-6,6 membrane.
- the “non-sieving” retention mechanism refers to retention caused by a pressure drop of the filter or a mechanism such as obstruction, diffusion and adsorption that is not related to the pore size.
- Non-sieving retention includes retention mechanisms such as obstruction, diffusion and adsorption that remove particles to be removed from the liquid to be purified regardless of the pressure drop of the filter or the pore size of the filter.
- Adsorption of particles on the filter surface can be mediated, for example, by intermolecular van der Waals forces and electrostatic forces.
- a disturbing effect occurs when particles moving through a non-sieving membrane layer having a serpentine path cannot be redirected fast enough to not contact the non-sieving membrane.
- Particle transport by diffusion arises primarily from the random or Brownian motion of small particles that create a certain probability that the particles will collide with the filter media. If there is no repulsive force between the particles and the filter, the non-sieving retention mechanism can be active.
- the material of the fiber membrane is not particularly limited as long as it is a polymer capable of forming a fiber membrane.
- the polymer include polyamide.
- the polyamide include nylon 6 and nylon 6,6.
- the polymer that forms the fiber membrane may be poly (ether sulfone).
- the surface energy of the fiber membrane is preferably higher than the polymer that is the material of the porous membrane on the secondary side. Examples of such a combination include a case where the material of the fiber membrane is nylon and the porous membrane is polyethylene (UPE).
- the method for producing the fiber membrane is not particularly limited, and a known method can be used.
- Examples of the method for producing a fiber membrane include electrospinning, electroblowing, and meltblowing.
- FIG. 2 is a schematic diagram showing a filtration device according to the second embodiment of the present invention.
- the filtration device 200 is a filtration device in which a filter 103 that is a filter A and a filter 201 (filter BU) that is different from the filter 103 are arranged in series via a pipe 202 between an inflow portion 101 and an outflow portion 102. .
- the inflow part 101, the filter 201, the pipe 202, the filter 103, and the outflow part 102 are configured so that the liquid to be purified can be circulated therein, and the above-described members are connected to each other to connect the flow path S ⁇ b> 2 (liquid to be purified). Is formed).
- each filter and piping is the same as that of the filtration device according to the first embodiment already described, and the following description is limited to only the parts different from the first embodiment. Do. Therefore, the matter which is not demonstrated below is the same as that of the filtration apparatus which concerns on 1st embodiment.
- the filter BU is a filter different from the filter A, and is a filter arranged in series with the filter A on the upstream side of the filter A on the flow path. On the flow passage, the inflow portion is on the upstream side, and the outflow portion is on the downstream side.
- the filter A and the filter BU are preferably different from each other in terms of obtaining a more excellent filtration device having the effect of the present invention, and the pore diameter and the material are preferably different from each other.
- the pore size of the filter BU is not particularly limited, and a filter having a pore size normally used for filtering the liquid to be purified can be used.
- the pore diameter of the filter is preferably 1 nm or more, more preferably 3 nm or more, and still more preferably 10 nm or more.
- limit especially as an upper limit 1.0 micrometer or less is preferable, other than the form used as the filter C mentioned later, less than 200 nm is more preferable, less than 100 nm is still more preferable, and 50 nm or less is especially preferable.
- the hole diameter of at least 1 filter BU is in the said range, and the hole diameter of filter BU arrange
- the filter A when a filtration device in which a filter BU having a hole diameter of 20 nm or more is arranged on the upstream side of the filter A on the flow path S2, the filter A is less likely to be clogged. It has been found that the lifetime of A can be further extended. As a result, it is possible to obtain a filtration device that can stably provide a chemical having superior defect suppression performance.
- the relationship between the hole diameter of the filter A and the hole diameter of the filter BU is not particularly limited, but the hole diameter of the filter BU is preferably larger than the hole diameter of the filter A.
- the filtration device according to the present embodiment may have a plurality of filters BU.
- the relationship between the pore sizes of the plurality of filters BU is not particularly limited.
- the pore size of the filter BU arranged on the most upstream side in the flow passage is the maximum in that a chemical solution having better defect suppression performance is easily obtained. It is preferable to become. By doing in this way, the lifetime of the filter (including the filter A) disposed downstream of the most upstream filter BU can be extended, and as a result, a chemical solution having better defect suppression performance can be stabilized. Filtration device that can be provided.
- the resin having an ion exchange group is not particularly limited, and a filter containing a material component capable of removing ions (for example, metal ions) by the non-sieving effect described in the first embodiment can be used.
- a filter containing a material component capable of removing ions (for example, metal ions) by the non-sieving effect described in the first embodiment can be used.
- an anion exchange group is preferable as the ion exchange group, and examples of the anion exchange group include a quaternary ammonium group.
- filter BU contains resin which has an anion exchange group as a material component, the chemical
- a material component of the filter BU a material in which an anion exchange group is introduced into a base material such as polyfluorocarbon and polyolefin is more preferable.
- Drawing 3 is a mimetic diagram of a filtration device showing a modification of a filtration device concerning a second embodiment of the present invention.
- the filtration device 300 includes a filter 103 that is a filter A, a filter 201 that is a filter BU, and a filter 104 that is a filter BD between the inflow portion 101 and the outflow portion 102.
- the filter 201 and the filter 103 And a filter 104 in which the filter 104 is arranged in series via a pipe 301 and a pipe 302.
- each filter and piping is the same as the filtration apparatus according to the first embodiment already described, and the following description is limited to only the parts different from the first embodiment. Do. Therefore, the matter which is not demonstrated below is the same as that of the filtration apparatus which concerns on 1st embodiment.
- the inflow portion 101, the filter 201, the pipe 301, the filter 103, the pipe 302, and the filter 104 are configured so that the liquid to be purified can be circulated therein, and the above-described members are connected to the flow path S3 (liquid to be purified). Is formed).
- the configuration of the piping and each filter is as described above. Since the filter 300 has the filter BU on the upstream side of the filter A on the flow path, the filter A has a longer life, and has the filter BD on the downstream side of the filter A on the flow path. Fine particles mixed in the purified liquid can be efficiently removed, and as a result, a chemical liquid having further excellent defect suppressing performance can be easily obtained.
- FIG. 4 is a schematic view showing a filtration device according to the third embodiment of the present invention.
- the filtration device 400 further includes a tank 401 disposed in series with the filter A between the inflow portion 101 and the outflow portion 102 and upstream of the filter 103 (filter A) on the flow path S4. It is.
- the tank 401, the filter 103 (filter A), and the filter 104 (filter BD) are arranged in series via the pipe 402 and the pipe 105.
- the tank 401 constitutes the flow path S4 together with the above-described filter, piping, and the like.
- each filter and piping is the same as that of the filtration device according to the first embodiment already described, and the following description is limited to only the parts different from the first embodiment. Do. Therefore, the matter which is not demonstrated below is the same as that of the filtration apparatus which concerns on 1st embodiment.
- the filtration apparatus Since the filtration apparatus according to the present embodiment has a tank on the upstream side of the filter 103, the liquid to be purified to be circulated through the filter 103 can be retained and homogenized, resulting in more excellent defects. A chemical solution having inhibitory performance is obtained.
- the liquid to be purified is returned to the flow path S4 from the downstream of the filter 103 (filter A) to the upstream of the filter 103 to the flow path S4.
- a tank 401 can be used to receive the liquid to be purified. In this way, since the returned liquid to be purified is retained and homogenized, it can be passed through the filter 103 again, so that a chemical solution having further superior defect suppression performance can be obtained.
- the material of the tank 401 is not particularly limited, but the same material as the housing material described above can be used, and at least a part of the wetted part (preferably 90% or more of the surface area of the wetted part, more preferably 99% or more) is preferably made of a corrosion-resistant material described later.
- FIG. 5 is a schematic diagram showing a modification of the filtration device according to the third embodiment of the present invention.
- the filtration device 500 further includes a tank 401 arranged in series with the filter A between the inflow portion 101 and the outflow portion 102 and on the downstream side of the filter 103 (filter A) on the flow path S5. It is.
- the filter 103 (filter A), the tank 401, and the filter 104 (filter BD) are arranged in series via a pipe 501 and a pipe 502.
- the tank 401 constitutes the flow path S5 together with the above-described filter, piping, and the like.
- each filter and piping is the same as that of the filtration device according to the first embodiment already described, and the following description is limited to only parts different from the first embodiment. Do. Therefore, the matter which is not demonstrated below is the same as that of the filtration apparatus which concerns on 1st embodiment.
- the filtration device Since the filtration device according to this embodiment has a tank on the downstream side of the filter A, the liquid to be purified filtered by the filter A can be retained.
- the liquid to be purified when the liquid to be purified is returned from the downstream side of the filter 103 (filter A) to the flow path S4 to the upstream side of the filter 103 with respect to the flow path S4, the return is returned.
- a tank 401 can be used to retain the liquid to be purified. In this way, since the liquid to be purified to be returned is retained and homogenized, it can be passed through the filter 103 again, so that a chemical solution having further superior defect suppression performance can be obtained.
- the tank 401 is disposed on the upstream side of the filter 104 (filter BD) on the flow passage S5.
- the flow passage S5 is used. It may be arranged on the downstream side of the filter 104 above.
- the tank 401 can be used to retain the liquid to be returned that is to be returned during circulation filtration.
- it can be the base point of the circulation filtration.
- the filter on the upstream side of the tank 401 filter 103 in the filtration device 500
- the filter on the downstream side of the tank 401 filtration
- the filter 1014 is often the object of circulation filtration as a reference filter.
- the base point of the circulation filtration includes both the case where the tank constitutes a return flow passage and the case where the downstream pipe of the tank constitutes a return flow passage.
- the tank 401 is disposed on the upstream side of the filter 104 (filter BD).
- the upstream side or the downstream side of the tank 401 in the flow path S5 can be the target of the circulation filtration.
- the upstream side of the tank 401 is the target of circulation filtration, the intention is that the liquid to be purified that has been sufficiently filtered by the filter A is finally passed through the filter A.
- the flow that removes fine particles mixed in the liquid to be purified without using the filter 104 can be adopted. As a result, the life of the filter BD becomes longer, and a chemical solution having excellent defect suppression performance can be manufactured more stably over a long period of time. is there.
- the filter BU and the filter A are arranged in series in this order (for example, the second embodiment), and the filter BU, the filter A, and the filter BD are in series in this order.
- a tank 401 may be further provided on the upstream side of the filter A.
- FIG. 6 is a schematic view showing a filtration device according to the fourth embodiment of the present invention.
- a filter 601 which is a filter C
- a tank 401
- a filter 103 which is a filter A
- a filter 104 which is a filter BD
- the inflow part 101, the filter 601, the pipe 602, the tank 401, the pipe 402, the filter 103, the pipe 105, the filter 104, and the outflow part 102 form the flow path S6.
- each filter and piping is the same as that of the filtration device according to the first embodiment already described, and the following description is limited to only parts different from the first embodiment. Do. Therefore, the matter which is not demonstrated below is the same as that of the filtration apparatus which concerns on 1st embodiment.
- the filter 601 (filter C) is a filter having a pore diameter of 10 nm or more disposed on the upstream side of the tank 401 in the flow path S6.
- a filter having a predetermined hole diameter is disposed upstream of the tank 401 in the flow passage S6, so that impurities contained in the liquid to be purified that flows in from the inflow portion 101 are preliminarily removed. Since it can be removed using the filter 601, the amount of impurities mixed in the flow path after the pipe 602 can be further reduced. For this reason, the lifetime of the filter A and the filter BD (and the filter BU if the filter BU is disposed) in the subsequent stage can be further extended. As a result, according to the filtration device, it is possible to stably produce a chemical solution having better defect suppression performance.
- the form of the filter C is not particularly limited, and may be the same filter as the filter A already described, or may be a different filter (filter B). Especially, it is preferable that it is a filter (filter B) different from the filter A at the point which can obtain the chemical
- the pore diameter is not particularly limited, and is preferably 10 nm or more, more preferably 20 nm or more, still more preferably more than 50 nm, and particularly preferably 100 nm or more.
- the filter A and the filter BD are arranged in series in this order on the flow path (for example, the second embodiment), and the filter BU, the filter A, and
- a tank is further provided on the downstream side of the filter A, and a filter C is provided on the upstream side of the tank. Good.
- FIG. 7 is a schematic view of a filtration device according to the fifth embodiment of the present invention.
- the filtration device 700 includes an inflow portion 101, an outflow portion 102, a filter 103 that is a filter A, and a filter 104 that is a filter BD.
- the filter 103 and the filter 104 are connected to the inflow portion 101 and the outflow portion 102.
- the inflow portion 101, the filter 103, the pipe 105, the filter 104, and the outflow portion 102 form a flow passage S7.
- each filter and piping is the same as the filtration apparatus according to the first embodiment already described, and the following description is limited to only parts different from the first embodiment. Do. Therefore, the matter which is not demonstrated below is the same as that of the filtration apparatus which concerns on 1st embodiment.
- the filtration device 700 can return the liquid to be purified from the downstream side of the filter 104 (reference filter) in the flow path S7 to the upstream side of the filter 103 (and upstream of the reference filter) in the flow path S7.
- a path R1 is formed.
- the filtration device 700 has a return pipe 701, and the return flow passage R ⁇ b> 1 is formed by the pipe 701.
- One end of the pipe 701 is connected to the flow path S7 on the downstream side of the filter 104 (and the filter 103), and the other end is connected to the flow path S7 on the upstream side of the filter 103.
- a pump, a damper, a valve, and the like may be disposed on the return flow passage R1.
- the liquid to be purified that circulates in the return flow passage R1 and is returned to the upstream side (in the flow passage S7) of the filter 103 is filtered by the filter 103 and the filter 104 in the process of flowing through the flow passage S7 again.
- This is called circulation filtration, and the filtration device 700 can carry out circulation filtration, and as a result, a chemical solution having better defect suppression performance can be easily obtained.
- the liquid to be purified can be returned from the downstream side of the filter 104 (filter BD, reference filter) to the upstream side of filter A (and the filter BD; upstream side of the reference filter) on the flow path S7.
- the piping 701 is disposed, the filtration apparatus according to the present embodiment can return the liquid to be purified from the downstream side of the filter A to the upstream side of the filter A using the filter A as a reference filter on the flow path. It may be configured.
- the return flow passage may be formed by a pipe connecting the pipe 105 and the inflow portion 101.
- the filter A is used as a reference filter, from the downstream side of the reference filter to the upstream side of the filter BU (and the upstream side of the reference filter).
- a return flow path that can return the liquid to be purified may be formed.
- the return flow passage R1 is formed only from the pipe, but it may be formed from one or more tanks and pipes already described.
- FIG. 8 is a schematic diagram illustrating a modification of the filtration device according to the fifth embodiment of the present invention.
- the filtration device 800 includes an inflow portion 101, tanks 401 (a) and 401 (b), an outflow portion 102, a filter 103 that is a filter A, and a filter 104 that is a filter BD.
- the tank 401 (a), The filter 103, the filter 104, and 401 (b) are arranged in series between the inflow portion 101 and the outflow portion 102, and the inflow portion 101, the tank 401 (a), the pipe 802, the filter 103, and the pipe 803.
- the filter 104, the pipe 804, the tank 401 (b), and the outflow portion 102 form a flow passage S8.
- each filter and piping is the same as that of the filtration device according to the first embodiment already described, and the following description is limited to only the parts different from the first embodiment. Do. Therefore, the matter which is not demonstrated below is the same as that of the filtration apparatus which concerns on 1st embodiment.
- the filtration device 800 is upstream of the tank 401 (a) disposed on the upstream side of the filter 103 on the flow path S8 from the downstream side of the tank 401 (b) disposed on the downstream side of the filter 104 on the flow path S8.
- a return flow passage R2 capable of returning the liquid to be purified to the side is formed.
- One end of the pipe 801 is connected to the flow path S8 on the downstream side of the tank 401 (b), and the other end is connected to the flow path S8 on the upstream side of the tank 401 (a).
- a pump, a damper, a valve, and the like may be disposed in the return flow passage R2.
- the base point of the return flow passage R2 is disposed on the downstream side of the tank 401 (b) on the flow passage, and the end point is disposed on the upstream side of the tank 401 (a) on the flow passage.
- the liquid to be purified can be returned after being retained during circulation filtration, and can be recirculated after being retained, resulting in a chemical solution having better defect suppression performance. It is done.
- the form which tank 401 (b) and the piping 801 connect directly may be sufficient, and the form which the tank 401 (a) and the piping 801 connect directly may be sufficient. It may be a form provided with both.
- FIG. 9 is a schematic view of a filtration device according to the fifth embodiment of the present invention.
- the filtration device 900 includes an inflow portion 101, an outflow portion 102, a filter 103 that is a filter A, and a filter 104 that is a filter BD.
- the filter 103 and the filter 104 are connected to the inflow portion 101 and the outflow portion 102.
- a flow passage S9 from the inflow portion 101 to the outflow portion 102 is formed.
- the inflow portion 101, the filter 103, the pipe 105, the filter 104, and the outflow portion 102 form a flow passage S9.
- the filtration device 900 is formed with a return flow path R3 that can return the liquid to be purified from the downstream side of the filter 104 on the flow path S9 to the downstream side of the filter 103 and the upstream side of the filter 104 on the flow path S9.
- the filtration device 900 has a return pipe 901, and a return flow passage R ⁇ b> 3 is formed by the pipe 901.
- One end of the pipe 901 is connected to the flow path S9 on the downstream side of the filter 104, and the other end is connected to the flow path S9 on the upstream side of the filter 104 and the downstream side of the filter 103.
- a pump, a damper, a valve, and the like may be disposed on the return flow passage R3.
- the liquid to be purified that circulates in the return flow path R2 and is returned to the downstream side of the filter 103 and upstream of the filter 104 is filtered by the filter 104 in the process of flowing again through the flow path S9.
- the filtration device 900 can perform circulation filtration, and as a result, a chemical solution having better defect suppression performance can be easily obtained.
- the liquid to be purified is returned from the downstream side of the filter 104 (filter BD) on the flow path S9 to the downstream side of the filter A on the flow path S9 and to the upstream side of the filter BD.
- the pipe 901 is arranged so as to be able to be used, as a filtration device according to the present embodiment, the liquid to be purified is located on the flow path from the downstream side of the filter B to the downstream side of the filter A and upstream of the filter B. As long as it can be returned.
- FIG. 10 is a schematic diagram illustrating a modification of the filtration device according to the present embodiment.
- the filtration apparatus 1000 includes an inflow portion 101, an outflow portion 102, a filter 103 that is a filter A, a filter 104-1 (reference filter) that is a filter BD, and a filter 104-2.
- the filtering device 104-1 and the filter 104-2 are arranged in series between the inflow portion 101 and the outflow portion 102, and have a flow passage S10 extending from the inflow portion 101 to the outflow portion 102.
- the inflow part 101, the filter 103, the pipe 105, the filter 104-1, the pipe 1001, the filter 104-2, and the outflow part 102 form a flow path S10.
- each filter and piping is the same as that of the filtration device according to the first embodiment already described, and the following description is limited to only parts different from the first embodiment. Do. Therefore, the matter which is not demonstrated below is the same as that of the filtration apparatus which concerns on 1st embodiment.
- the filtering device 1000 is located on the flow path S10 from the downstream side of the filter 104-1 (reference filter) to the downstream side of the filter 103 and the upstream side of the filter 104-1 (reference filter) with respect to the flow path S10.
- a return flow passage R4 capable of returning the liquid to be purified is formed.
- the filtration device 1000 has a return pipe 1002, and a return flow passage R ⁇ b> 4 is formed by the pipe 1002.
- One end of the pipe 1002 is connected to the flow path S10 on the downstream side of the filter 103 and upstream of the filter 104-1, and the other end is connected to the flow path S10 on the downstream side of the filter 104-1 and upstream of the filter 104-2.
- a pump, a damper, a valve, and the like may be disposed in the return flow passage R4.
- the liquid to be purified returned to the upstream side of the filter 104-1 on the downstream side of the filter 103 on the flow path S10 by the return flow path R4 is again filtered by the filter 104-1 in the process of flowing through the flow path S10. Filtered.
- circulation filtration can be performed, and as a result, a chemical solution having better defect suppression performance can be easily obtained.
- the flow path R4 is formed, the filtration device according to the present embodiment is not limited to the above, and the liquid to be purified can be returned from the downstream side of the filter 104-2 to the upstream side of the filter 104-2.
- a return flow passage capable of returning the liquid to be purified from the downstream side of the filter 104-2 in which the return flow passage is formed to the downstream side of the filter A and the upstream side of the filter 104-1 is formed.
- a filtration device in which a return flow passage capable of returning from the downstream side of the filter 104-1 or the filter 104-2 to the upstream side of the filter 103 is formed.
- the method for producing a chemical solution according to the embodiment of the present invention is a method for producing a chemical solution by purifying the liquid to be purified to obtain the chemical solution, and the chemical solution is filtered by filtering the liquid to be purified using the filtration device described above. Having a filtration step to obtain.
- [Purified liquid] Although it does not restrict
- the solvent include an organic solvent and water, and it is preferable to contain an organic solvent.
- the water content exceeds 50% by mass with respect to the total mass of the solvent contained in the liquid to be purified.
- Organic solvent-based liquid to be purified contains a solvent, and the content of the organic solvent is 50% by mass or more based on the total mass of the solvent contained in the liquid to be purified.
- the liquid to be purified contains an organic solvent.
- the content of the organic solvent in the liquid to be purified is not particularly limited, but generally 99.0% by mass or more is preferable with respect to the total mass of the liquid to be purified. Although it does not restrict
- An organic solvent may be used individually by 1 type, or may use 2 or more types together. When two or more organic solvents are used in combination, the total content is preferably within the above range.
- the organic solvent intends the liquid organic compound contained with content exceeding 10,000 mass ppm per component with respect to the total mass of the said to-be-purified liquid. That is, in this specification, the liquid organic compound contained exceeding 10,000 mass ppm with respect to the total mass of the liquid to be purified corresponds to the organic solvent.
- the liquid state means a liquid at 25 ° C. and atmospheric pressure.
- the type of the organic solvent is not particularly limited, and a known organic solvent can be used.
- the organic solvent include alkylene glycol monoalkyl ether carboxylate, alkylene glycol monoalkyl ether, alkyl lactate ester, alkyl alkoxypropionate, cyclic lactone (preferably having 4 to 10 carbon atoms), and monoketone which may have a ring. Examples thereof include compounds (preferably having 4 to 10 carbon atoms), alkylene carbonate, alkyl alkoxyacetate, and alkyl pyruvate.
- the organic solvent for example, those described in JP-A-2016-57614, JP-A-2014-219664, JP-A-2016-138219, and JP-A-2015-135379 may be used. Good.
- organic solvents examples include propylene glycol monomethyl ether (PGMM), propylene glycol monoethyl ether (PGME), propylene glycol monopropyl ether (PGMP), propylene glycol monomethyl ether acetate (PGMEA), ethyl lactate (EL), methyl methoxypropionate (MPM), cyclopentanone (CyPn), cyclohexanone (CyHe), ⁇ -butyrolactone ( ⁇ BL), diisoamyl ether (DIAE), butyl acetate (nBA), isoamyl acetate (iAA), isopropanol (IPA), 4-methyl -2-pentanol (MIBC), dimethyl sulfoxide (DMSO), n-methyl-2-pyrrolidone (NMP), diethylene glycol (DEG), ethylene glycol (E G), dipropylene glycol (DPG), propylene glycol (PG), ethylene carbonate (EC), propylene carbonate (
- the kind and content of the organic solvent in the liquid to be purified can be measured using a gas chromatograph mass spectrometer.
- the liquid to be purified may contain components other than those described above.
- examples of other components include inorganic substances (metal ions, metal particles, metal oxide particles, and the like), resins, organic substances other than resins, and water.
- the liquid to be purified may contain an inorganic substance. It does not restrict
- the metal-containing particles only need to contain metal atoms, and the form is not particularly limited.
- a single metal atom, a compound containing a metal atom (hereinafter also referred to as “metal compound”), a complex thereof, and the like can be given.
- the metal-containing particles may contain a plurality of metal atoms.
- the composite is not particularly limited, but a so-called core-shell type particle having a single metal atom and a metal compound covering at least a part of the single metal atom, a solid solution containing a metal atom and another atom Particles, eutectic particles containing metal atoms and other atoms, aggregate particles of simple metal atoms and metal compounds, aggregate particles of different types of metal compounds, and continuous from the particle surface toward the center or Examples thereof include a metal compound whose composition changes intermittently.
- the atom other than the metal atom contained in the metal compound is not particularly limited, and examples thereof include a carbon atom, an oxygen atom, a nitrogen atom, a hydrogen atom, a sulfur atom, and a phosphorus atom.
- the metal-containing particles may contain the above metal atoms alone or in combination of two or more.
- the inorganic substance may be added to the liquid to be purified, or may be unintentionally mixed with the liquid to be purified in the manufacturing process.
- medical solution for example, when an inorganic substance is contained in the raw material (for example, organic solvent) used for manufacture of a chemical
- the liquid to be purified may contain a resin.
- the chemical solution may further contain a resin.
- a resin P having a group that decomposes by the action of an acid to generate a polar group is more preferable.
- the resin is more preferably a resin having a repeating unit represented by the formula (AI) described later, which is a resin whose solubility in a developer containing an organic solvent as a main component is reduced by the action of an acid.
- the resin having a repeating unit represented by the formula (AI) described later has a group (hereinafter also referred to as “acid-decomposable group”) that decomposes by the action of an acid to generate an alkali-soluble group.
- Examples of polar groups include alkali-soluble groups.
- Examples of the alkali-soluble group include a carboxy group, a fluorinated alcohol group (preferably a hexafluoroisopropanol group), a phenolic hydroxyl group, and a sulfo group.
- the polar group is protected by a group capable of leaving by an acid (acid leaving group).
- the acid leaving group include -C (R 36 ) (R 37 ) (R 38 ), -C (R 36 ) (R 37 ) (OR 39 ), and -C (R 01 ) (R 02 ) (OR 39 ) and the like.
- R 36 to R 39 each independently represents an alkyl group, a cycloalkyl group, an aryl group, an aralkyl group or an alkenyl group.
- R 36 and R 37 may be bonded to each other to form a ring.
- R 01 and R 02 each independently represents a hydrogen atom, an alkyl group, a cycloalkyl group, an aryl group, an aralkyl group or an alkenyl group.
- the resin P preferably contains a repeating unit represented by the formula (AI).
- Xa 1 represents a hydrogen atom or an alkyl group which may have a substituent.
- T represents a single bond or a divalent linking group.
- Ra 1 to Ra 3 each independently represents an alkyl group (linear or branched) or a cycloalkyl group (monocyclic or polycyclic). Two of Ra 1 to Ra 3 may combine to form a cycloalkyl group (monocyclic or polycyclic).
- Examples of the alkyl group that may have a substituent represented by Xa 1 include a methyl group and a group represented by —CH 2 —R 11 .
- R 11 represents a halogen atom (fluorine atom or the like), a hydroxyl group, or a monovalent organic group.
- Xa 1 is preferably a hydrogen atom, a methyl group, a trifluoromethyl group or a hydroxymethyl group.
- Examples of the divalent linking group for T include an alkylene group, —COO—Rt— group, —O—Rt— group, and the like.
- Rt represents an alkylene group or a cycloalkylene group.
- T is preferably a single bond or a —COO—Rt— group.
- Rt is preferably an alkylene group having 1 to 5 carbon atoms, more preferably a —CH 2 — group, a — (CH 2 ) 2 — group, or a — (CH 2 ) 3 — group.
- the alkyl group for Ra 1 to Ra 3 is preferably an alkyl group having 1 to 4 carbon atoms.
- Examples of the cycloalkyl group represented by Ra 1 to Ra 3 include a monocyclic cycloalkyl group such as a cyclopentyl group or a cyclohexyl group, or a multicyclic group such as a norbornyl group, a tetracyclodecanyl group, a tetracyclododecanyl group, or an adamantyl group.
- a cyclic cycloalkyl group is preferred.
- the cycloalkyl group formed by combining two of Ra 1 to Ra 3 includes a monocyclic cycloalkyl group such as a cyclopentyl group or a cyclohexyl group, or a norbornyl group, a tetracyclodecanyl group, or a tetracyclododecanyl group. Or a polycyclic cycloalkyl group such as an adamantyl group is preferred. A monocyclic cycloalkyl group having 5 to 6 carbon atoms is more preferable.
- the cycloalkyl group formed by combining two of Ra 1 to Ra 3 is, for example, a group in which one of the methylene groups constituting the ring has a hetero atom such as an oxygen atom or a hetero atom such as a carbonyl group. It may be replaced.
- the repeating unit represented by the formula (AI) preferably has, for example, an embodiment in which Ra 1 is a methyl group or an ethyl group, and Ra 2 and Ra 3 are bonded to form the above-described cycloalkyl group.
- Each of the above groups may have a substituent.
- substituents include an alkyl group (1 to 4 carbon atoms), a halogen atom, a hydroxyl group, an alkoxy group (1 to 4 carbon atoms), a carboxy group, And alkoxycarbonyl groups (having 2 to 6 carbon atoms) and the like, and those having 8 or less carbon atoms are preferred.
- the content of the repeating unit represented by the formula (AI) is preferably from 20 to 90 mol%, more preferably from 25 to 85 mol%, further preferably from 30 to 80 mol%, based on all repeating units in the resin P. preferable.
- the resin P preferably contains a repeating unit Q having a lactone structure.
- the repeating unit Q having a lactone structure preferably has a lactone structure in the side chain, more preferably a repeating unit derived from a (meth) acrylic acid derivative monomer.
- the repeating unit Q having a lactone structure may be used alone or in combination of two or more, but is preferably used alone.
- the content of the repeating unit Q having a lactone structure is preferably from 3 to 80 mol%, more preferably from 3 to 60 mol%, based on all repeating units in the resin P.
- the lactone structure preferably has a repeating unit having a lactone structure represented by any of the following formulas (LC1-1) to (LC1-17).
- a lactone structure represented by formula (LC1-1), formula (LC1-4), formula (LC1-5), or formula (LC1-8) is preferable, and represented by formula (LC1-4).
- the lactone structure is more preferable.
- the lactone structure portion may have a substituent (Rb 2 ).
- Preferred substituents (Rb 2 ) include an alkyl group having 1 to 8 carbon atoms, a cycloalkyl group having 4 to 7 carbon atoms, an alkoxy group having 1 to 8 carbon atoms, an alkoxycarbonyl group having 2 to 8 carbon atoms, and a carboxy group.
- n 2 represents an integer of 0 to 4. When n 2 is 2 or more, a plurality of substituents (Rb 2 ) may be the same or different, and a plurality of substituents (Rb 2 ) may be bonded to form a ring. .
- the resin P may contain a repeating unit having a phenolic hydroxyl group.
- the repeating unit having a phenolic hydroxyl group include repeating units represented by the following general formula (I).
- R 41 , R 42 and R 43 each independently represents a hydrogen atom, an alkyl group, a halogen atom, a cyano group or an alkoxycarbonyl group.
- R 42 may form a ring with Ar 4, R 42 in this case represents a single bond or an alkylene group.
- X 4 represents a single bond, —COO—, or —CONR 64 —, and R 64 represents a hydrogen atom or an alkyl group.
- L 4 represents a single bond or an alkylene group.
- Ar 4 represents an (n + 1) -valent aromatic ring group, and when bonded to R 42 to form a ring, represents an (n + 2) -valent aromatic ring group.
- n represents an integer of 1 to 5.
- alkyl group of R 41 , R 42 and R 43 in the general formula (I) a methyl group, ethyl group, propyl group, isopropyl group, n-butyl group, sec-butyl which may have a substituent Group, hexyl group, 2-ethylhexyl group, octyl group, dodecyl group and the like, preferably an alkyl group having 20 or less carbon atoms, more preferably an alkyl group having 8 or less carbon atoms, and still more preferably an alkyl group having 3 or less carbon atoms.
- the cycloalkyl group of R 41 , R 42 and R 43 in the general formula (I) may be monocyclic or polycyclic.
- the cycloalkyl group is preferably a monocyclic cycloalkyl group having 3 to 8 carbon atoms, such as a cyclopropyl group, a cyclopentyl group and a cyclohexyl group, which may have a substituent.
- Examples of the halogen atom of R 41 , R 42 and R 43 in the general formula (I) include a fluorine atom, a chlorine atom, a bromine atom and an iodine atom, and a fluorine atom is preferable.
- alkyl group contained in the alkoxycarbonyl group of R 41 , R 42 and R 43 in the general formula (I) the same alkyl groups as those described above for R 41 , R 42 and R 43 are preferable.
- each group examples include an alkyl group, a cycloalkyl group, an aryl group, an amino group, an amide group, a ureido group, a urethane group, a hydroxy group, a carboxy group, a halogen atom, an alkoxy group, a thioether group, and an acyl group.
- the substituent preferably has 8 or less carbon atoms.
- Ar 4 represents an (n + 1) -valent aromatic ring group.
- the divalent aromatic ring group when n is 1 may have a substituent, for example, an arylene group having 6 to 18 carbon atoms such as a phenylene group, a tolylene group, a naphthylene group and an anthracenylene group, and , Aromatic ring groups containing heterocycles such as thiophene, furan, pyrrole, benzothiophene, benzofuran, benzopyrrole, triazine, imidazole, benzimidazole, triazole, thiadiazole and thiazole.
- n + 1) -valent aromatic ring group in the case where n is an integer of 2 or more include (n-1) arbitrary hydrogen atoms removed from the above-described specific examples of the divalent aromatic ring group.
- the group formed is mentioned.
- the (n + 1) -valent aromatic ring group may further have a substituent.
- Examples of the substituent that the above-described alkyl group, cycloalkyl group, alkoxycarbonyl group, alkylene group, and (n + 1) -valent aromatic ring group may have include R 41 , R 42, and R 43 in the general formula (I).
- R 64 represents a hydrogen atom or an alkyl group
- the alkyl group for R 64 in, which may have a substituent, a methyl group, an ethyl group, a propyl group, Examples thereof include alkyl groups having 20 or less carbon atoms such as isopropyl group, n-butyl group, sec-butyl group, hexyl group, 2-ethylhexyl group, octyl group and dodecyl group, and alkyl groups having 8 or less carbon atoms are more preferable.
- X 4 is preferably a single bond, —COO— or —CONH—, and more preferably a single bond or —COO—.
- an alkylene group having 1 to 8 carbon atoms such as a methylene group, an ethylene group, a propylene group, a butylene group, a hexylene group and an octylene group which may have a substituent is preferable.
- Ar 4 is preferably an aromatic ring group having 6 to 18 carbon atoms which may have a substituent, and more preferably a benzene ring group, a naphthalene ring group or a biphenylene ring group.
- the repeating unit represented by the general formula (I) preferably has a hydroxystyrene structure. That is, Ar 4 is preferably a benzene ring group.
- the content of the repeating unit having a phenolic hydroxyl group is preferably from 0 to 50 mol%, more preferably from 0 to 45 mol%, still more preferably from 0 to 40 mol%, based on all repeating units in the resin P.
- the resin P may further contain a repeating unit containing an organic group having a polar group, particularly a repeating unit having an alicyclic hydrocarbon structure substituted with a polar group. This improves the substrate adhesion and developer compatibility.
- the alicyclic hydrocarbon structure of the alicyclic hydrocarbon structure substituted with a polar group is preferably an adamantyl group, a diamantyl group or a norbornane group.
- As the polar group a hydroxyl group or a cyano group is preferable.
- the content thereof is preferably 1 to 50 mol% with respect to all repeating units in the resin P, and 1 to 30 mol%. More preferred is 5 to 25 mol%, further preferred is 5 to 20 mol%.
- the resin P may contain a repeating unit represented by the following general formula (VI).
- R 61 , R 62 and R 63 each independently represents a hydrogen atom, an alkyl group, a cycloalkyl group, a halogen atom, a cyano group or an alkoxycarbonyl group.
- R 62 may be bonded to Ar 6 to form a ring, and R 62 in this case represents a single bond or an alkylene group.
- X 6 represents a single bond, —COO—, or —CONR 64 —.
- R 64 represents a hydrogen atom or an alkyl group.
- L 6 represents a single bond or an alkylene group.
- Ar 6 represents an (n + 1) -valent aromatic ring group, and represents an (n + 2) -valent aromatic ring group when bonded to R 62 to form a ring.
- Y 2 independently represents a hydrogen atom or a group capable of leaving by the action of an acid when n ⁇ 2. However, at least one of Y 2 represents a group capable of leaving by the action of an acid.
- n represents an integer of 1 to 4.
- the group Y 2 leaving by the action of an acid is preferably a structure represented by the following general formula (VI-A).
- L 1 and L 2 each independently represent a hydrogen atom, an alkyl group, a cycloalkyl group, an aryl group, or a group in which an alkylene group and an aryl group are combined.
- M represents a single bond or a divalent linking group.
- Q represents an alkyl group, a cycloalkyl group which may contain a hetero atom, an aryl group which may contain a hetero atom, an amino group, an ammonium group, a mercapto group, a cyano group or an aldehyde group. At least two of Q, M, and L 1 may combine to form a ring (preferably a 5-membered or 6-membered ring).
- the repeating unit represented by the general formula (VI) is preferably a repeating unit represented by the following general formula (3).
- Ar 3 represents an aromatic ring group.
- R 3 represents a hydrogen atom, an alkyl group, a cycloalkyl group, an aryl group, an aralkyl group, an alkoxy group, an acyl group, or a heterocyclic group.
- M 3 represents a single bond or a divalent linking group.
- Q 3 represents an alkyl group, a cycloalkyl group, an aryl group or a heterocyclic group. At least two of Q 3 , M 3 and R 3 may be bonded to form a ring.
- the aromatic ring group represented by Ar 3 is the same as Ar 6 in the general formula (VI) when n in the general formula (VI) is 1, and is preferably a phenylene group or a naphthylene group, more preferably a phenylene group. preferable.
- the resin P may further contain a repeating unit having a silicon atom in the side chain.
- the repeating unit having a silicon atom in the side chain include a (meth) acrylate repeating unit having a silicon atom and a vinyl repeating unit having a silicon atom.
- the repeating unit having a silicon atom in the side chain is typically a repeating unit having a group having a silicon atom in the side chain. Examples of the group having a silicon atom include a trimethylsilyl group, a triethylsilyl group, and triphenyl.
- Silyl group tricyclohexylsilyl group, tristrimethylsiloxysilyl group, tristrimethylsilylsilyl group, methylbistrimethylsilylsilyl group, methylbistrimethylsiloxysilyl group, dimethyltrimethylsilylsilyl group, dimethyltrimethylsiloxysilyl group, and the following cyclic groups
- linear polysiloxane, cage-type, ladder-type, or random-type silsesquioxane structures can be used.
- R and R 1 each independently represents a monovalent substituent. * Represents a bond.
- repeating unit having the above group for example, a repeating unit derived from an acrylate compound or a methacrylate compound having the above group or a repeating unit derived from a compound having the above group and a vinyl group is preferable.
- the content thereof is preferably 1 to 30 mol%, more preferably 5 to 25 mol%, based on all repeating units in the resin P. Is more preferably 5 to 20 mol%.
- the weight average molecular weight of the resin P is preferably 1,000 to 200,000, more preferably 3,000 to 20,000, and more preferably 5,000 to 15,000 as a polystyrene conversion value by GPC (Gel permeation chromatography) method. Further preferred.
- GPC Gel permeation chromatography
- the degree of dispersion is usually 1 to 5, preferably 1 to 3, more preferably 1.2 to 3.0, and still more preferably 1.2 to 2.0.
- the water-based liquid to be purified contains more than 50% by mass of water, preferably 50 to 95% by mass, based on the total mass of the solvent contained in the liquid to be purified.
- the water is not particularly limited, it is preferable to use ultrapure water used in semiconductor manufacturing, and it is more preferable to use water with further refinement of the ultrapure water to reduce inorganic anions and metal ions. preferable.
- the purification method is not particularly limited, purification using a filtration membrane or an ion exchange membrane and purification by distillation are preferred. Further, for example, purification is preferably performed by a method described in JP-A-2007-254168.
- the aqueous liquid to be purified may contain an oxidizing agent.
- the oxidizing agent is not particularly limited, and a known oxidizing agent can be used.
- the oxidizing agent include hydrogen peroxide, peroxide, nitric acid, nitrate, iodate, periodate, hypochlorite, chlorite, chlorate, perchlorate, and persulfate.
- examples thereof include salts, dichromates, permanganates, ozone water, silver (II) salts, and iron (III) salts.
- the content of the oxidizing agent is not particularly limited, but is preferably 0.1% by mass or more, and preferably 99.0% by mass or less, based on the total mass of the polishing liquid.
- an oxidizing agent may be used individually by 1 type, or may use 2 or more types together. When using 2 or more types of oxidizing agents together, it is preferable that total content is in the said range.
- the aqueous refining liquid may contain an inorganic acid. It does not restrict
- An inorganic acid may be used individually by 1 type, or may use 2 or more types together. When two or more inorganic acids are used in combination, the total content is preferably within the above range.
- the aqueous purified solution may contain an anticorrosive agent. It does not restrict
- the anticorrosive include 1,2,4-triazole (TAZ), 5-aminotetrazole (ATA), 5-amino-1,3,4-thiadiazole-2-thiol, 3-amino-1H-1,2, , 4 triazole, 3,5-diamino-1,2,4-triazole, tolyltriazole, 3-amino-5-mercapto-1,2,4-triazole, 1-amino-1,2,4-triazole, 1 -Amino-1,2,3-triazole, 1-amino-5-methyl-1,2,3-triazole, 3-mercapto-1,2,4-triazole, 3-isopropyl-1,2,4-triazole , Naphthotriazole, 1H-tetrazole-5-acetic acid, 2-mercaptobenzo
- anticorrosive examples include aliphatic carboxylic acids such as dodecanoic acid, palmitic acid, 2-ethylhexanoic acid, and cyclohexane acid; citric acid, malic acid, oxalic acid, malonic acid, succinic acid, itaconic acid, maleic acid, glycol Acid, mercaptoacetic acid, thioglycolic acid, salicylic acid, sulfosalicylic acid, anthranilic acid, N-methylanthranilic acid, 3-amino-2-naphthoic acid, 1-amino-2-naphthoic acid, 2-amino-1-naphthoic acid Carboxylic acids having chelating ability such as 1-aminoanthraquinone-2-carboxylic acid, tannic acid, and gallic acid;
- the anticorrosive agent includes palm fatty acid salt, castor sulfated oil salt, lauryl sulfate salt, polyoxyalkylene allyl phenyl ether sulfate salt, alkylbenzene sulfonic acid, alkylbenzene sulfonate, alkyl diphenyl ether disulfonate, alkylnaphthalene sulfone.
- Anionic surfactants such as acid salts, dialkylsulfosuccinate salts, isopropyl phosphate, polyoxyethylene alkyl ether phosphate salts, polyoxyethylene allyl phenyl ether phosphate salts; oleylamine acetate, lauryl pyridinium chloride, cetyl pyridinium chloride, lauryl trimethyl ammonium Chloride, stearyltrimethylammonium chloride, behenyltrimethylammonium chloride , Cationic surfactants such as didecyldimethylammonium chloride; coconut alkyldimethylamine oxide, fatty acid amidopropyldimethylamine oxide, alkylpolyaminoethylglycine hydrochloride, amide betaine type active agent, alanine type active agent, lauryl iminodipropionic acid, etc.
- Amphoteric surfactants polyoxyethylene octyl ether, polyoxyethylene decyl ether, polyoxyethylene lauryl ether, polyoxyethylene lauryl amine, polyoxyethylene oleyl amine, polyoxyethylene polystyryl phenyl ether, polyoxyalkylene polystyryl phenyl ether
- Nonionic surfactant of polyoxyalkylene primary alkyl ether or polyoxyalkylene secondary alkyl ether Other polyoxyalkylenes such as diethylene dilaurate, polyoxyethylene laurate, polyoxyethylenated castor oil, polyoxyethylenated hydrogenated castor oil, sorbitan laurate, polyoxyethylene sorbitan laurate, fatty acid diethanolamide, etc.
- Nonionic surfactants Fatty acid alkyl esters such as octyl stearate and trimethylolpropane tridecanoate; Polyether polyols such as polyoxyalkylene butyl ether, polyoxyalkylene oleyl ether and trimethylolpropane tris (polyoxyalkylene) ether should be used You can also. Examples of the commercially available products include New Calgen FS-3PG (manufactured by Takemoto Yushi Co., Ltd.) and Phosten HLP-1 (manufactured by Nikko Chemicals).
- hydrophilic polymer can also be used as an anticorrosive.
- hydrophilic polymers include polyglycols such as polyethylene glycol, alkyl ethers of polyglycols, polysaccharides such as polyvinyl alcohol, polyvinyl pyrrolidone, and alginic acid, carboxylic acid-containing polymers such as polymethacrylic acid, and polyacrylic acid, Examples include polyacrylamide, polymethacrylamide, and polyethyleneimine.
- specific examples of such hydrophilic polymers include water-soluble polymers described in paragraphs 0042 to 0044 of JP2009-88243A and paragraph 0026 of JP2007-194261A.
- a cerium salt can also be used as an anticorrosive.
- the cerium salt is not particularly limited, and a known cerium salt can be used.
- the cerium salt include trivalent cerium salts such as cerium acetate, cerium nitrate, cerium chloride, cerium carbonate, cerium oxalate, and cerium sulfate.
- tetravalent cerium salts include cerium sulfate, cerium ammonium sulfate, cerium ammonium nitrate, diammonium cerium nitrate, and cerium hydroxide.
- the anticorrosive agent may contain a substituted or unsubstituted benzotriazole.
- Suitable substituted benzotriazoles include, but are not limited to, benzotriazoles substituted with alkyl groups, aryl groups, halogen groups, amino groups, nitro groups, alkoxy groups, or hydroxyl groups.
- Substituted benzotriazoles also include those fused with one or more aryl (eg, phenyl) or heteroaryl groups.
- the content of the anticorrosive in the liquid to be purified is preferably adjusted so as to be 0.01 to 5% by mass and adjusted to be 0.05 to 5% by mass with respect to the total mass of the chemical solution. More preferably, the content is adjusted to 0.1 to 3% by mass.
- An anticorrosive agent may be used individually by 1 type, or may use 2 or more types together. When using 2 or more types of anticorrosive agents together, it is preferable that total content is in the said range.
- the aqueous refining liquid may contain an organic solvent. Although it does not restrict
- the content of the organic solvent is preferably 5 to 35% by mass with respect to the total mass of the solvent contained in the liquid to be purified.
- the pH of the liquid to be purified is not particularly limited, but 0 to 9 is preferable and 0 to 7 is more preferable from the viewpoint of obtaining a chemical solution having better defect suppression performance.
- the pH of the liquid to be purified means a value measured by the glass electrode method using the liquid to be purified adjusted to 25 ° C.
- medical solution which concerns on this embodiment has the filtration process of filtering the said to-be-purified liquid using the filtration apparatus already demonstrated, and obtaining a chemical
- the said filtration apparatus has the flow path formed by arrange
- the supply pressure of the liquid to be purified to each filter is not particularly limited, but generally 0.00010 to 1.0 MPa is preferable.
- the supply pressure P 2 is preferably 0.00050 to 0.090 MPa, more preferably 0.0010 to 0.050 MPa, and more preferably 0.0050 to 0 in that a chemical having superior defect suppression performance can be obtained. .040 MPa is more preferable.
- the filtration pressure affects the filtration accuracy, it is preferable that the pressure pulsation during filtration be as small as possible.
- the filtration rate particularly limited, a more excellent defect suppression performance that easily obtained chemical having, preferably 1.0 L / min / m 2 or more, 0.75 L / min / m 2 or more, and 0 More preferably, it is 6 L / min / m 2 or more.
- the filter is set with a differential pressure resistance that ensures filter performance (the filter is not broken). If this value is large, the filtration speed can be increased by increasing the filtration pressure. That is, the upper limit of the filtration rate usually depends on the differential pressure resistance of the filter, but is usually preferably 10.0 L / min / m 2 or less.
- the temperature at which the liquid to be purified is passed through the filter is not particularly limited, but is generally less than room temperature.
- a filtration process in a clean environment. Specifically, it is preferably performed in a clean room that satisfies Class 1000 (Fed. Std. 209E) of Class 1000 (Class 6 in ISO 14644-1: 2015), and a clean room that satisfies Class 100 (Class 5 in ISO 14644-1: 2015). Is more preferable, and a clean room satisfying Class 10 (Class 4 in ISO 14644-1: 2015) is more preferable, and has a cleanliness level (Class 2 or Class 1) of Class 1 (Class 3 in ISO 14644-1: 2015) or higher A clean room is particularly preferred. In addition, it is preferable to implement each process mentioned later in the said clean environment.
- the filtration step may be a circulation filtration step.
- the circulation filtration step is a step of filtering the liquid to be purified with at least the filter A, returning the liquid to be purified after filtering with the filter A to the upstream of the filter A with respect to the flow path, and filtering again with the filter A.
- the number of circulating filtrations is not particularly limited, but is generally preferably 1 to 10 times.
- the circulating liquid may be returned upstream of the filter A. At this time, the return flow is repeated so that the filtration by at least one filter B in addition to the filter A is also repeated. You may adjust the road.
- medical solution which concerns on this embodiment may have processes other than the above.
- Examples of the process other than the above include a filter cleaning process, an apparatus cleaning process, a charge removal process, and a liquid preparation process. Below, each process is explained in full detail.
- the filter cleaning process is a process of cleaning the filter A and the filter B before the filtration process. Although it does not restrict
- Examples of the method of immersing the filter in the immersion liquid include a method of filling the immersion container with the immersion liquid and immersing the filter in the immersion liquid.
- the immersion liquid preferably contains water or an organic solvent as a main component, and more preferably contains an organic solvent as a main component, in that a more excellent effect of the present invention can be obtained.
- a main component means the component contained 99.9 mass% or more with respect to the total mass of immersion liquid, and it is more preferable to contain 99.99 mass% or more.
- the organic solvent is not particularly limited, and the organic solvents described above can be used as the organic solvent contained in the liquid to be purified.
- the cleaning liquid preferably contains at least one organic solvent selected from the group consisting of ester solvents and ketone solvents in that the effects of the present invention can be obtained. These may be used in combination.
- ester solvent examples include ethyl acetate, methyl acetate, butyl acetate, sec-butyl acetate, methoxybutyl acetate, amyl acetate, normal propyl acetate, isopropyl acetate, ethyl lactate, methyl lactate, and butyl lactate.
- ketone solvent examples include, but are not limited to, acetone, 2-heptanone (MAK), methyl ethyl ketone (MEK), methyl isobutyl ketone, diisobutyl ketone, cyclohexanone, diacetone alcohol and the like.
- the time for immersing the filter in the immersion liquid is not particularly limited, but is preferably 7 days to 1 year from the standpoint that more excellent effects of the present invention can be obtained. Although it does not restrict
- Examples of the method for immersing the filter in the immersion liquid include a method in which the immersion container is filled with the immersion liquid and the filter is immersed in the immersion liquid.
- the housing of the filter unit can be used in the filtration apparatus already described. That is, a method of filling a dipping solution in the housing in a state in which a filter (typically a filter cartridge) is housed in a housing included in the filtration device, and allowing to stand in that state.
- an immersion container is prepared separately from the housing of the purification apparatus (that is, the immersion container is prepared outside the purification apparatus), the immersion container prepared separately is filled with the immersion liquid, and the filter is attached.
- the method of immersing is also mentioned. Especially, the method which fills immersion liquid in the container for immersion prepared outside the filtration apparatus, and immerses a filter in the said immersion liquid by the point which the impurity eluted from the filter does not mix in a filtration apparatus is preferable.
- the shape, size, and the like of the immersion container can be appropriately selected depending on the number and size of the filters to be immersed, and are not particularly limited.
- the material for the immersion container is not particularly limited, but it is preferable that at least the liquid contact portion is formed of the corrosion-resistant material described above.
- polyfluorocarbon PTFE, PFA: perfluoroalkoxyalkane and PCTFE: polychlorotrifluoroethylene, etc.
- PPS polyphenylene sulfide
- POM polyoxymethylene
- PP, PE, etc. PP, PE, etc.
- PPS polyphenylene sulfide
- POM polyoxymethylene
- PP polyfluorocarbon
- PPS polyphenylene sulfide
- POM polyoxymethylene
- Method of cleaning by passing the cleaning solution through the filter There is no particular limitation on the method of cleaning by passing the cleaning liquid through the filter.
- a filter typically a filter cartridge
- the filter housing is installed in the filter housing.
- the cleaning liquid once passed through the filter is not used again for cleaning but is discharged out of the filtration device. In other words, it is preferable not to circulate and wash.
- the cleaning device means a device different from the filtration device provided outside the filtration device.
- limit especially as a form of a washing
- the apparatus of the structure similar to a filtration apparatus can be used.
- the cleaning liquid is not particularly limited, and a known cleaning liquid can be used. Especially, it is preferable that it is the same as that of the immersion liquid already demonstrated as a form of a washing
- the device cleaning step is a step of cleaning the wetted part of the filtration device before the filtration step.
- the method for washing the wetted part of the filtration device before the filtration step is not particularly limited, but in the following, the filter is a cartridge filter, and the cartridge filter is housed in a housing disposed on the flow path.
- the apparatus will be described as an example.
- the liquid contact part of the filtration apparatus is cleaned using the cleaning liquid, and after the process A, the cartridge filter is accommodated in the housing, and the cleaning liquid is further used. It is preferable to have the process B which wash
- Step A is a step of cleaning the liquid contact portion of the filtration device using the cleaning liquid in a state where the cartridge filter is removed from the housing.
- “With the filter removed from the housing” means to remove the filter cartridge from the housing or to wash the wetted part of the filtration device with the washing liquid before storing the filter cartridge in the housing.
- the method of cleaning the liquid contact portion of the filtration device with the filter removed from the housing (hereinafter also referred to as “no filter stored”) using the cleaning liquid is not particularly limited. A method of introducing the cleaning liquid from the inflow part and recovering from the outflow part is mentioned.
- a method of cleaning the wetted part of the filter device not containing the filter using the cleaning liquid in that a more excellent effect of the present invention can be obtained a method of filling the inside of the filter device not containing the filter with the cleaning liquid Is mentioned.
- the liquid contact portion of the filtration apparatus not containing the filter comes into contact with the cleaning liquid.
- the impurities adhering to the wetted part of the filtration device are transferred (typically eluted) to the cleaning liquid.
- cleaning should just be discharged
- the cleaning liquid is not particularly limited, and a known cleaning liquid can be used.
- the cleaning liquid preferably contains water or an organic solvent as a main component, and more preferably contains an organic solvent as a main component, in that a more excellent effect of the present invention can be obtained.
- a main component means the component contained 99.9 mass% or more with respect to the total mass of a washing
- the organic solvent is not particularly limited, and the water and organic solvents already described as the organic solvent contained in the chemical solution can be used.
- the organic solvent PGMEA, cyclohexanone, ethyl lactate, butyl acetate, MIBC, MMP (3-methylmethoxypropionate), MAK, n-pentyl acetate, ethylene glycol can be obtained because the effects of the present invention are more excellent.
- ⁇ Process B is a method of cleaning the filtration device using a cleaning liquid in a state where the filter is housed in the housing.
- a method for washing the filtration device using the washing liquid in addition to the washing method in Step A already described, a method for passing the washing liquid through the filtration device can also be used.
- the method for passing the cleaning liquid through the filtration device is not particularly limited, but the cleaning liquid may be introduced from the inflow portion and discharged from the outflow portion. In addition, it does not restrict
- the neutralization step is a step of reducing the charged potential of the liquid to be purified by neutralizing the liquid to be purified.
- the static elimination method is not particularly limited, and a known static elimination method can be used.
- Examples of the static elimination method include a method in which a liquid to be purified is brought into contact with a conductive material.
- the contact time for contacting the liquid to be purified with the conductive material is preferably 0.001 to 60 seconds, more preferably 0.001 to 1 second, and still more preferably 0.01 to 0.1 seconds.
- the conductive material include stainless steel, gold, platinum, diamond, and glassy carbon.
- Examples of the method of bringing the liquid to be purified into contact with the conductive material include a method in which a grounded mesh made of a conductive material is disposed so as to cross the flow path and the liquid to be purified is circulated therethrough.
- the to-be-purified liquid preparation step is a step for preparing the to-be-purified liquid to be introduced from the inflow portion of the filtration device.
- the method for preparing the liquid to be purified is not particularly limited. Typically, a method for purchasing a commercially available product (for example, a so-called “high purity grade product”), a method obtained by reacting one or more raw materials, and dissolving each component in a solvent Methods and the like.
- the method for obtaining the liquid to be purified (typically the liquid to be purified containing an organic solvent) by reacting the raw materials is not particularly limited, and a known method can be used.
- a method of obtaining a liquid to be purified containing an organic solvent by reacting one or two or more raw materials in the presence of a catalyst.
- a method of reacting acetic acid and n-butanol in the presence of sulfuric acid to obtain butyl acetate reaction of ethylene, oxygen, and water in the presence of Al (C 2 H 5 ) 3 To obtain 1-hexanol; a method in which cis-4-methyl-2-pentene is reacted in the presence of Ipc 2 BH (Diisopinocalyphenylborane) to obtain 4-methyl-2-pentanol; propylene oxide, methanol, and A method of reacting acetic acid in the presence of sulfuric acid to obtain PGMEA (propylene glycol 1-monomethyl ether 2-acetate); reacting acetone and hydrogen in the presence of copper oxide-zinc oxide-aluminum oxide to obtain IPA (Isopropyl alcohol): a reaction between lactic acid and ethanol to produce milk And the like; a method of obtaining ethyl.
- PGMEA propylene glycol 1-monomethyl ether 2-a
- this step may have a preliminary purification step of purifying in advance before the liquid to be purified flows into the filtration device.
- a preliminary purification step of purifying in advance before the liquid to be purified flows into the filtration device.
- the method for purifying the liquid to be purified using the distillation apparatus is not particularly limited.
- the liquid to be purified is purified by previously purifying the liquid to be purified using a distillation apparatus prepared separately from the filtration apparatus. Obtained, stored in a portable tank, transported to a filtration device and introduced, and a method using a purification device described later.
- FIG. 11 is a schematic diagram showing the relationship between each apparatus when a chemical solution is produced using a distilled liquid to be purified that has been purified in advance by a distiller.
- the form of the filtration apparatus 400 is the same as that of the filtration apparatus which concerns on 3rd embodiment of this invention already demonstrated, description is abbreviate
- a filtration device 400 and a distillation device 1101 are disposed in the chemical manufacturing site 1100.
- the distillation apparatus 1101 includes a tank 401 (a), a distiller 1102, and a portable tank 1103, which are connected by a pipe 1104 and a pipe 1105, respectively, and the tank 401 (a) pipe 1104 and a distiller 1102.
- the flow path S11 is formed by the pipe 1105 and the portable tank 1103.
- the form of the tank 401 (a) and each pipe is not particularly limited, and tanks and pipes having the same form as those described as the tank and the pipe included in the filtration device according to the embodiment of the present invention can be used.
- the form of the distiller 1102 can use the same distiller as the distiller which the refiner
- the liquid to be purified introduced into the tank 401 (a) is distilled by the distiller 1102, and the obtained liquid to be purified is stored in the portable tank 1103.
- the form of the portable tank is not particularly limited, but at least a part of the wetted part (preferably 90% or more of the surface area of the wetted part, more preferably 99% or more of the surface area of the wetted part) will be described later. It is preferable to consist of materials.
- the distilled liquid to be purified once stored in the portable tank 1103 is conveyed by the transport means 1106 (the flow of F1 in FIG. 11), and then the distilled liquid to be purified is filtered from the inflow portion 101 of the filtration device. Introduced into the apparatus 400.
- FIG. 11 demonstrated the form in which the distillation apparatus and the filtration apparatus are arrange
- the purification apparatus used in this step is a purification apparatus having the filtration apparatus already described.
- purifier which concerns on embodiment of this invention was arrange
- purifier is demonstrated, showing drawings.
- the content regarding the structure of a filtration apparatus is the same as the content already demonstrated, and description is abbreviate
- FIG. 12 is a schematic diagram showing 1st embodiment of the refiner
- the purification apparatus 1200 includes a second inflow portion 1201, a second outflow portion 1202, and a distiller 1203 disposed between the second inflow portion 1201 and the second outflow portion 1202.
- the 2nd outflow part 1202 is connected with the inflow part 101 which a filtration apparatus has.
- the second inflow part 1201, the distiller 1203, the second outflow part 1202 the inflow part 101, the filter 103 (filter A), the pipe 105, the filter 104 (filter BD), and the outflow A flow passage S12 is formed by the portion 102. That is, the distiller 1203 is connected to the inflow portion 101 of the filtration device 100.
- the liquid to be purified that has flowed into the purification device 1200 from the second inflow portion 1201 is distilled in the distiller 1203 and then introduced from the inflow portion 101 to the filtration device 100 via the second outflow portion 1202. .
- the next step filtration step
- the next step can be carried out without taking the distilled liquid to be purified out of the device, so that a chemical solution having better defect suppression performance can be obtained.
- the form of the distiller 1203 is not particularly limited, and a known distiller (for example, a distillation column) can be used.
- a known distiller for example, a distillation column
- the material similar to that of the housing already described can be used as the material of the distiller 1203.
- the distiller is not particularly limited, and a known distiller can be used.
- the distiller may be a batch type or a continuous type, but a continuous type is preferred.
- the distiller may have a filler inside.
- the form of the filling is not particularly limited, but at least a part of the wetted part is preferably made of a corrosion-resistant material described later, and 90% or more of the area of the wetted part is preferably made of a corrosion-resistant material, More preferably, 99% of the area of the wetted part is made of a corrosion-resistant material.
- the purification device 1200 there is a filtering device in a form (for example, the first embodiment of the filtering device) in which a filter A and a filter BD are arranged in series in this order between the inflow portion and the outflow portion.
- the filter device and the inflow portion and the outflow portion in the form in which the filter BU and the filter A are arranged in series in this order between the inflow portion and the outflow portion.
- positioned in series in this order may be provided.
- the purifying apparatus has a flow path S12 formed by the second inflow portion 1201, the distiller 1203, the second outflow portion 1202, the inflow portion 101, the filter 103, the pipe 105, the filter 104, and the outflow portion 102.
- a return flow path capable of returning the liquid to be purified may be formed from the downstream side of the filter 103 (filter A) to the upstream side of the filter 103 (filter A) on the flow path S120.
- limit especially as a form of a return flow path it is the same as that of having demonstrated in 5th embodiment of the filtration apparatus. Further, the form of the return flow passage may be the same as that described in the sixth embodiment of the filtration device.
- the purification apparatus may have a tank on the upstream side and / or the downstream side of the filter 103 on the flow path S12.
- the form of the tank is not particularly limited, and the same tank as described above can be used.
- FIG. 13 is a schematic diagram showing a second embodiment of the purification apparatus.
- the purifier 1300 includes a second inflow portion 1301, a second outflow portion 1302, and a distiller 1303 and a distiller 1304 arranged in series between the second inflow portion 1301 and the second outflow portion 1302.
- the second outflow part 1302 is connected to the inflow part 101 of the filtration device.
- purifier 1300 the 2nd inflow part 1301, the distiller 1303, the piping 1305, the distiller 1304, the 2nd outflow part 1302, the inflow part 101, the filter 103 (filter A), the piping 105, the filter 104 ( A flow passage S13 is formed by the filter BD) and the outflow portion 102.
- purifier which concerns on this embodiment contains the some distiller connected in series.
- the last-stage distiller is connected with a filtration apparatus.
- the liquid to be purified that has flowed from the second inflow portion 1301 is distilled by the distiller 1303, flows through the pipe 1305, and is introduced into the distiller 1304.
- FIG. 13 shows a form in which a distiller 1303 and a distiller 1304 are connected by a pipe 1305, but the purification apparatus according to the present embodiment is not limited to the above, and the condensate of the distiller 1304 is used as a purification apparatus. You may have separately the piping which can be returned to the distiller 1303 again.
- the liquid to be purified contains two or more compounds having different boiling points by appropriately controlling the operating conditions of the two distillers. Even so, the target compound (chemical solution) can be purified with higher purity.
- the corrosion resistant material will be described.
- at least a part of the wetted part is formed of a corrosion-resistant material, and 90% or more of the wetted part is resistant to corrosion. More preferably, it is made of a corrosive material, and more preferably 99% or more of the wetted part is made of a corrosion-resistant material.
- each member for example, the tank described above
- each The member includes a base material and a coating layer disposed on the base material, and the coating layer is formed of a corrosion-resistant material.
- Corrosion resistant materials are non-metallic materials and electropolished metallic materials.
- the non-metallic material is not particularly limited.
- the metal material whose sum total of Cr and Ni content is more than 25 mass% with respect to the metal material total mass is mentioned, Especially, 30 mass% or more is more. preferable.
- the upper limit of the total content of Cr and Ni in the metal material is not particularly limited, but generally 90% by mass or less is preferable.
- the metal material include stainless steel and Ni—Cr alloy.
- Stainless steel is not particularly limited, and known stainless steel can be used. Especially, the alloy containing 8 mass% or more of Ni is preferable, and the austenitic stainless steel containing 8 mass% or more of Ni is more preferable.
- austenitic stainless steel for example, SUS (Steel Use Stainless) 304 (Ni content 8 mass%, Cr content 18 mass%), SUS304L (Ni content 9 mass%, Cr content 18 mass%), SUS316 ( Ni content 10 mass%, Cr content 16 mass%), SUS316L (Ni content 12 mass%, Cr content 16 mass%), etc. are mentioned.
- the Ni—Cr alloy is not particularly limited, and a known Ni—Cr alloy can be used. Among these, a NiCr alloy having a Ni content of 40 to 75% by mass and a Cr content of 1 to 30% by mass is preferable.
- the Ni—Cr alloy include Hastelloy (trade name, the same applies hereinafter), Monel (trade name, the same applies hereinafter), Inconel (product name, the same applies hereinafter), and the like. More specifically, Hastelloy C-276 (Ni content 63 mass%, Cr content 16 mass%), Hastelloy-C (Ni content 60 mass%, Cr content 17 mass%), Hastelloy C-22 ( Ni content 61 mass%, Cr content 22 mass%) etc. are mentioned. Further, the Ni—Cr alloy may further contain B, Si, W, Mo, Cu, Co, etc. in addition to the above-described alloy, if necessary.
- the method for electropolishing the metal material is not particularly limited, and a known method can be used.
- a known method can be used.
- the methods described in JP-A-2015-227501, paragraphs 0011 to 0014, JP-A-2008-264929, paragraphs 0036 to 0042, and the like can be used.
- the metal material is electropolished so that the Cr content in the surface passive layer is higher than the Cr content in the parent phase. For this reason, it is presumed that metal impurities containing metal atoms are unlikely to flow out in the liquid to be purified when a refining device in which the wetted part is formed from a metal material that has been electropolished.
- the metal material may be buffed.
- the buffing method is not particularly limited, and a known method can be used.
- the size of the abrasive grains used for buffing finishing is not particularly limited, but is preferably # 400 or less in that the unevenness on the surface of the metal material tends to be smaller.
- the buffing is preferably performed before the electrolytic polishing.
- the method for producing a chemical liquid according to the second embodiment of the present invention is a method for producing a chemical liquid by purifying the liquid to be purified to obtain the chemical liquid, and the liquid to be purified is a porous substrate made of polytetrafluoroethylene.
- a first porous membrane having a non-crosslinked coating containing a perfluorosulfonic acid polymer formed to cover at least a portion of the substrate, and containing polytetrafluoroethylene blended with the perfluorosulfonic acid polymer A method for producing a chemical solution, comprising a step of filtering using a filter A containing at least one selected from the group consisting of a second porous membrane, and a filter B different from the filter A to obtain a chemical solution is there.
- the liquid to be purified is filtered using a filter B that is different from the filter A and the filter A.
- the filter A and the filter B may be passed in this order, or the filter B and the filter A may be passed in this order.
- a to-be-purified liquid is used using the several filter A and / or the several filter B in order. May be filtered.
- the form of filter B is not particularly limited, but the filter described as filter BU is preferably used. Further, when the filter A and the filter B are used in this order, the form of the filter B is not particularly limited, but the filter described as the filter BD is preferably used.
- the chemical solution produced using the filtration device is preferably used for the production of a semiconductor substrate.
- it is more preferably used for forming a fine pattern having a node of 10 nm or less (for example, a process including pattern formation using EUV).
- the filtration device is preferably used for the production of a chemical solution for the production of a semiconductor substrate.
- the filtration device includes a lithography process, an etching process, an ion implantation process, a peeling process, and the like. In the manufacturing process, it is used to treat inorganic substances and / or organic substances after completion of each process or before moving to the next process.
- a cleaning liquid, an etching liquid, a rinsing liquid, and a pretreatment liquid are used. More preferably, it is used for the production of a resist solution, a pre-wet solution, a developer, etc., and at least one selected from the group consisting of a cleaning solution, an etching solution, a rinse solution, a pretreatment solution, and a resist solution. It is preferably used for production.
- the said filtration apparatus can be used also for manufacture of the chemical
- the said filtration apparatus can be used also for manufacture of the chemical
- the said filtration apparatus for at least 1 sort (s) of production selected from the group which consists of a prewetting liquid, a developing solution, and a rinse liquid in the pattern formation using EUV (extreme ultraviolet rays).
- the chemical produced by the filtration device may be stored in a container and stored until use. Such a container and the chemical solution contained in the container are collectively referred to as a chemical solution container. From the stored chemical solution container, the chemical solution is taken out and used.
- a container having a high cleanliness in the container and for preventing impurities from being eluted from the chemical solution during storage is preferable for manufacturing a semiconductor substrate.
- limit especially as a container which can be used,
- the "clean bottle” series by Aicero Chemical Co., Ltd., the “pure bottle” by Kodama resin industry, etc. are mentioned, However, It is not restrict
- a multi-layer bottle having a six-layer structure with six kinds of resin on the inner wall of the container or a multi-layer bottle having a seven-layer structure with six kinds of resins is used. It is also preferable. Examples of these containers include containers described in JP-A-2015-123351.
- At least a part of the wetted part of the container is made of the corrosion-resistant material already described. It is preferable that 90% or more of the area of the liquid contact portion is made of the above material in that a more excellent effect of the present invention can be obtained.
- the chemical solution 1 was produced using the purification apparatus described in FIG. 14 includes a filter BU-1, a tank T-1, a filter BU-2, a filter FA, a tank T-2, a filter BD-1, and a filter BD between an inflow portion and an outflow portion.
- -2 is a filtration device connected in series, and a distiller connected in front of the filtration device (D1 and D2 double distillers, described as “Dual Duplex” in Table 1).
- Each unit forms a flow path S-14 together with the piping, and from the downstream side of the filter FA (filter FA corresponds to the filter A already described) to the tank T-1 in the flow path S-14.
- a return flow path R-14-1 capable of returning the liquid to be purified is formed, and a return flow capable of returning the liquid to be purified from the downstream side of the filter BD-2 to the tank T-2 in the flow path S-14.
- a flow path R-14-2 is formed.
- Table 1 shows the material components and pore diameters contained in each filter used in the production of the chemical solution 1.
- PFSA / PTFE Commercially available Entegris, Inc. , Fluoroguard AT (pore size 20 nm or 200 nm) was immersed in a polymer solution prepared in an aqueous methanol solution until a 0.25% PFSA solution (Aquivion PFSA 24: D83-24B Solvay Plastics) was sufficiently wetted. Drained, then dried and washed with ultrapure water for 24 hours. The critical wet surface tension of the filter was adjusted by controlling the content of PFSA in the PFSA solution.
- Polypropylene-IEX Filter obtained by introducing a cation exchange group into a polyethylene base material-Nylon: Nylon-UPE: Ultra high molecular weight polyethylene-PTFE: Polytetrafluoroethylene-PFSA / PTFE blend PFSA Additives (Aquivion PFSA 24: D83-24B Solvay Plastics) are mixed with an appropriate amount of PTFE resin, equilibrated, and then pressurized to create billets, and extrusion to form sheet-like PTFE, resulting in a predetermined pore size. It was obtained by stretching. The critical wet surface tension of the filter was adjusted by controlling the amount of the PFSA additive.
- the liquid to be purified commercially available high-purity grade “cyclohexanone” was purchased and purified using the above purification apparatus.
- the chemical solution 1 was obtained by circulating and filtering three times for each return flow passage using the return flow passages R-14-1 and R-14-2.
- each product to be purified described in Table 1 was purified to obtain a chemical solution.
- Each purification device (or filtration device) is shown in FIGS.
- the material components and the pore diameters of the filter FA, the filters BU-1 to BU-3, and the filters BD-1 to BD-2 are as shown in Table 1.
- R- number
- Table 1 shows the critical wet surface tension (CWST) of the filter FA.
- “-” means that the filter was not used, and the same applies to other tables in the present specification.
- the number of defects was 30 / wafer or less. A The number of defects exceeded 30 / wafer and was 50 / wafer or less. B The number of defects exceeded 50 / wafer and was 100 / wafer or less. C The number of defects exceeded 100 / wafer and was 200 / wafer or less. D The number of defects exceeded 200 / wafer and was 500 / wafer or less. E The number of defects exceeded 500 / wafer.
- the resist resin composition was obtained by mixing the following components.
- Acid-decomposable resin represented by the following formula (weight average molecular weight (Mw) 7500): the numerical value described in each repeating unit means mol%): 100 parts by mass
- Quencher shown below 5 parts by mass (mass ratio was 0.1: 0.3: 0.3: 0.2 in order from the left).
- the polymer type has a weight average molecular weight (Mw) of 5000.
- the numerical value described in each repeating unit means molar ratio.
- Hydrophobic resin shown below: 4 parts by mass (mass ratio is (1) :( 2) 0.5: 0.5) Of the following hydrophobic resins, the hydrophobicity of the formula (1) The weight average molecular weight (Mw) of the functional resin is 7000, and the weight average molecular weight (Mw) of the hydrophobic resin of the formula (2) is 8,000. In each hydrophobic resin, the numerical value described in each repeating unit means a molar ratio.
- test method Next, the test method will be described. First, a silicon wafer of about 300 mm was pre-wetted with the chemical solution 1, and then the resist resin composition was spin-coated on the pre-wet silicon wafer. Thereafter, the substrate was heated and dried at 150 ° C. for 90 seconds on a hot plate to form a resist film having a thickness of 9 ⁇ m. With respect to this resist film, an ArF excimer laser scanner (manufactured by ASML, through a mask having a line and space pattern such that the line width of the pattern formed after reduction projection exposure and development is 30 nm and the space width is 30 nm.
- ASML ArF excimer laser scanner
- the number of AA bridge defects was less than 1 / cm 2 .
- a The number of bridge defects was 1 / cm 2 or more and less than 2 / cm 2 .
- B The number of bridge defects was 2 / cm 2 or more and less than 5 / cm 2 .
- C The number of bridge defects was 5 / cm 2 or more and less than 10 / cm 2 .
- D The number of bridge defects was 10 / cm 2 or more and less than 15 / cm 2 .
- E The number of bridge defects was 15 / cm 2 or more.
- the difference between the average value of AA line width and the maximum (minimum) was less than ⁇ 2% with respect to the average value.
- a The difference between the average value of the line width and the maximum (minimum) was less than ⁇ 5% with respect to the average value.
- the difference between the average value of B line width and the maximum (minimum) was less than ⁇ 10% with respect to the average value.
- the difference between the average value of the C line width and the maximum (minimum) was less than ⁇ 20% with respect to the average value.
- the difference between the average value of D line width and the maximum (minimum) was ⁇ 20% or more with respect to the average value. E Shots that cannot be measured for line width were included.
- AA Life span was more than 10 times.
- a Life span was 5 times or more and less than 10 times.
- B Life span was 2 times or more and less than 5 times.
- C Life span was more than 1 time and less than 2 times.
- D Life was less than 1 time.
- Table 2 shows the material components and pore diameters contained in each filter in the filtration device of FIG. Note that the abbreviations relating to the material components of the filter in Table 2 are the same as those in Table 1, and a description thereof is omitted.
- a The number of metal defects / residue defects was 1.5% or less.
- B The number of metal defects / the number of residual defects exceeded 1.5% and was 2.0% or less.
- the resist resin composition 2 is a mixture of the following components.
- the resin synthesis method is simplified.
- Acid diffusion control agent shown below: 0.03g
- a chemical solution 60 was produced using the filtration device described in FIG.
- a filter BU-1, a filter BU-2, a filter BU-3, a filter FA, and a filter BD-2 are connected in series between the inflow portion and the outflow portion.
- Each unit forms a flow passage S-30 with the pipe.
- Table 3 shows the material components and pore sizes contained in each filter used for the purification of the chemical solution 60.
- a chemical solution 61 and a chemical solution 62 were produced in the same manner as the chemical solution 60 except that each filter described in Table 3 was used.
- a chemical solution 63 was produced in the same manner as the chemical solution 60 except that the filtration device shown in FIG. 29 was used instead of the filtration device shown in FIG. In addition, the filter used for filtration is as having described in Table 3.
- the resist resin composition was spin-coated on a silicon wafer of about 300 mm. Then, it was dried by heating at 120 ° C. for 60 seconds on a hot plate to form a resist film having a thickness of 40 nm.
- an EUV exposure apparatus Micro Exposure Tool, manufactured by Exitech, NA 0.3, Quadrupole, outer sigma 0.68, inner sigma 0.36
- a silicon wafer provided with the exposed resist film was placed on a heated hot plate with the silicon wafer surface facing down, and baked at 90 ° C. for 60 seconds.
- the resist film after baking was subjected to paddle development with a developer for 30 seconds and then rinsed.
- the wafer was rotated at a rotational speed of 2000 rpm for 30 seconds to obtain a 1: 1 line and space pattern.
- the number of AA scum defects was less than 1 / cm 2 .
- a The number of scum defects was 1 / cm 2 or more and less than 2 / cm 2 .
- B The number of scum defects was 2 / cm 2 or more and less than 5 / cm 2 .
- C The number of scum defects was 5 / cm 2 or more and less than 10 / cm 2 .
- D The number of scum defects was 10 / cm 2 or more and less than 20 / cm 2 .
- E The number of scum defects was 20 / cm 2 or more.
- Table 1 is divided into a first group: Table 1 (1-1) to Table 1 (1-4) and a second group: Table 1 (2-1) to Table 1 (2-4).
- Table 1 describes the filter of the filtration device (or purification device) used for purification of each chemical solution and the evaluation result of the obtained chemical solution over the corresponding rows of the four contingency tables of each group.
- chemical solution 1 is described in the first line of each of the first group of Table 1: Table 1 (1-1) to Table 1 (1-4). This indicates that the chemical liquid 1 was manufactured by the purification apparatus described in FIG. 14, and that the liquid to be purified used for manufacturing the chemical liquid 1 contains CHN (cyclohexanone).
- medical solution 1 was wash
- the purification apparatus includes a double-type distiller, BU-1 (a filter having a pore diameter of 200 nm containing PP arranged on the most upstream side of the flow passage), and BU-2 (located on the downstream side of BU-1).
- BU-1 a filter having a pore diameter of 200 nm containing PP arranged on the most upstream side of the flow passage
- BU-2 located on the downstream side of BU-1).
- a tank TU-1 on the upstream side of the filter A (FA), and the FA (filter A) is a PFSA / PTFE filter having a pore diameter of 20 nm.
- the CWST is 35 ⁇ 10 ⁇ 5 N / cm
- downstream of the filter FA is BD-1 (a filter with nylon having a pore diameter of 10 nm) and BD-2 (containing UPE).
- BD-1 a filter with nylon having a pore diameter of 10 nm
- BD-2 containing UPE
- the chemical solution 1 has a residual defect suppression performance of AA, a spot-like defect suppression performance of AA, a bridge defect suppression performance of AA, a pattern width uniform performance of AA, and a purification device filter life of AA. It is A.
- the results are similarly described in each table of the first group, and for the chemical solutions 31 to 48, the results are described in each table of the second group.
- Table 2 is divided into Table 2 (1-1) to Table 2 (1-3).
- Table 2 describes the filtration device used for purification of each chemical solution and the evaluation results of the obtained chemical solution over the corresponding rows of each contingency table.
- the chemical solution 50 is described in the first row of each contingency table. This indicates that the chemical solution 50 was manufactured by the filtration device described in FIG. 28, and that the liquid to be purified used for manufacturing the chemical solution 50 is SPM (4: 1). Moreover, it has shown that pH of SPM (4: 1) was 1.0 or less. Moreover, it has shown that the filter of the filtration apparatus used for manufacture of the chemical
- the filtration device has BU-1 (filter having a pore diameter of 200 nm containing PTFE) and BU-2 (filter having a pore diameter of 20 nm containing PTFE), and FA (filter A) has a pore diameter of 20 nm. It has a PFSA / PTFE filter (CWST: 35 ⁇ 10 ⁇ 5 N / cm), and on the downstream side thereof, BD-1 (a filter having a pore diameter of 10 nm containing PTFE) and BD-2 (a pore diameter containing PTFE of 10 nm) It is shown that it has a filter.
- the evaluation of the chemical solution 50 indicates that the number of residual defects is 2932 / wafer, of which the number of metal residual defects is 36 / wafer, the ratio is 1.2%, and the evaluation is A. Similarly, the results of the chemical solutions 51 to 54 are described in the respective tables in Table 2.
- Table 3 is divided into Table 3 (1-1) to Table 3 (1-3).
- Table 3 describes the filtration device used for purification of each chemical solution and the evaluation results of the obtained chemical solution over the corresponding rows of each contingency table.
- the chemical solution 60 is described in the first row of each contingency table. This indicates that the chemical liquid 60 was manufactured by the filtration device described in FIG. 30, and that the liquid to be purified used for manufacturing the chemical 60 is the resist resin composition 2.
- medical solution 60 was wash
- the filtration apparatus has BU-1 (filter with a pore diameter of 20 nm containing PTFE), BU-2 (filter with a pore diameter of 2 nm containing UPE), and BU-3 (filter with a pore diameter of 10 nm containing Nylon).
- F-A filter A
- BD-1 pore diameter containing UPE of 2 nm is provided downstream thereof. It is shown that it has a filter.
- the chemical solution 60 contains 0.09 mass ppb Mg, 0.37 mass ppb Ca relative to the total mass of the chemical solution, the Cr content is less than the detection limit, and the Fe content is 0.15 mass ppb.
- the content of Ni is less than the detection limit value, and the total content of metal components is 0.61 mass ppb with respect to the total mass of the chemical solution.
- positioned in the downstream of the filter A with the filter B is the residue defect suppression performance more excellent compared with the chemical
- the chemical liquid 45 manufactured using a filtration device (including a purification device) including a filter having a pore size of 20 nm or less in the filter BD is superior to the chemical solution 44 in terms of residue defect suppression performance and more. It had excellent bridge defect suppression performance.
- medical solution 1 manufactured using the filtration apparatus in which the filter BD arrange
- the chemical solution 1 compared with the chemical solution 46, the chemical solution 1 has better residue defect suppression performance, better stain-like defect suppression performance, better bridge defect suppression performance, and better pattern width uniformity performance.
- the chemical solution 1 manufactured using the apparatus has a better residue defect suppression performance, a better bridge defect suppression performance, and a better pattern field uniform performance.
- the chemical solution 1 manufactured using the filtration device (including the purification device) including the filter BU disposed on the upstream side of the filter A on the flow path is superior to the chemical solution 47. Residual defect suppression performance, better spot-like defect suppression performance, better bridge defect suppression performance, and better pattern width uniformity performance.
- purification apparatus containing) at least 1 of filter BU has a hole diameter of 10 nm or more has the residue defect suppression performance more excellent compared with the chemical
- the filtration apparatus (including the purification apparatus) used for the production of the chemical liquid 1 has a lower productivity cost (more than the filtration apparatus (including the purification apparatus) used for the production of the chemical liquid 48 production apparatus). Had excellent productivity).
- the chemical solution 1 manufactured using a filtration device (including a purification device) containing a resin having an ion-exchange group in the filter BU is superior to the chemical solution 12 in terms of better residue defect suppression performance, and more excellent. It had excellent bridge defect suppression performance and better pattern width uniformity performance.
- the filtration device (including the purification device) used for the production of the chemical solution 1 has a longer filter life than the filtration device (including the purification device) used for the production of the chemical solution 12, and the productivity cost. Was lower (has better productivity).
- the chemical solution 1 manufactured using a filtration device (including a purification device) having a filter having a pore diameter of 10 nm or more arranged in series with the tank on the upstream side of the flow path with respect to the tank is compared with the chemical solution 48.
- the filtration device (including the purification device) used for the production of the chemical solution 1 had lower productivity costs (more excellent) than the filtration device (including the purification device) used for the production of the chemical solution 48. Had productivity).
- the chemical solution 50 obtained by purifying the liquid to be purified having a pH in the range of 0 to 9 had better defect suppression performance than the chemical solution 54. This indicates that the filtration device according to the embodiment of the present invention has a more excellent effect for purifying a liquid to be purified having a pH in the range of 0 to 9.
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Abstract
Description
近年、フォトリソグラフィ技術の進歩によりパターンの微細化が進んでいる。
このような配線形成工程に用いられる薬液には、更なる欠陥抑制性能の向上を求められている。このような薬液は、一般に、薬液に求められる成分を主成分として含有する被精製液をフィルタ等を用いて精製して不純物等を除くことにより得られると考えられている。
本明細書においては、後述する有機溶剤系被精製液を精製して得られる薬液のうち、実質的に樹脂を含有しない薬液(典型的には、プリウェット液、現像液、及び、リンス液等のレジスト膜の形成の際に用いられる薬液)については、後述する実施例における[試験例1]に記載した残渣欠陥抑制性能を「欠陥抑制性能」とする。また、樹脂を含有し、レジスト膜の形成に用いられるレジスト樹脂組成物については、後述する実施例における[試験例3]に記載したスカム欠陥抑制性能を「欠陥抑制性能」とする。また、後述する水系被精製液を精製して得られる薬液(典型的には、エッチング液、レジスト剥離液、及び、現像液等として用いられる薬液)については、後述する実施例における[試験例2]に記載した、残渣欠陥数に対するメタル残渣欠陥数の比率(メタル欠陥比率)が所定の範囲内にあることとする。
以下、単に「欠陥抑制性能」という場合、薬液の種類に応じたそれぞれの欠陥抑制性能(残渣欠陥抑制性能、スカム欠陥抑制性能、又は、メタル欠陥比率)を意味する。
[2] フィルタBは、流通路上において、フィルタAの下流側に配置されたフィルタBDを少なくとも1つを含む、[1]に記載のろ過装置。
[3] 少なくとも1つのフィルタBDは、20nm以下の孔径を有する、[2]に記載のろ過装置。
[4] 少なくとも1つのフィルタBDがポリオレフィン、ポリアミド、ポリフルオロカーボン、ポリスチレン、ポリスルホン、及び、ポリエーテルスルホンからなる群より選択される少なくとも1種を含有する、[2]又は[3]に記載のろ過装置。
[5] 流通路上において、最も下流側に配置されたフィルタBDが、10nm以下の孔径を有し、ポリテトラフルオロエチレン、ポリエチレン、及び、ナイロンからなる群より選択される少なくとも1種を含有する、[2]~[4]のいずれかに記載のろ過装置。
[6] 少なくとも1つのフィルタBDのうち、いずれかのフィルタBDからなる基準フィルタの下流側から、基準フィルタの上流側へと、被精製液を返送可能な返送流通路を有する、[2]~[5]のいずれかに記載のろ過装置。
[7] フィルタBは、流通路上においてフィルタAの上流側に配置されたフィルタBUを少なくとも1つ含む、[1]~[6]のいずれかに記載のろ過装置。
[8] 少なくとも1つのフィルタBUは、10nm以上の孔径を有する、[7]に記載のろ過装置。
[9] 少なくとも1つのフィルタBUは、20nm以上の孔径を有する、[7]又は[8]に記載のろ過装置。
[10] フィルタBUが、イオン交換基を有する樹脂を含有する、[7]~[9]のいずれかに記載のろ過装置。
[11] イオン交換基が、陰イオン交換基を含む、[10]記載のろ過装置。
[12] 流通路上に、フィルタAと直列に配置されたタンクを更に有する[1]~[11]のいずれかに記載のろ過装置。
[13] タンクに対して流通路の上流側に、タンクと直列に配置された、孔径10nm以上のフィルタCを更に有する[12]に記載のろ過装置。
[14] タンクに対して流通路の上流側に、タンクと直列に配置された、孔径20nm以上のフィルタCを更に有する[12]に記載のろ過装置。
[15] 流通路上における、フィルタAの下流側から、フィルタAの上流側へと、被精製液を返送可能な返送流通路を有する、[1]に記載のろ過装置。
[16] 被精製液のpHが0~9である、[1]~[15]のいずれかに記載のろ過装置。
[17] 薬液が、洗浄液、エッチング液、リンス液、前処理液、及び、レジスト液からなる群より選択される少なくとも1種である、[1]~[16]のいずれかに記載のろ過装置。
[18] フィルタAの臨界湿潤表面張力が27×10-5N/cm以上である、[1]~[17]のいずれかに記載のろ過装置。
[19] フィルタAの臨界湿潤表面張力が30×10-5N/cm以上である、[1]~[18]のいずれかに記載のろ過装置。
[20] 被精製液を精製して、半導体基板製造用の薬液を製造するためのろ過装置であって、流入部と、流出部と、フィルタAと、フィルタAとは異なる少なくとも1つのフィルタBと、を有し、フィルタA及びフィルタBは、流入部及び流出部の間に直列に配置され、流入部から流出部にいたる流通路を有するろ過装置であって、フィルタAは、ポリテトラフルオロエチレン製の多孔質基材と、基材の少なくとも一部を覆うように形成されたペルフルオロスルホン酸ポリマーを含有する非架橋コーティングとを有する第1多孔質膜、及び、ペルフルオロスルホン酸ポリマーとブレンドされたポリテトラフルオロエチレンを含有する第2多孔質膜、からなる群より選択される少なくとも1種を含む、ろ過装置。
[21] [1]~[20]のいずれかに記載のろ過装置と、ろ過装置の流入部に接続された少なくとも1つの蒸留器と、を有する精製装置。
[22] 少なくとも1つの蒸留器は、直列に接続された複数の蒸留器を含む、[21]に記載の精製装置。
[23] 被精製液を精製して薬液を得る、薬液の製造方法であって、[1]~[20]のいずれかに記載のろ過装置を用いて、被精製液を精製して薬液を得る、ろ過工程を有する、薬液の製造方法。
[24] ろ過工程の前に、フィルタA、及び、フィルタBを洗浄するフィルタ洗浄工程を更に有する、[23]に記載の薬液の製造方法。
[25] ろ過工程の前に、ろ過装置の接液部を洗浄する装置洗浄工程を更に有する、[23]又は[24]に記載の薬液の製造方法。
[26] 被精製液を精製して薬液を得る、薬液の製造方法であって、被精製液を、ポリテトラフルオロエチレン製の多孔質基材と、基材の少なくとも一部を覆うように形成されたペルフルオロスルホン酸ポリマーを含有する非架橋コーティングとを有する第1多孔質膜、及び、ペルフルオロスルホン酸ポリマーとブレンドされたポリテトラフルオロエチレンを含有する第2多孔質膜、からなる群より選択される少なくとも1種を含むフィルタA、及び、フィルタAとは異なるフィルタB、を用いてろ過して薬液を得る工程を有する、薬液の製造方法。
以下に記載する構成要件の説明は、本発明の代表的な実施形態に基づいてなされることがあるが、本発明はそのような実施形態に制限されない。
なお、本明細書において、「~」を用いて表される数値範囲は、「~」の前後に記載される数値を下限値及び上限値として含む範囲を意味する。
本発明の実施形態に係るろ過装置は、流入部と、流出部と、フィルタAと、フィルタAとは異なる少なくとも1つのフィルタBと、を有し、フィルタA及びフィルタBは、流入部及び流出部の間に直列に配置され、流入部から流出部にいたる流通路(被精製液の流れる経路)を有するろ過装置であって、(言い換えれば、流入部と流出部との間に、フィルタAと上記フィルタAとは異なる少なくとも1つのフィルタBとが直列に配置され、流入部から流出部にいたる流通路を有するろ過装置であって、)フィルタAは、後述する第1多孔質膜、及び、第2多孔質膜からなる群より選択される少なくとも1種である、ろ過装置である。ろ過装置は、流入部から流出部にいたる流通路を有し、流入部と流出部との間にフィルタAと上記フィルタAとは異なる少なくとも1つのフィルタBとが直列に配置されている。本発明の実施形態に係るろ過装置はフィルタAとフィルタBとが流通路上に直列に配置されているため、被精製液は、フィルタA及びフィルタB(又は、フィルタB及びフィルタA)によって順次ろ過される。以下、本発明の実施形態に係るろ過装置について説明するが、以下の説明では、フィルタに導入した被精製液の全量をフィルタでろ過する、全量ろ過方式(デッドエンド方式)のろ過装置を例示するが、本発明の実施形態に係るろ過装置としては上記に制限されず、導入した被精製液を精製済み被精製液と濃縮液とに分離する(更に濃縮液を再度被精製液としてフィルタに導入する場合もある)クロスフロー方式のろ過装置であってもよく、これらを組み合わせた方式であってもよい。以下では、上記ろ過装置の実施形態について、図面を用いて説明する。
図1は、本発明の第一実施形態に係るろ過装置を表す模式図である。
ろ過装置100は、流入部101と流出部102の間に、フィルタAであるフィルタ103と、上記フィルタ103とは異なるフィルタ104(フィルタBD)とが配管105を介して直列に配置されたろ過装置である。
流入部101、フィルタ103、配管105、フィルタ104、及び、流出部102は、それぞれの内部に被精製液を流通できるよう構成されており、上記部材が連結されて、流通路S1(被精製液が流れる経路)が形成されている。
流入部101、配管105、及び、流出部102の形態としては特に制限されないが、典型的には、内部に被精製液を流通可能に形成された中空円筒状の形態が挙げられる。これらの材料成分としては特に制限されないが、接液部(被精製液をろ過するに際して、被精製液が接触する可能性のある部分)は、後述する耐腐食材料で形成されていることが好ましい。
なお、ろ過装置100は、被精製液を流通させる目的で、流通路S1上に(例えば、流入部101、配管105、及び、流出部102等)に、図示しないポンプ、ダンパ、及び、弁等を有していてもよい。
また、より優れた本発明の効果を有するろ過装置が得られる点で、ハウジングの接液部の少なくとも一部、好ましくは接液部の表面積に対して90%、より好ましくは接液部の表面積に対して99%は、後述する耐腐食材料からなることが好ましい。なお、本明細書において接液部とは、被精製液が接触する可能性のある部分(但し、フィルタ自体を除く)を意味し、ハウジング等のユニットの内壁等を意味する。
フィルタAは後述する第1多孔質膜、及び、第2多孔質膜からなる群より選択される少なくとも1種の膜を有する。
第1多孔質膜は、ポリテトラフルオロエチレン(PTFE)製の多孔質基材と、多孔質基材を覆うように形成されたペルフルオロスルホン(PFSA)酸ポリマーを含有する非架橋コーティングとを有する。なお、第1多孔質膜が有する多孔質基材は、非架橋コーティングにより覆われていない領域があってもよいが、その表面(多孔質膜の最表面から連通する孔の表面も含む)の全体が非架橋コーティングで覆われていることが好ましい。
第1多孔質膜の製造方法としては特に制限されないが、典型的には、PTFE製の多孔質基材上にペルフルオロスルホン酸(PFSA)ポリマーを含有するポリマー分散液を塗布して非架橋コーティング(層)を形成する方法が好ましい。
なお、本明細書において、孔径とは、イソプロパノール(IPA)又は、HFE-7200(「ノベック7200」、3M社製、ハイドロフロオロエーテル、C4F9OC2H5)のバブルポイントによって決定される孔径を意味する。
一方で、被精製液の表面張力との関係では、第1多孔質膜の臨界湿潤表面張力と、被精製液の表面張力との差の絶対値がより小さい方が、第1多孔質膜が被精製液で濡れやすく、結果として優れた欠陥抑制性能を有する薬液が得られやすい。
例えば、イソプロピルアルコールの表面張力が、20.8(25℃)×10-5N/cmであるように、一般に、有機溶剤の表面張力は、15×10-5~35×10-5N/cm程度であることが多く、被精製液が有機溶剤を含有する場合(後述する有機溶剤系被精製液等である場合)、被精製液の表面張力との差をより小さくする観点からは、第1多孔質膜の臨界湿潤表面張力は、一般に、40×10-5N/cm以下が好ましい。
なお、第1多孔質膜の臨界湿潤表面張力は、ペルフルオロスルホン酸ポリマーを含有する非架橋コーティングにおけるペルフルオロスルホン酸ポリマーの含有量により調整可能である。具体的には、非架橋コーティング中におけるペルフルオロスルホン酸ポリマーの含有量を多くすれば、より高い臨界湿潤表面張力を有する第1多孔質膜が得られやすく、非架橋コーティング中におけるペルフルオロスルホン酸ポリマーの含有量を少なくすれば、より低い臨界湿潤表面張力を有す第1多孔質膜が得られやすい。
第2多孔質膜は、ペルフルオロスルホン酸ポリマーとブレンドされたポリテトラフルオロエチレンを含有する多孔質膜である。
PTFEとしては特に制限されず、公知のPTFEを使用できる。
PTFEとブレンドするPFSAとしては特に制限されないが、例えば、Solvay Specialty Polymers(Borger、Texas)からアクイヴィオン(Aquivion)(登録商標)PFSA(例えば、アクイヴィオンPFSA D83-24B、アクイヴィオンPFSA D83-06A、及びアクイヴィオンPFSA D79-20BS)として入手可能であり、これはテトラフルオロエチレンとスルホニルフルオリドビニルエーテル(SFVE)F2C=CF-O-CF2-CF2-SO2Fの短い側鎖(SSC)のコポリマーをベースとしている。アイオノマー分散液はそのスルホン酸形態を含有する。適切なPFSA添加剤の別の例はデュポン(DuPont)(登録商標)ナフィオン(Nafion)(登録商標)PFSAポリマー分散液である。
臨界湿潤表面張力が27×10-5N/cm以上であると、被精製液に含有される金属不純物等をより効率的に除去することができ、結果としてより優れた欠陥抑制性能を有する薬液が得られる。この点において、臨界湿潤表面張力は、30×10-5N/cm以上がより好ましく、33×10-5N/cm以上が更に好ましい。
一方で、被精製液の表面張力との関係では、第2多孔質膜の臨界湿潤表面張力と、被精製液の表面張力との差の絶対値がより小さい方が、第2多孔質膜が被精製液で濡れやすく、結果として優れた欠陥抑制性能を有する薬液が得られやすい。
被精製液が有機溶剤を含有する場合(後述する「有機溶剤系被精製液」等である場合)、被精製液の表面張力との差をより小さくする観点からは、第2多孔質膜の臨界湿潤表面張力は40×10-5N/cm以下が好ましい。
なお、第2多孔質膜の臨界湿潤表面張力は、ペルフルオロスルホン酸ポリマーとブレンドされたポリテトラフルオロエチレンにおける、ペルフルオロスルホン酸ポリマーの含有量によって調整可能である。具体的には、ペルフルオロスルホン酸ポリマーの含有量を多くすれば、より高い臨界湿潤表面張力を有する第2多孔質膜が得られ、ペルフルオロスルホン酸ポリマーの含有量を少なくすれば、より低い臨界湿潤表面張力を有する第2多孔質膜が得られやすい。
フィルタBDは、フィルタAとは異なるフィルタであって、流通路上においてフィルタAの下流側に、フィルタAと直列に配置されたフィルタである。本明細書において、フィルタ同士が異なるとは、孔径、材料、及び、細孔構造からなる群より選択される少なくとも1種が異なることを意味する。なかでもより優れた本発明の効果を有するろ過装置が得られる点で、フィルタAとフィルタBDとは、少なくとも孔径が異なることが好ましく、孔径と材料とが異なることが好ましい。なお、材料が異なるとは、典型的には構成する成分(材料成分)が異なる形態が挙げられる。
本発明者らの検討によれば、フィルタAを用いて被精製液をろ過すると、フィルタAに起因する微粒子が発生し、被精製液に混入することを知見している。本実施形態に係るろ過装置は、流通路上においてフィルタAの下流側にフィルタBDを有しているため、フィルタAに起因する微粒子を被精製液からろ別することができ、より優れた欠陥抑制性能を有する薬液が得られやすい。
この場合、最も下流側に配置されたフィルタBDは材料成分として、ポリエチレン(特に超高分子量ポリエチレン;UPE)、ポリテトラフルオロエチレン、及び、ナイロンからなる群より選択される少なくとも1種を含有することが好ましく、ポリエチレン、又は、ポリテトラフルオロエチレンを含有することより好ましく、ポリテトラフルオロエチレンを含有することが更に好ましい。
このとき、フィルタBDが含有する材料成分によって、除去対象となる不純物は異なることが多い。例えば、ナイロンを含有するフィルタBDは、被精製液中において、膜上に形成されると推測される親水性の層によってゲル状の不純物が吸着除去されやすいと推測され、超高分子量ポリエチレンを含有するフィルタBDは、ふるい効果によって粒子状の不純物を除去しやすいものと推測される。
フィルタBDは材料成分として、6-ナイロン、及び、6,6-ナイロン等のポリアミド;ポリエチレン、及び、ポリプロピレン等のポリオレフィン;ポリスチレン;ポリイミド;ポリアミドイミド;ポリ(メタ)アクリレート;ポリテトラフルオロエチレン、パーフルオロアルコキシアルカン、パーフルオロエチレンプロペンコポリマー、エチレン・テトラフルオロエチレンコポリマー、エチレン-クロロトリフロオロエチレンコポリマー、ポリクロロトリフルオロエチレン、ポリフッ化ビニリデン、及び、ポリフッ化ビニル等のポリフルオロカーボン;ポリビニルアルコール;ポリエステル;セルロース;セルロースアセテート等を含有することが好ましい。なかでも、より優れた耐溶剤性を有し、得られる薬液がより優れた欠陥抑制性能を有する点で、ナイロン(なかでも、6,6-ナイロンが好ましい)、ポリオレフィン(なかでも、ポリエチレンが好ましい)、ポリ(メタ)アクリレート、及び、ポリフルオロカーボン(なかでも、ポリテトラフルオロエチレン(PTFE)、パーフルオロアルコキシアルカン(PFA)が好ましい。)からなる群から選択される少なくとも1種を含有することが好ましい。これらの重合体は単独で又は二種以上を組み合わせて使用できる。
また、樹脂以外にも、ケイソウ土、及び、ガラス等であってもよい。
すなわち、フィルタとしては、上記で挙げた各材料を基材として、上記基材にイオン交換基を導入したものが好ましい。典型的には、上記基材の表面にイオン交換基を有する基材を含む層を含むフィルタが好ましい。表面修飾された基材としては特に制限されず、製造がより容易な点で、上記重合体にイオン交換基を導入したものが好ましい。
ポリオレフィンとしては、ポリエチレン、及び、ポリプロピレン等が挙げられ、中でも、超高分子量ポリエチレンが好ましい。ポリアミドとしては、6-ナイロン、及び、6,6-ナイロン等が挙げられる。ポリフルオロカーボンとしてはポリテトラフルオロエチレン(PTFE)、パーフルオロアルコキシアルカン、パーフルオロエチレンプロペンコポリマー、エチレン・テトラフルオロエチレンコポリマー、エチレン-クロロトリフロオロエチレンコポリマー、ポリクロロトリフルオロエチレン、ポリフッ化ビニリデン、及び、ポリフッ化ビニル等が挙げられ、なかでも、PTFEが好ましい。
例えば、樹脂等の粉末を焼結して形成すれば多孔質膜が得られ、及び、エレクトロスピニング、エレクトロブローイング、及び、メルトブローイング等の方法により形成すれば繊維膜が得られる。これらは、それぞれ細孔構造が異なる。
ふるい膜の典型的な例としては、ポリテトラフルオロエチレン(PTFE)膜とUPE膜が含まれるが、これらに制限されない。
なお、「ふるい保持機構」とは、除去対象粒子が多孔質膜の細孔径よりも大きいことによる結果の保持を指す。ふるい保持力は、フィルタケーキ(膜の表面での除去対象となる粒子の凝集)を形成することによって向上させることができる。フィルタケーキは、2次フィルタの機能を効果的に果たす。
多孔質膜における細孔の大きさの分布とその膜中における位置の分布は、特に制限されない。大きさの分布がより小さく、かつ、その膜中における分布位置が対称であってもよい。また、大きさの分布がより大きく、かつ、その膜中における分布位置が非対称であってもよい(上記の膜を「非対称多孔質膜」ともいう。)。非対称多孔質膜では、孔の大きさは膜中で変化し、典型的には、膜一方の表面から膜の他方の表面に向かって孔径が大きくなる。このとき、孔径の大きい細孔が多い側の表面を「オープン側」といい、孔径が小さい細孔が多い側の表面を「タイト側」ともいう。
また、非対称多孔質膜としては、例えば、細孔の大きさが膜の厚さ内のある位置においてで最小となるもの(これを「砂時計形状」ともいう。)が挙げられる。
なかでも、多孔質膜は、超高分子量ポリエチレンを材料成分として含有することが好ましい。超高分子量ポリエチレンは、極めて長い鎖を有する熱可塑性ポリエチレンを意味し、分子量が百万以上、典型的には、200~600万が好ましい。
なお、本明細書で使用される「非ふるい」による保持機構は、フィルタの圧力降下、又は、細孔径に関連しない、妨害、拡散及び吸着などの機構によって生じる保持を指す。
図2は、本発明の第二実施形態に係るろ過装置を表す模式図である。
ろ過装置200は、流入部101及び流出部102の間に、フィルタAであるフィルタ103及び上記フィルタ103とは異なるフィルタ201(フィルタBU)が配管202を介して直列に配置されたろ過装置である。
流入部101、フィルタ201、配管202、フィルタ103、及び、流出部102は、それぞれの内部に被精製液を流通できるよう構成されており、上記部材が連結されて、流通路S2(被精製液が流れる経路)が形成されている。
フィルタBUは、フィルタAとは異なるフィルタであって、流通路上においてフィルタAの上流側に、フィルタAと直列に配置されたフィルタである。流通路上において、流入部が上流側であり、流出部が下流側である。より優れた本発明の効果を有するろ過装置が得られる点で、フィルタAとフィルタBUとは、少なくとも材料が異なることが好ましく、孔径と材料とが異なることが好ましい。
フィルタBUとしては、ポリフルオロカーボン、及び、ポリオレフィン等の基材に、イオン交換基を導入した材料がより好ましい。
なかでもイオン交換基としては、陰イオン交換基が好ましく、陰イオン交換基としては例えば、4級アンモニウム基等が挙げられる。フィルタBUが陰イオン交換基を有する樹脂を材料成分として含有する場合、より優れた欠陥抑制性能を有する薬液が得られやすい。
フィルタBUの材料成分としては、ポリフルオロカーボン、及び、ポリオレフィン等の基材に、陰イオン交換基を導入した物がより好ましい。
図3は、本発明の第二実施形態に係るろ過装置の変形例を表すろ過装置の模式図である。ろ過装置300は、流入部101と流出部102との間に、フィルタAであるフィルタ103と、フィルタBUであるフィルタ201と、フィルタBDであるフィルタ104とを有し、フィルタ201と、フィルタ103と、フィルタ104とが配管301、及び、配管302を介して直列に配置されたろ過装置である。
ろ過装置300は、流通路上においてフィルタAの上流側にフィルタBUを有するため、フィルタAはより長寿命となり、流通路上においてフィルタAの下流側にフィルタBDを有するため、フィルタAに起因して被精製液に混入する微粒子が効率よく除去でき、結果として更に優れた欠陥抑制性能を有する薬液が得られやすい。
図4は本発明の第三実施形態に係るろ過装置を表す模式図である。
ろ過装置400は、流入部101と流出部102との間であって、流通路S4上においてフィルタ103(フィルタA)の上流側に、フィルタAと直列に配置されたタンク401を更に有するろ過装置である。タンク401と、フィルタ103(フィルタA)と、フィルタ104(フィルタBD)とは、配管402及び配管105を介して直列に配置されている。タンク401は上記のフィルタ及び配管等とともに、流通路S4を構成している。
なお、タンク401の材料は特に制限されないが、既に説明したハウジングの材料と同様の材料が使用でき、その接液部の少なくとも一部(好ましくは接液部の表面積の90%以上、より好ましくは99%以上)は後述する耐腐食材料からなることが好ましい。
図5は本発明の第三実施形態に係るろ過装置の変形例を表す模式図である。
ろ過装置500は、流入部101と流出部102との間であって、流通路S5上においてフィルタ103(フィルタA)の下流側に、フィルタAと直列に配置されたタンク401を更に有するろ過装置である。フィルタ103(フィルタA)と、タンク401と、フィルタ104(フィルタBD)とは、配管501及び配管502を介して直列に配置されている。タンク401は上記のフィルタ及び配管等とともに、流通路S5を構成している。
図6は本発明の第四実施形態に係るろ過装置を表す模式図である。
ろ過装置600は、流入部101と流出部102の間に、フィルタCであるフィルタ601と、タンク401と、フィルタAであるフィルタ103と、フィルタBDであるフィルタ104とが配管602、配管402、及び、配管105を介して直列に配置されたろ過装置である。
ろ過装置600では、流入部101、フィルタ601、配管602、タンク401、配管402、フィルタ103、配管105、フィルタ104、及び、流出部102が、流通路S6を形成している。
なお、本実施形態に係るろ過装置としては、流通路上にフィルタAとフィルタBDがこの順に直列に配置された形態(例えば第二実施形態)、及び、流通路上にフィルタBU、フィルタA,及び、フィルタBDがこの順に直列に配置された形態(例えば第二実施形態の変形例)において、フィルタAの下流側にタンクを更に有し、上記タンクの上流側にフィルタCを有する形態であってもよい。
図7は本発明の第五実施形態に係るろ過装置の模式図である。ろ過装置700は、流入部101と、流出部102と、フィルタAであるフィルタ103と、フィルタBDであるフィルタ104とを有し、フィルタ103とフィルタ104とが、流入部101と流出部102との間に直列に配置され、流入部101から流出部102にいたる流通路S7が形成されたろ過装置である。
ろ過装置700では、流入部101と、フィルタ103と、配管105と、フィルタ104と、流出部102とが、流通路S7を形成している。
また、図7では、返送流通路R1が配管のみから形成されているが、既に説明した1つ又は複数のタンク及び配管から形成されていてもよい。
ろ過装置800は、流入部101と、タンク401(a)、401(b)、流出部102とフィルタAであるフィルタ103と、フィルタBDであるフィルタ104とを有し、タンク401(a)、フィルタ103、フィルタ104、及び、401(b)とが、流入部101と流出部102との間に直列に配置され、流入部101と、タンク401(a)、配管802、フィルタ103、配管803、フィルタ104、配管804、タンク401(b)、及び、流出部102とが、流通路S8を形成している。
図9は本発明の第五実施形態に係るろ過装置の模式図である。ろ過装置900は、流入部101と、流出部102と、フィルタAであるフィルタ103と、フィルタBDであるフィルタ104とを有し、フィルタ103とフィルタ104とが、流入部101と流出部102との間に直列に配置され、流入部101から流出部102にいたる流通路S9が形成されたろ過装置である。
ろ過装置900では、流入部101と、フィルタ103と、配管105と、フィルタ104と、流出部102とが、流通路S9を形成している。
ろ過装置1000では、流入部101と、フィルタ103と、配管105と、フィルタ104-1と、配管1001と、フィルタ104-2と、流出部102とが、流通路S10を形成している。
本発明の実施形態に係る薬液の製造方法は、被精製液を精製して薬液を得る、薬液の製造方法であって、既に説明したろ過装置を用いて被精製液をろ過して、薬液を得るろ過工程を有する。
本発明の実施形態に係る薬液の製造方法が適用できる被精製液としては特に制限されないが、溶剤を含有することが好ましい。溶剤としては有機溶剤、及び、水等が挙げられ、有機溶剤を含有することが好ましい。以下では、被精製液中に含有される溶剤の全質量に対して、有機溶剤の含有量(複数の有機溶剤を含有する場合にはその合計含有量)が50質量%を超える有機溶剤系と、被精製液中に含有される溶剤の全質量に対して、水の含有量が50質量%を超える水系とに分けて説明する。
(有機溶剤)
有機溶剤系の被精製液は、溶剤を含有し、被精製液に含有される溶剤の全質量に対して有機溶剤の含有量が50質量%以上である。
被精製液は、有機溶剤を含有する。被精製液中における有機溶剤の含有量としては特に制限されないが、一般に被精製液の全質量に対して、99.0質量%以上が好ましい。上限値としては特に制限されないが、一般に、99.99999質量%以下が好ましい。
有機溶剤は1種を単独で用いても、2種以上を併用してもよい。2種以上の有機溶剤を併用する場合には、合計含有量が上記範囲内であることが好ましい。
なお、本明細書において液状とは、25℃、大気圧下において、液体であることを意味する。
また、有機溶剤としては、例えば、特開2016-57614号公報、特開2014-219664号公報、特開2016-138219号公報、及び、特開2015-135379号公報に記載のものを用いてもよい。
被精製液は、上記以外の他の成分を含有してもよい。他の成分としては、例えば、無機物(金属イオン、金属粒子、及び、金属酸化物粒子等)、樹脂、樹脂以外の有機物、及び、水等が挙げられる。
被精製液は、無機物を含有してもよい。無機物としては特に制限されず、金属イオン、及び、金属含有粒子等が挙げられる。
被精製液は樹脂を含有してもよい。
上記薬液は更に樹脂を含有してもよい。樹脂としては、酸の作用により分解して極性基を生じる基を有する樹脂Pがより好ましい。上記樹脂としては、酸の作用により有機溶剤を主成分とする現像液に対する溶解性が減少する樹脂である、後述する式(AI)で表される繰り返し単位を有する樹脂がより好ましい。後述する式(AI)で表される繰り返し単位を有する樹脂は、酸の作用により分解してアルカリ可溶性基を生じる基(以下、「酸分解性基」ともいう)を有する。
極性基としては、アルカリ可溶性基が挙げられる。アルカリ可溶性基としては、例えば、カルボキシ基、フッ素化アルコール基(好ましくはヘキサフルオロイソプロパノール基)、フェノール性水酸基、及びスルホ基が挙げられる。
樹脂Pは、式(AI)で表される繰り返し単位を含有することが好ましい。
Xa1は、水素原子又は置換基を有していてもよいアルキル基を表す。
Tは、単結合又は2価の連結基を表す。
Ra1~Ra3は、それぞれ独立に、アルキル基(直鎖状又は分岐鎖状)又はシクロアルキル基(単環又は多環)を表す。
Ra1~Ra3の2つが結合して、シクロアルキル基(単環又は多環)を形成してもよい。
Xa1は、水素原子、メチル基、トリフルオロメチル基又はヒドロキシメチル基が好ましい。
Tは、単結合又は-COO-Rt-基が好ましい。Rtは、炭素数1~5のアルキレン基が好ましく、-CH2-基、-(CH2)2-基、又は、-(CH2)3-基がより好ましい。
Ra1~Ra3の2つが結合して形成されるシクロアルキル基としては、シクロペンチル基、若しくはシクロヘキシル基等の単環のシクロアルキル基、又は、ノルボルニル基、テトラシクロデカニル基、テトラシクロドデカニル基、若しくはアダマンチル基等の多環のシクロアルキル基が好ましい。炭素数5~6の単環のシクロアルキル基がより好ましい。
また、樹脂Pは、ラクトン構造を有する繰り返し単位Qを含有することが好ましい。
ラクトン構造を有する繰り返し単位Qは、1種単独で用いてもよく、2種以上を併用していてもよいが、1種単独で用いることが好ましい。
ラクトン構造を有する繰り返し単位Qの含有量は、樹脂P中の全繰り返し単位に対して、3~80モル%が好ましく、3~60モル%がより好ましい。
ラクトン構造としては、下記式(LC1-1)~(LC1-17)のいずれかで表されるラクトン構造を有する繰り返し単位を有することが好ましい。ラクトン構造としては式(LC1-1)、式(LC1-4)、式(LC1-5)、又は式(LC1-8)で表されるラクトン構造が好ましく、式(LC1-4)で表されるラクトン構造がより好ましい。
また、樹脂Pは、フェノール性水酸基を有する繰り返し単位を含有していてもよい。
フェノール性水酸基を有する繰り返し単位としては、例えば、下記一般式(I)で表される繰り返し単位が挙げられる。
R41、R42及びR43は、各々独立に、水素原子、アルキル基、ハロゲン原子、シアノ基又はアルコキシカルボニル基を表す。但し、R42はAr4と結合して環を形成していてもよく、その場合のR42は単結合又はアルキレン基を表す。
L4は、単結合又はアルキレン基を表す。
Ar4は、(n+1)価の芳香環基を表し、R42と結合して環を形成する場合には(n+2)価の芳香環基を表す。
nは、1~5の整数を表す。
(n+1)価の芳香環基は、更に置換基を有していてもよい。
樹脂Pは、極性基を有する有機基を含有する繰り返し単位、特に、極性基で置換された脂環炭化水素構造を有する繰り返し単位を更に含有していてもよい。これにより基板密着性、現像液親和性が向上する。
極性基で置換された脂環炭化水素構造の脂環炭化水素構造としては、アダマンチル基、ジアマンチル基又はノルボルナン基が好ましい。極性基としては、水酸基又はシアノ基が好ましい。
樹脂Pは、下記一般式(VI)で表される繰り返し単位を含有していてもよい。
R61、R62及びR63は、各々独立に、水素原子、アルキル基、シクロアルキル基、ハロゲン原子、シアノ基、又はアルコキシカルボニル基を表す。但し、R62はAr6と結合して環を形成していてもよく、その場合のR62は単結合又はアルキレン基を表す。
X6は、単結合、-COO-、又は-CONR64-を表す。R64は、水素原子又はアルキル基を表す。
L6は、単結合又はアルキレン基を表す。
Ar6は、(n+1)価の芳香環基を表し、R62と結合して環を形成する場合には(n+2)価の芳香環基を表す。
Y2は、n≧2の場合には各々独立に、水素原子又は酸の作用により脱離する基を表す。但し、Y2の少なくとも1つは、酸の作用により脱離する基を表す。
nは、1~4の整数を表す。
Mは、単結合又は2価の連結基を表す。
Qは、アルキル基、ヘテロ原子を含んでいてもよいシクロアルキル基、ヘテロ原子を含んでいてもよいアリール基、アミノ基、アンモニウム基、メルカプト基、シアノ基又はアルデヒド基を表す。
Q、M、L1の少なくとも2つが結合して環(好ましくは、5員若しくは6員環)を形成してもよい。
Ar3は、芳香環基を表す。
R3は、水素原子、アルキル基、シクロアルキル基、アリール基、アラルキル基、アルコキシ基、アシル基又はヘテロ環基を表す。
M3は、単結合又は2価の連結基を表す。
Q3は、アルキル基、シクロアルキル基、アリール基又はヘテロ環基を表す。
Q3、M3及びR3の少なくとも二つが結合して環を形成してもよい。
樹脂Pは、更に、側鎖に珪素原子を有する繰り返し単位を含有していてもよい。側鎖に珪素原子を有する繰り返し単位としては、例えば、珪素原子を有する(メタ)アクリレート系繰り返し単位、及び、珪素原子を有するビニル系繰り返し単位などが挙げられる。側鎖に珪素原子を有する繰り返し単位は、典型的には、側鎖に珪素原子を有する基を有する繰り返し単位であり、珪素原子を有する基としては、例えば、トリメチルシリル基、トリエチルシリル基、トリフェニルシリル基、トリシクロヘキシルシリル基、トリストリメチルシロキシシリル基、トリストリメチルシリルシリル基、メチルビストリメチルシリルシリル基、メチルビストリメチルシロキシシリル基、ジメチルトリメチルシリルシリル基、ジメチルトリメチルシロキシシリル基、及び、下記のような環状もしくは直鎖状ポリシロキサン、又はカゴ型あるいははしご型もしくはランダム型シルセスキオキサン構造などが挙げられる。式中、R、及び、R1は各々独立に、1価の置換基を表す。*は、結合手を表す。
水系の被精製液は、被精製液が含有する溶剤の全質量に対して、水を50質量%超含有し、50~95質量%が好ましい。
上記水は、特に限定されないが、半導体製造に使用される超純水を用いることが好ましく、その超純水を更に精製し、無機陰イオン及び金属イオン等を低減させた水を用いることがより好ましい。精製方法は特に限定されないが、ろ過膜又はイオン交換膜を用いた精製、並びに、蒸留による精製が好ましい。また、例えば、特開2007―254168号公報に記載されている方法により精製を行うことが好ましい。
水系の被精製液は、酸化剤を含有してもよい、酸化剤としては特に制限されず、公知の酸化剤が使用できる。酸化剤としては、例えば、過酸化水素、過酸化物、硝酸、硝酸塩、ヨウ素酸塩、過ヨウ素酸塩、次亜塩素酸塩、亜塩素酸塩、塩素酸塩、過塩素酸塩、過硫酸塩、重クロム酸塩、過マンガン酸塩、オゾン水、銀(II)塩、及び鉄(III)塩等が挙げられる。
水系被精製液は無機酸を含有してもよい。無機酸としては特に制限されず、公知の無機酸を用いることができる。無機酸としては例えば、硫酸、リン酸、及び、塩酸等が挙げられる。なお、無機酸は上述した酸化剤には含まれない。
被精製液中の無機酸の含有量としては特に制限されないが、被精製液の全質量に対して0.1質量%以上が好ましく、99.0質量%以下が更に好ましい。
無機酸は、1種を単独で用いても、2種以上を併用してもよい。2種以上の無機酸を併用する場合には、合計含有量が上記範囲内であることが好ましい。
水系被精製液は、防食剤を含有してもよい。防食剤としては特に制限されず、公知の防食剤が使用できる。防食剤としては例えば、1,2,4-トリアゾール(TAZ)、5-アミノテトラゾール(ATA)、5-アミノ-1,3,4-チアジアゾール-2-チオール、3-アミノ-1H-1,2,4トリアゾール、3,5-ジアミノ-1,2,4-トリアゾール、トリルトリアゾール、3-アミノ-5-メルカプト-1,2,4-トリアゾール、1-アミノ-1,2,4-トリアゾール、1-アミノ-1,2,3-トリアゾール、1-アミノ-5-メチル-1,2,3-トリアゾール、3-メルカプト-1,2,4-トリアゾール、3-イソプロピル-1,2,4-トリアゾール、ナフトトリアゾール、1H-テトラゾール-5-酢酸、2-メルカプトベンゾチアゾール(2-MBT)、1-フェニル-2-テトラゾリン-5-チオン、2-メルカプトベンゾイミダゾール(2-MBI)、4-メチル-2-フェニルイミダゾール、2-メルカプトチアゾリン、2,4-ジアミノ-6-メチル-1,3,5-トリアジン、チアゾール、イミダゾール、ベンゾイミダゾール、トリアジン、メチルテトラゾール、ビスムチオールI、1,3-ジメチル-2-イミダゾリジノン、1,5-ペンタメチレンテトラゾール、1-フェニル-5-メルカプトテトラゾール、ジアミノメチルトリアジン、イミダゾリンチオン、4-メチル-4H-1,2,4-トリアゾール-3-チオール、5-アミノ-1,3,4-チアジアゾール-2-チオール、ベンゾチアゾール、リン酸トリトリル、インダゾール、アデニン、シトシン、グアニン、チミン、ホスフェート阻害剤、アミン類、ピラゾール類、プロパンチオール、シラン類、第2級アミン類、ベンゾヒドロキサム酸類、複素環式窒素阻害剤、アスコルビン酸、チオ尿素、1,1,3,3-テトラメチル尿素、尿素、尿素誘導体類、尿酸、エチルキサントゲン酸カリウム、グリシン、ドデシルホスホン酸、イミノ二酢酸、ホウ酸、マロン酸、コハク酸、ニトリロ三酢酸、スルホラン、2,3,5-トリメチルピラジン、2-エチル-3,5-ジメチルピラジン、キノキサリン、アセチルピロール、ピリダジン、ヒスタジン(histadine)、ピラジン、グルタチオン(還元型)、システイン、シスチン、チオフェン、メルカプトピリジンN-オキシド、チアミンHCl、テトラエチルチウラムジスルフィド、2,5-ジメルカプト-1,3-チアジアゾールアスコルビン酸、カテコール、t-ブチルカテコール、フェノール、及びピロガロールが挙げられる。
上記の市販品としては、例えばニューカルゲンFS-3PG(竹本油脂社製)、及びホステンHLP-1(日光ケミカルズ社製)等が挙げられる。
親水性ポリマーとしては、例えば、ポリエチレングリコール等のポリグリコール類、ポリグリコール類のアルキルエーテル、ポリビニルアルコール、ポリビニルピロリドン、アルギン酸等の多糖類、ポリメタクリル酸、及びポリアクリル酸等のカルボン酸含有ポリマー、ポリアクリルアミド、ポリメタクリルアミド、及びポリエチレンイミン等が挙げられる。そのような親水性ポリマーの具体例としては、特開2009-88243号公報0042~0044段落、特開2007-194261号公報0026段落に記載されている水溶性ポリマーが挙げられる。
セリウム塩としては特に制限されず、公知のセリウム塩を用いることができる。
セリウム塩としては、例えば、3価のセリウム塩として、酢酸セリウム、硝酸セリウム、塩化セリウム、炭酸セリウム、シュウ酸セリウム、及び硫酸セリウム等が挙げられる。また、4価のセリウム塩として、硫酸セリウム、硫酸セリウムアンモニウム、硝酸セリウムアンモニウム、硝酸二アンモニウムセリウム、及び水酸化セリウム等が挙げられる。
防食剤は1種を単独で用いても、2種以上を併用してもよい。2種以上の防食剤を併用する場合には、合計含有量が上記範囲内であることが好ましい。
水系被精製液は、有機溶剤を含有してもよい。有機溶剤としては特に制限されないが、有機溶剤系被精製液が含有する被精製液として既に説明したとおりである。有機溶剤を含有する場合、被精製液が含有する溶剤の全質量に対して、有機溶剤の含有量は5~35質量%が好ましい。
被精製液のpHとしては特に制限されないが、より優れた欠陥抑制性能を有する薬液が得られる点で、0~9が好ましく、0~7がより好ましい。なお、本明細書において、被精製液のpHとは、25℃に調整した被精製液を用いて、ガラス電極法により測定した値を意味する。
本実施形態に係る薬液の製造方法は、既に説明したろ過装置を用いて、上記被精製液をろ過して、薬液を得るろ過工程を有する。
上記ろ過装置は、フィルタAとフィルタBとが直列に配置されて形成された流通路を有する。各フィルタに対する被精製液の供給圧力としては特に制限されないが、一般に、0.00010~1.0MPaが好ましい。
なかでも、より優れた欠陥抑制性能を有する薬液が得られる点で、供給圧力P2は、0.00050~0.090MPaが好ましく、0.0010~0.050MPaがより好ましく、0.0050~0.040MPaが更に好ましい。
また、ろ過圧力はろ過精度に影響を与えることから、ろ過時における圧力の脈動は可能な限り少ない方が好ましい。
フィルタにはフィルタ性能(フィルタが壊れない)を保障する耐差圧が設定されており、この値が大きい場合にはろ過圧力を高めることでろ過速度を高めることができる。つまり、上記ろ過速度上限は、通常、フィルタの耐差圧に依存するが、通常、10.0L/分/m2以下が好ましい。
なお、後述する各工程も、上記クリーン環境下にて実施することが好ましい。
循環ろ過の回数としては特に制限されないが、一般に1~10回が好ましい。なお、循環ろ過はフィルタAによるろ過を繰り返すよう、被精製液をフィルタAの上流に返送すればよいが、この際、フィルタAに加えて少なくとも1のフィルタBによるろ過も合わせ繰り返すよう、返送流通路を調整してもよい。
本実施形態に係る薬液の製造方法は、上記以外の工程を有していてもよい。上記以外の工程としては、例えば、フィルタ洗浄工程、装置洗浄工程、除電工程、及び、被精製液準備工程等が挙げられる。以下では、各工程について詳述する。
フィルタ洗浄工程は、ろ過工程の前にフィルタA及びフィルタBを洗浄する工程である。フィルタを洗浄する方法としては特に制限されないが、例えば、フィルタを浸漬液に浸漬する方法、フィルタに洗浄液を通液して洗浄する方法、及び、これらの組合せ等が挙げられる。
フィルタを浸漬液に浸漬する方法としては、例えば、浸漬用容器を浸漬液で満たし、上記浸漬液にフィルタを浸漬する方法が挙げられる。
浸漬液としては特に制限されず、公知の浸漬液を使用できる。なかでもより優れた本発明の効果が得られる点で、浸漬液としては、水又は有機溶剤を主成分として含有することが好ましく、有機溶剤を主成分として含有することがより好ましい。本明細書において主成分とは、浸漬液の全質量に対して99.9質量%以上含有される成分を意味し、99.99質量%以上含有することがより好ましい。
ケトン系溶剤としては、例えば、アセトン、2-ヘプタノン(MAK)、メチルエチルケトン(MEK)、メチルイソブチルケトン、ジイソブチルケトン、及び、シクロヘキサノン、ジアセトンアルコール等が挙げられるが上記に制限されない。
浸漬液の温度としては特に制限されないが、より優れた本発明の効果が得られる点で、20℃以上が好ましい。
浸漬用容器としては、既に説明したろ過装置において、フィルタユニットが有するハウジングも使用できる。すなわち、ろ過装置が有するハウジングにフィルタ(典型的にはフィルタカートリッジ)を収納した状態で、ハウジング内に浸漬液を満たし、その状態で静置する方法が挙げられる。
また、上記以外にも、浸漬用容器を精製装置が有するハウジングとは別途準備し(すなわち、精製装置外において浸漬用容器を準備し)、別途準備した浸漬用容器に浸漬液を満たし、フィルタを浸漬する方法も挙げられる。
なかでも、フィルタから溶出した不純物がろ過装置内に混入しない点で、ろ過装置外に準備した浸漬用容器に浸漬液を満たし、上記浸漬液にフィルタを浸漬する方法が好ましい。
浸漬用容器の材料としては、特に制限されないが、少なくとも接液部が、既に説明した耐腐食材料で形成されていることが好ましい。
また、浸漬用容器の材料としては、ポリフルオロカーボン(PTFE、PFA:パーフルオロアルコキシアルカン、及び、PCTFE:ポリクロロトリフルオロエチレン等)、PPS(ポリフェニレンスルフィド)、POM(ポリオキシメチレン)、並びに、ポリオレフィン(PP、及び、PE等)からなる群から選択される少なくとも1種を含有することが好ましく、ポリフルオロカーボン、PPS、及び、POMからなる群から選択される少なくとも1種を含有することがより好ましく、ポリフルオロカーボンを含有することが更に好ましく、PTFE、PFA、及び、PCTFEからなる群から選択される少なくとも1種を含有することが特に好ましく、PTFEを含有することが最も好ましい。
また、浸漬用容器は、使用前に洗浄することが好ましく、洗浄の際には浸漬液を使用して洗浄(いわゆる共洗い)することが好ましい。
フィルタに洗浄液を通液して洗浄する方法としては特に制限されないが、例えば、既に説明したろ過装置のフィルタユニットのフィルタハウジングに、フィルタ(典型的にはフィルタカートリッジ)を収納し、上記フィルタハウジングに洗浄液を導入することで、フィルタに洗浄液を通液する方法が挙げられる。
フィルタに洗浄液を通液して洗浄する場合における洗浄液としては特に制限されず、公知の洗浄液が使用できる。なかでも、より優れた本発明の効果が得られる点で、洗浄液の形態としては、既に説明した浸漬液と同様であることが好ましい。
装置洗浄工程は、ろ過工程の前に、ろ過装置の接液部を洗浄する工程である。ろ過工程の前にろ過装置の接液部を洗浄する方法としては特に制限されないが、以下では、フィルタがカートリッジフィルタであり、上記カートリッジフィルタが、流通路上に配置されたハウジング内に収納されるろ過装置を例として説明する。
工程Aは、ハウジングからカートリッジフィルタが取り除かれた状態で、洗浄液を用いてろ過装置の接液部を洗浄する工程である。ハウジングからフィルタが取り除かれた状態で、とは、ハウジングからフィルタカートリッジを取り除くか、ハウジングにフィルタカートリッジを収納する前に、洗浄液を用いてろ過装置の接液部を洗浄することを意味する。
ハウジングからフィルタが取り除かれた状態における(以下「フィルタ未収納の」ともいう。)ろ過装置の接液部を、洗浄液を用いて洗浄する方法としては特に制限されない。流入部から洗浄液を導入し、流出部から回収する方法が挙げられる。
洗浄液としては特に制限されず、公知の洗浄液を使用できる。なかでもより優れた本発明の効果が得られる点で、洗浄液としては、水又は有機溶剤を主成分として含有することが好ましく、有機溶剤を主成分として含有することがより好ましい。本明細書において主成分とは、洗浄液の全質量に対して99.9質量%以上含有される成分を意味し、99.99質量%以上含有することがより好ましい。
工程Bは、ハウジングにフィルタが収納された状態で、洗浄液を用いてろ過装置を洗浄する方法である。
洗浄液を用いてろ過装置を洗浄する方法としては、既に説明した工程Aにおける洗浄方法のほか、ろ過装置に洗浄液を通液する方法も使用できる。ろ過装置に洗浄液を通液する方法としては特に制限されないが、流入部から洗浄液を導入し、流出部から排出すればよい。なお、本工程で使用できる洗浄液としては特に制限されず、工程Aで説明した洗浄液を使用できる。
除電工程は、被精製液を除電することで、被精製液の帯電電位を低減させる工程である。除電方法としては特に制限されず、公知の除電方法を用いることができる。除電方法としては、例えば、被精製液を導電性材料に接触させる方法が挙げられる。
被精製液を導電性材料に接触させる接触時間は、0.001~60秒が好ましく、0.001~1秒がより好ましく、0.01~0.1秒が更に好ましい。導電性材料としては、ステンレス鋼、金、白金、ダイヤモンド、及びグラッシーカーボン等が挙げられる。
被精製液を導電性材料に接触させる方法としては、例えば、導電性材料からなる接地されたメッシュを、流通路を横切るように配置し、ここに被精製液を流通させる方法等が挙げられる。
被精製液準備工程は、ろ過装置の流入部から流入させる被精製液を準備する工程である。被精製液を準備する方法としては特に制限されない。典型的には、市販品(例えば、「高純度グレード品」と呼ばれるもの等)を購入する方法、1種又は2種以上の原料を反応させて得る方法、及び、各成分を溶剤に溶解する方法等が挙げられる。
より具体的には、例えば、酢酸とn-ブタノールとを硫酸の存在下で反応させ、酢酸ブチルを得る方法;エチレン、酸素、及び、水をAl(C2H5)3の存在下で反応させ、1-ヘキサノールを得る方法;シス-4-メチル-2-ペンテンをIpc2BH(Diisopinocampheylborane)の存在下で反応させ、4-メチル-2-ペンタノールを得る方法;プロピレンオキシド、メタノール、及び、酢酸を硫酸の存在下で反応させ、PGMEA(プロピレングリコール1-モノメチルエーテル2-アセタート)を得る方法;アセトン、及び、水素を酸化銅-酸化亜鉛-酸化アルミニウムの存在下で反応させて、IPA(isopropyl alcohol)を得る方法;乳酸、及び、エタノールを反応させて、乳酸エチルを得る方法;等が挙げられる。
図11は蒸留器で予め精製された蒸留済み被精製液を使用して薬液を製造する場合の各装置の関係を表す模式図である。
図11において、ろ過装置400の形態は、既に説明した本発明の第三実施形態に係るろ過装置と同様のため説明は省略する。
タンク401(a)及び各配管の形態は特に制限されず、本発明の実施形態に係るろ過装置が有するタンク及び配管として説明したのと同様の形態のタンク及び配管が使用できる。蒸留器1102の形態は、本発明の実施形態に係る精製装置が有する蒸留器と同様の蒸留器を使用でき、その形態は後述する。
(精製装置)
本工程で使用する精製装置は、既に説明したろ過装置を有する精製装置である。本発明の実施形態に係る精製装置は、既に説明したろ過装置と、第2の流入部と、第2の流出部と、第2の流入部と第2の流出部との間に配置された少なくとも1つの蒸留器と、を有し、上記第2の流出部と既に説明したろ過装置が有する流入部とが接続され、上記第2の流入部から、上記ろ過装置が有する流出部にいたる流通路が形成された精製装置である。以下では、上記精製装置について、図面を示しながら説明する。
なお、下記の説明において、ろ過装置の構成に関する内容は、既に説明した内容と同様であり説明を省略する。
図12は本発明の精製装置の第一実施形態を表す模式図である。精製装置1200は、第2の流入部1201と、第2の流出部1202と、第2の流入部1201と第2の流出部1202との間に配置された蒸留器1203と、を有し、第2の流出部1202が、ろ過装置が有する流入部101と接続されている。これにより精製装置1200においては、第2の流入部1201、蒸留器1203、第2の流出部1202、流入部101、フィルタ103(フィルタA)、配管105、フィルタ104(フィルタBD)、及び、流出部102により流通路S12が形成されている。
すなわち、蒸留器1203が、ろ過装置100の流入部101に接続されている。
図13は精製装置の第二実施形態を表す模式図である。精製装置1300は、第2の流入部1301と、第2の流出部1302と、第2の流入部1301と第2の流出部1302との間に直列に配置された蒸留器1303及び蒸留器1304と、を有し、第2の流出部1302が、ろ過装置が有する流入部101と接続されている。これにより精製装置1300においては、第2の流入部1301、蒸留器1303、配管1305、蒸留器1304、第2の流出部1302、流入部101、フィルタ103(フィルタA)、配管105、フィルタ104(フィルタBD)、及び、流出部102により流通路S13が形成されている。
すなわち、本実施形態に係る精製装置は、直列に接続された複数の蒸留器を含む。なお、直列に接続された蒸留器を3つ以上含む場合は、最後段の蒸留器がろ過装置と接続される。
次に、耐腐食材料について説明する。これまで説明した本発明の実施形態に係るろ過装置、及び、精製装置は、その接液部の少なくとも一部が耐腐食材料で形成されていることが好ましく、接液部の90%以上が耐腐食材料で形成されていることがより好ましく、接液部の99%以上が耐腐食材料で形成されていることが更に好ましい。
金属材料としては例えば、ステンレス鋼、及びNi-Cr合金等が挙げられる。
Ni-Cr合金としては、例えば、ハステロイ(商品名、以下同じ。)、モネル(商品名、以下同じ)、及びインコネル(商品名、以下同じ)等が挙げられる。より具体的には、ハステロイC-276(Ni含有量63質量%、Cr含有量16質量%)、ハステロイ-C(Ni含有量60質量%、Cr含有量17質量%)、ハステロイC-22(Ni含有量61質量%、Cr含有量22質量%)等が挙げられる。
また、Ni-Cr合金は、必要に応じて、上記した合金の他に、更に、B、Si、W、Mo、Cu、及び、Co等を含有していてもよい。
なお、金属材料はバフ研磨されていてもよい。バフ研磨の方法は特に制限されず、公知の方法を用いることができる。バフ研磨の仕上げに用いられる研磨砥粒のサイズは特に制限されないが、金属材料の表面の凹凸がより小さくなりやすい点で、#400以下が好ましい。なお、バフ研磨は、電解研磨の前に行われることが好ましい。
本発明の第二の実施形態に係る薬液の製造方法は、被精製液を精製して薬液を得る、薬液の製造方法であって、被精製液を、ポリテトラフルオロエチレン製の多孔質基材と、基材の少なくとも一部を覆うように形成されたペルフルオロスルホン酸ポリマーを含有する非架橋コーティングとを有する第1多孔質膜、及び、ペルフルオロスルホン酸ポリマーとブレンドされたポリテトラフルオロエチレンを含有する第2多孔質膜、からなる群より選択される少なくとも1種を含むフィルタA、並びに、フィルタAとは異なるフィルタB、を用いてろ過して薬液を得る工程を有する、薬液の製造方法である。
本実施形態に係る薬液の製造方法は、被精製液をフィルタA及びフィルタAとは異なるフィルタBを用いてろ過する。被精製液をろ過する際、フィルタA、フィルタBの順に通液してもよいし、フィルタB、フィルタAの順に通液してもよい。
なお、本実施形態に係る薬液の製造方法としては、フィルタA及びフィルタBを用いていれば特に制限されず、複数のフィルタA、及び/又は、複数のフィルタBを順番に用いて被精製液をろ過してもよい。
上記ろ過装置を用いて製造される薬液は半導体基板の製造に用いられることが好ましい。特に、ノード10nm以下の微細パターンを形成するため(例えば、EUVを用いたパターン形成を含む工程)に用いられることがより好ましい。
言い換えれば、上記ろ過装置は、半導体基板の製造用の薬液の製造に用いられることが好ましく、具体的には、リソグラフィー工程、エッチング工程、イオン注入工程、及び、剥離工程等を含有する半導体デバイスの製造工程において、各工程の終了後、又は、次の工程に移る前に、無機物、及び/又は、有機物を処理するために使用され、具体的には洗浄液、エッチング液、リンス液、前処理液、レジスト液、プリウェット液、及び、現像液等の製造に用いられることがより好ましく、洗浄液、エッチング液、リンス液、前処理液、及び、レジスト液からなる群より選択される少なくとも1種の製造に用いられることが好ましい。
また、上記ろ過装置は、レジスト液に含有される樹脂の希釈液、レジスト液に含有される溶剤の製造にも使用できる。
また、上記ろ過装置は、医療用途又は洗浄用途の溶媒の製造にも使用できる。特に、容器、配管、及び、基板(例えば、ウェハ、及び、ガラス等)等の洗浄に用いる薬液の製造に使用できる。
なかでも、上記ろ過装置は、EUV(極紫外線)を用いたパターン形成における、プリウェット液、現像液、及び、リンス液からなる群より選択される少なくとも1種の製造に使用するのが好ましい。
上記ろ過装置により製造された薬液は、容器に収容されて使用時まで保管されてもよい。このような容器と、容器に収容された薬液とをあわせて薬液収容体という。保管された薬液収容体からは、薬液が取り出され使用される。
使用可能な容器としては、特に制限されないが、例えば、アイセロ化学(株)製の「クリーンボトル」シリーズ、及び、コダマ樹脂工業製の「ピュアボトル」等が挙げられるが、これらに制限されない。
図14に記載した精製装置を使用して、薬液1を製造した。図14の精製装置は、流入部と流出部の間に、フィルタBU-1、タンクT-1、フィルタBU-2、フィルタF-A、タンクT-2、フィルタBD-1、及び、フィルタBD-2が、直列に接続されたろ過装置と、上記ろ過装置の前段に接続された蒸留器(D1及びD2の2連の蒸留器、表1中では「2連式」と記載した。)とを有する。各ユニットは配管と共に流通路S-14を形成するとともに、流通路S-14においてフィルタF-A(フィルタF-Aは既に説明したフィルタAに該当する)の下流側からタンクT-1へと、被精製液を返送可能な返送流通路R-14-1が形成され、流通路S-14において、フィルタBD-2の下流側からタンクT-2へと、被精製液を返送可能な返送流通路R-14-2が形成されている。
なお、薬液1の製造に用いた各フィルタが含有する材料成分、及び、孔径は表1に示した。
・PFSA/PTFE:
市販品のEntegris, inc., 製Fluoroguard AT(孔径20nm、又は、200nm)を、0.25%のPFSA溶液(アクイヴィオンPFSA 24:D83-24B Solvay Plastics)をメタノール水溶媒中で調製したポリマー液へ十分濡れるまで浸漬した後、水切りし、その後乾燥させて、超純水を用いて24時間洗浄して得たもの。なお、フィルタの臨界湿潤表面張力は、PFSA溶液中におけるPFSAの含有量を制御して調整した。
・PP:ポリプロピレン
・IEX:ポリエチレン製の基材に、陽イオン交換基を導入して得られたフィルタ
・Nylon:ナイロン
・UPE:超高分子量ポリエチレン
・PTFE:ポリテトラフルオロエチレン
・PFSA/PTFEブレンド
PFSA添加剤(アクイヴィオンPFSA 24:D83-24B SolvayPlastics)を適量のPTFE樹脂と混合し、平衡化させた後、加圧してビレットを作成し、押し出し成型でシート状PTFEを作成し、所定の孔径となるように延伸して得たもの。なお、フィルタの臨界湿潤表面張力は、PFSA添加剤の量を制御して調整した。
・CHN:シクロヘキサノン
・PGMEA/PGME(7:3):PGMEAとPGMEの7:3(体積基準)の混合物
・nBA:酢酸ブチル
・PC/PGMEA(1:9):PCとPGMEAの1:9(体積基準)の混合物
・EL:乳酸エチル
・MIBC:4-メチル-2-ペンタノール
・IPA:イソプロパノール
表1に記載した精製装置(又はろ過装置)を用いて、表1に記載した各被精製物を精製して薬液を得た。なお、各精製装置(又はろ過装置)は、図15~図27に示した。フィルタF-A、フィルタBU-1~BU-3、フィルタBD-1~BD-2の材料成分及び孔径は表1に示したとおりである。なお、被精製液の精製に際して、使用したろ過装置にR-(数字)で示した返送流通路が形成されているものは、それぞれの返送流通路について3回循環ろ過した。
また、表1には、フィルタF-Aの臨界湿潤表面張力(CWST)も合わせて記載した。なお、表中、「-」はそのフィルタを使用しなかったことを意味し、本願明細書における他の表についても同様である。
直径約300mmのシリコンウェハ(Bare-Si)上に、薬液1をスピン塗布し、薬液塗布済みウェハを得た。使用した装置は、Lithius ProZであり、塗布の条件は以下のとおりだった。
・塗布の際のシリコンウェハの回転数:2,200rpm、60sec
SP-5にて計測された全欠陥の増加数を残渣欠陥数として計上し、G6にて形状観測を行い、粒子状ではないもの(シミ状)の欠陥をシミ状欠陥として計上した。結果は以下の基準により評価し、表1に示した。
なお、ウェハ上に存在する欠陥の数が少ないほど、薬液はより優れた欠陥抑制性能を有する。なお、以下の評価において、「欠陥数」とは、それぞれ残渣欠陥数、及び、シミ状欠陥数を表す。上記と同様の方法により薬液2~48についても評価した。結果を表1に示した。
A 欠陥数が30個/ウェハを超え、50個/ウェハ以下だった。
B 欠陥数が50個/ウェハを超え、100個/ウェハ以下だった。
C 欠陥数が100個/ウェハを超え、200個/ウェハ以下だった。
D 欠陥数が200個/ウェハを超え、500個/ウェハ以下だった。
E 欠陥数が500個/ウェハを超えた。
薬液1をプリウェット液として用いて、薬液のブリッジ欠陥抑制性能を評価した。まず、使用したレジスト組成物について説明する。
レジスト樹脂組成物は、以下の各成分を混合して得た。
PGMEA(プロピレングリコールモノメチルエーテルアセテート):3質量部
シクロヘキサノン:600質量部
γ-BL(γ-ブチロラクトン):100質量部
次に試験方法について説明する。まず、約300mmのシリコンウェハを薬液1でプリウェットし、次に、上記レジスト樹脂組成物を上記プリウェット済みシリコンウェハに回転塗布した。その後、ホットプレート上で150℃にて90秒間加熱乾燥を行い、9μmの厚みのレジスト膜を形成した。
このレジスト膜に対し、縮小投影露光及び現像後に形成されるパターンのライン幅が30nm、スペース幅が30nmとなるような、ラインアンドスペースパターンを有するマスクを介して、ArFエキシマレーザースキャナー(ASML製、PAS5500/850C波長248nm)を用いて、NA=0.60、σ=0.75の露光条件でパターン露光した。照射後に120℃にて60秒間ベークして、その後、現像、及び、リンスし、110℃にて60秒ベークして、ライン幅が30nm、スペース幅が30nmのレジストパターンを形成した。
A ブリッジ欠陥数が1個/cm2以上、2個/cm2未満だった。
B ブリッジ欠陥数が2個/cm2以上、5個/cm2未満だった。
C ブリッジ欠陥数が5個/cm2以上、10個/cm2未満だった。
D ブリッジ欠陥数が10個/cm2以上、15個/cm2未満だった。
E ブリッジ欠陥数が15個/cm2以上だった。
上記レジストパターンについて、測長SEM(CG4600, Hitach-HighTech)にて、パターンを100ショット分取得し、LWR(Line Width Roughness)の平均値と最大(又は最小)線幅との差を求めた。結果は以下の基準により評価し、表1に示した。なお、上記「差」が小さいほど、薬液は、より優れたパターン幅の均一性能を有する。なお、「LWRの平均値と最大(又は最小)線幅との差」は、LWRの平均値と最大線幅と、LWRの平均値と最小線幅の差のうち、絶対値が大きい値を採用した。
A 線幅の平均値と最大(最小)との差が、平均値に対して±5%未満だった。
B 線幅の平均値と最大(最小)との差が、平均値に対して±10%未満だった。
C 線幅の平均値と最大(最小)との差が、平均値に対して±20%未満だった。
D 線幅の平均値と最大(最小)との差が、平均値に対して±20%以上だった。
E 線幅の測定ができないショットが含まれていた。
表1に記載した各精製装置(又はろ過装置)を用いて被精製液を連続して精製した。被精製液を通液して精製装置(又はろ過装置)の状態が安定した後、すぐに得られた薬液を試験用(初期サンプル)として回収し、その後、通液量10000kgごとに精製後に得られた薬液を試験用(経時サンプル)として回収した。試験用に回収した薬液は、「評価1」で説明した薬液の残渣欠陥抑制性能の評価法により評価し、単位面積当たりの欠陥数を初期サンプルと比較して、経時サンプルの欠陥数が2倍となったときの通液量をフィルタの「寿命」とした。図26に記載したろ過装置を使用した場合の寿命を1とし、各装置のフィルタの寿命を比で評価した。結果は以下の基準により評価し、表1に示した。なお、図26の装置については評価結果に「基準」と表記した。
A 寿命が5倍以上、10倍未満だった。
B 寿命が2倍以上、5倍未満だった。
C 寿命が1倍以上、2倍未満だった。
D 寿命が1倍未満だった。
表1に記載した各精製装置(又はろ過装置)を用いて被精製液を連続して精製した。被精製液を通液して精製装置(又はろ過装置)の状態が安定した後、単位時間当たりの被精製液の流量(フローレート)を一定とし、各精製装置(又はろ過装置)が有するフィルタのうち、少なくとも1つのフィルタにかかる差圧が初期値の1.1倍を超えたときを、フィルタの交換時期とした。
通算5,000tonの薬液を製造するために必要とした全フィルタの交換回数を以下の基準により評価し、表1の「生産性コスト」欄に記載した。なお、交換回数がより少ないほど生産性コストはより低く、好ましい。言い換えれば、交換回数がより少ないほど、ろ過装置はより優れた生産性を有する。
B:交換回数が3回以上、6回以下だった。
C:交換回数が7回以上だった。
被精製液として、SPM(Sulfuric acid-Hydrogen Peroxide Mixture)、リン酸水溶液(リン酸含有量85質量%)、及び、2.38%水酸化テトラメチルアンモニウム水溶液(表2中、「TMAH」と記載した。)を購入して準備した。
次に、図28に記載したろ過装置を使用して、薬液50、51を製造した。図28のろ過装置は、流入部と流出部の間に、フィルタBU-1、フィルタBU-2、フィルタF-A、フィルタBD-1、及び、フィルタBD-2が、直列に接続され、流通路S-28が形成されたろ過装置である。なお、図28のろ過装置における各フィルタが含有する材料成分、及び、孔径は表2に示した。
なお、表2中におけるフィルタの材料成分に係る略号は、表1と同様であり、説明を省略する。
図28に記載したろ過装置に代えて、図29に記載したろ過装置(フィルタF-Aを有し、流通路S-29が形成されている)を用いたこと以外は、薬液50及び薬液51と同様にして、薬液52及び薬液53を製造した。フィルタF-Aの材料成分等については、表2に示した。
直径約300mmのベアシリコンウェハを準備し、各薬液を用いて3分間処理して、処理済みウェハを得た。次に、KLA-Tencor社製のウェハ検査装置「SP-5」とアプライドマテリアル社の全自動欠陥レビュー分類装置「SEMVision G6」を用いて、薬液塗布済みウェハの全面に存在する30nm以上のサイズの欠陥の数、及び、その組成を調べた。
計測された欠陥のうち、金属原子が検出された欠陥をメタル残渣欠陥として計上し、残渣欠陥数全体に対するメタル欠陥数の個数比を求めた。結果は、以下の基準により評価し、結果を欠陥数と共に表2に示した。
B メタル欠陥数/残渣欠陥数が、1.5%を超え、2.0%以下だった。
C メタル欠陥数/残渣欠陥数が、2.0%を超え、3.0%以下だった。
D メタル欠陥数/残渣欠陥数が、3.0%を超え、4.0%以下だった。
E メタル欠陥数/残渣欠陥数が、4.0%を超えた。
被精製液として、以下の成分を含有するレジスト樹脂組成物2を準備した。
レジスト樹脂組成物2は、以下の各成分をそれぞれ混合したものである。
次に、反応容器中に69.5gのシクロヘキサノンを入れ、窒素ガス雰囲気下、85℃に保持した反応容器中のシクロヘキサノンに混合液を4時間かけて滴下して、反応液を得た。反応液を2時間に亘って加熱しながら撹拌した後、反応液を室温まで放冷した。次に、反応液に、メタノール49.6gと4.9gのトリエチルアミンとを加え、50℃で18時間加熱撹拌した後、反応液を室温まで放冷した。次に、反応液に酢酸エチル200gと水200gとを加え、分液操作し、有機層を回収した。有機層を水で3回洗浄した後、溶媒を減圧留去した。残った固体をPGMEA(プロピレングリコールモノメチルエーテルアセテート)200gに溶解し、溶媒を減圧留去することで共沸脱水した後、シクロヘキサノン198.5gを加え、溶液を得た。次に、溶液を、2336gの、n-ヘプタン及び酢酸エチルの混合溶液(n-ヘプタン/酢酸エチル=9/1(質量比))中に滴下し、固体を沈殿させ、ろ過した。次に、701gの、n-ヘプタン及び酢酸エチルの混合溶液(n-ヘプタン/酢酸エチル=9/1(質量比))を用いて、ろ過した固体のかけ洗いを行なった。その後、洗浄後の固体を減圧乾燥して、23.8gの樹脂(A-1)を得た。1H-NMR及び13C-NMRより、樹脂中の組成比は、繰り返し単位(a)/繰り返し単位(c)/繰り返し単位(b)=30/20/50(モル比)と算出された。なお、スキームには、樹脂の合成方法を簡略化して表した。
PGMEA(プロピレングリコールモノメチルエーテルアセテート):60g
PGME(プロピレングリコールモノメチルエーテル):15g
表3に記載した各フィルタを使用したことを除いては、薬液60と同様にして、薬液61、薬液62を製造した。
図30に記載したろ過装置に代えて、図29に記載したろ過装置を用いたこと以外は薬液60と同様にして、薬液63を製造した。なお、ろ過に使用したフィルタは表3に記載したとおりである。
得られた薬液について、Agilent社製ICP-MS 8900を用いて金属成分の含有量を測定した。結果を表3に示した。なお、表3中には、特定の金属成分の薬液の全質量に対する含有量(質量ppb)と金属成分の総合計量(質量ppb)をあわせて記載した。なお、表3中、「<0.01」とは、結果が検出限界値未満たったことを表わしている。
次に、EUV露光装置(Exitech社製 Micro Exposure Tool、NA0.3、Quadrupole、アウターシグマ0.68、インナーシグマ0.36)を用いて、露光マスク(ライン/スペース=1/1を有するスペース幅(光透過部の幅)=10nmマスク)を使用して、レジスト膜を備えるシリコンウェハをパターン露光した。パターン露光後、加熱したホットプレート上に、露光後のレジスト膜を備えるシリコンウェハを、シリコンウェハ面を下にして載置し、90℃で60秒間ベークした。ベーク後のレジスト膜を、現像液で30秒間パドル現像して、その後、リンスした。次いで、2000rpmの回転数で30秒間ウェハを回転させて、1:1ラインアンドスペースパターンを得た。
A スカム欠陥数が1個/cm2以上、2個/cm2未満だった。
B スカム欠陥数が2個/cm2以上、5個/cm2未満だった。
C スカム欠陥数が5個/cm2以上、10個/cm2未満だった。
D スカム欠陥数が10個/cm2以上、20個/cm2未満だった。
E スカム欠陥数が20個/cm2以上だった。
表1には、各グループの4つの分割表の対応する行にわたって、各薬液の精製に用いたろ過装置(又は精製装置)が有するフィルタ、及び、得られた薬液の評価結果が記載されている。
例えば、表1の第1グループ:表1(1-1)~表1(1-4)のそれぞれの1行目には、薬液1について記載されている。
これは、薬液1が、図14に記載した精製装置により製造されたことを示し、薬液1の製造に用いた被精製液は、CHN(シクロヘキサノン)を含有することを示している。また、薬液1の製造に用いた精製装置のフィルタは、「PGMEA 1day浸漬」の条件で事前に洗浄されたことを示している。また、精製装置は、2連式の蒸留器と、BU-1(流通路の最も上流側に配置されたPPを含有する孔径200nmのフィルタ)、BU-2(BU-1の下流側に配置された孔径15nmのIEXフィルタ)、とを有し、フィルタA(F-A)の上流側にタンクTU-1を有し、F-A(フィルタA)としては、孔径20nmのPFSA/PTFEフィルタを有し、そのCWSTは35×10-5N/cmであり、フィルタF-Aの下流側には、BD-1(ナイロンを含有する孔径10nmのフィルタ)、BD-2(UPEを含有する孔径3nmフィルタ)を有し、更に、フィルタF-Aの下流側には、タンクTD-1を有することを示している。
更に薬液1は残渣欠陥抑制性能がAA、シミ状欠陥抑制性能がAA、ブリッジ欠陥抑制性能がAA、パターン幅の均一性能がAA、そして、精製装置のフィルタの寿命がAAで、生産性コストはAであったことを示している。
薬液2~30については、同様に第1グループの各表に結果が記載され、薬液31~48については、第2グループの各表に結果が記載されている。
例えば、各分割表のそれぞれの1行目には、薬液50について記載されている。
これは、薬液50が図28に記載されたろ過装置により製造されたことを示し、薬液50の製造に用いた被精製液は、SPM(4:1)であることを示している。また、SPM(4:1)のpHは1.0以下だったことを示している。また、薬液50の製造に用いたろ過装置のフィルタは「PGMEA 1day浸漬」の条件で事前に洗浄されたことを示している。また、ろ過装置は、BU-1(PTFEを含有する孔径200nmのフィルタ)、BU-2(PTFEを含有する孔径20nmのフィルタ)を有し、F-A(フィルタA)としては、孔径20nmのPFSA/PTFEフィルタ(CWST:35×10-5N/cm)を有し、その下流側には、BD-1(PTFEを含有する孔径10nmのフィルタ)、BD-2(PTFEを含有する孔径10nmのフィルタ)を有することを示している。
薬液50の評価は、残渣欠陥数が2932個/ウェハであり、そのうち、メタル残渣欠陥数が36個/ウェハであり、比率が1.2%、評価がAだったことを示している。
薬液51~薬液54についても同様に表2の各表に結果が記載されている。
例えば、各分割表のそれぞれの1行目には、薬液60について記載されている。
これは、薬液60が図30に記載されたろ過装置により製造されたことを示し、薬60の製造に用いた被精製液は、レジスト樹脂組成物2であることを示している。また、薬液60の製造に用いたろ過装置のフィルタは「PGMEA 1day浸漬」の条件で事前に洗浄されたことを示している。また、ろ過装置は、BU-1(PTFEを含有する孔径20nmのフィルタ)、BU-2(UPEを含有する孔径2nmのフィルタ)、BU-3(Nylonを含有する孔径10nmのフィルタ)を有し、F-A(フィルタA)としては、孔径20nmのPFSA/PTFE(CWST:35×10-5N/cm)フィルタを有し、その下流側には、BD-1(UPEを含有する孔径2nmのフィルタ)を有することを示している。
薬液60は、薬液の全質量に対してMgを0.09質量ppb含有し、Caを0.37質量ppb含有し、Crの含有量は検出限界値未満であり、Feを0.15質量ppb含有し、Niの含有量は検出限界値未満であり、金属成分の合計含有量としては薬液の全質量に対して0.61質量ppbであったことを示している。
また、薬液60のスカム欠陥抑制性能はAAだったことを示している。
また、フィルタBDが20nm以下の孔径を有するフィルタを含むろ過装置(を含む精製装置)を用いて製造された薬液45は、薬液44と比較して、より優れた残渣欠陥抑制性能、及び、より優れたブリッジ欠陥抑制性能を有していた。
また、最も下流側に配置されたフィルタBDが10nm以下の孔径を有するろ過装置(を含む精製装置)を用いて製造された薬液1は、薬液7と比較して、より優れた欠陥抑制性能、より優れたブリッジ欠陥抑制性能、及び、より優れたパターン幅の均一性能を有していた。また、同じく薬液1は、薬液46と比較して、より優れた残渣欠陥抑制性能、より優れたシミ状欠陥抑制性能、より優れたブリッジ欠陥抑制性能、及び、より優れたパターン幅の均一性能を有していた。
また、少なくとも1つのBDフィルタのうちのいずれかのフィルタBDからなる基準フィルタの下流側から、上記基準フィルタの上流側へと被精製液を返送可能な返送流通路を有するろ過装置(を含む精製装置)を用いて製造された薬液1は、薬液14と比較して、より優れた残渣欠陥抑制性能、より優れたブリッジ欠陥抑制性能、及び、より優れたパターンパ場の均一性能を有していた。
また、フィルタBが、流通路上においてフィルタAの上流側に配置されたフィルタBUを含むろ過装置(を含む精製装置)を用いて製造された薬液1は、薬液47と比較して、より優れた残渣欠陥抑制性能、より優れたシミ状欠陥抑制性能、より優れたブリッジ欠陥抑制性能、より優れたパターン幅の均一性能を有していた。
また、フィルタBUの少なくとも1つが10nm以上の孔径を有する、ろ過装置(を含む精製装置)を用いて製造された薬液1は、薬液48と比較して、より優れた残渣欠陥抑制性能を有していた。また、薬液1の製造に用いたろ過装置(を含む精製装置)は、薬液48の製造装置の製造に用いたろ過装置(を含む精製装置)と比較して生産性コストがより低かった(より優れた生産性を有していた)。
また、少なくとも1つのフィルタBUの孔径が20nm以上である、薬液1の製造に用いたろ過装置(を含む精製装置)は、薬液2及び薬液6の製造に用いたろ過装置と比較して、生産性コストがより低かった(より優れた生産性を有していた)。
また、フィルタBUがイオン交換基を有する樹脂を含有するろ過装置(を含む精製装置)を用いて製造された、薬液1は、薬液12と比較して、より優れた残渣欠陥抑制性能、より優れたブリッジ欠陥抑制性能、より優れたパターン幅の均一性能を有していた。また、薬液1の製造に用いたろ過装置(を含む精製装置)は、薬液12の製造に用いたろ過装置(を含む精製装置)と比較してフィルタの寿命がより長く、また、生産性コストがより低かった(より優れた生産性を有していた)。
また、タンクに対して流通路の上流側にタンクと直列に配置された孔径10nm以上のフィルタを有するろ過装置(を含む精製装置)を用いて製造された薬液1は、薬液48と比較して、より優れた残渣欠陥抑制性能を有していた。また、薬液1の製造に用いたろ過装置(を含む精製装置)は、薬液48の製造に用いたろ過装置(を含む精製装置)と比較して、生産性コストがより低かった(より優れた生産性を有していた)。
また、pHが0~9の範囲内である被精製液を精製して得られた薬液50は、薬液54と比較してより優れた欠陥抑制性能を有していた。これは、本発明の実施形態に係るろ過装置が、pHが0~9の範囲内である被精製液の精製用としてより優れた効果を有することを示している。
101 流入部
102 流出部
103、104、201、601、104-1、104-2 フィルタ
105、202、301、302、402、501、502、602、701、801、802、803、804,901、1001、1002、1104、1105、1305 配管
401、401(a)、401(b) タンク
1100 製造場
1101 蒸留装置
1102、1203、1303、1304 蒸留器
1103 可搬型タンク
1106 運搬手段
1200、1300 精製装置
1201、1301 第2の流入部
1202、1302 第2の流出部
Claims (26)
- 流入部と、
流出部と、
フィルタAと、
前記フィルタAとは異なる少なくとも1つのフィルタBと、を有し、
前記フィルタA及び前記フィルタBは、前記流入部及び前記流出部の間に直列に配置され、前記流入部から前記流出部にいたる流通路を有する、被精製液を精製して、薬液を得るためのろ過装置であって、
前記フィルタAは、
ポリテトラフルオロエチレン製の多孔質基材と、前記多孔質基材を覆うように形成されたペルフルオロスルホン酸ポリマーを含有する非架橋コーティングとを有する第1多孔質膜、及び、
ペルフルオロスルホン酸ポリマーとブレンドされたポリテトラフルオロエチレンを含有する第2多孔質膜、
からなる群より選択される少なくとも1種を含む、ろ過装置。 - 前記フィルタBは、前記流通路上において、前記フィルタAの下流側に配置されたフィルタBDを少なくとも1つを含む、請求項1に記載のろ過装置。
- 少なくとも1つの前記フィルタBDは、20nm以下の孔径を有する、請求項2に記載のろ過装置。
- 少なくとも1つの前記フィルタBDがポリオレフィン、ポリアミド、ポリフルオロカーボン、ポリスチレン、ポリスルホン、及び、ポリエーテルスルホンからなる群より選択される少なくとも1種を含有する、請求項2又は3に記載のろ過装置。
- 前記流通路上において、最も下流側に配置された前記フィルタBDが、10nm以下の孔径を有し、ポリテトラフルオロエチレン、ポリエチレン、及び、ナイロンからなる群より選択される少なくとも1種を含有する、請求項2~4のいずれか一項に記載のろ過装置。
- 少なくとも1つの前記フィルタBDのうち、いずれかのフィルタBDからなる基準フィルタの下流側から、前記基準フィルタの上流側へと、前記被精製液を返送可能な返送流通路を有する、請求項2~5のいずれか一項に記載のろ過装置。
- 前記フィルタBは、前記流通路上において前記フィルタAの上流側に配置されたフィルタBUを少なくとも1つ含む、請求項1~6のいずれか一項に記載のろ過装置。
- 少なくとも1つの前記フィルタBUは、10nm以上の孔径を有する、請求項7に記載のろ過装置。
- 少なくとも1つの前記フィルタBUは、20nm以上の孔径を有する、請求項7又は8に記載のろ過装置。
- 前記フィルタBUが、イオン交換基を有する樹脂を含有する、請求項7~9のいずれか一項に記載のろ過装置。
- 前記イオン交換基が、陰イオン交換基を含む、請求項10記載のろ過装置。
- 前記流通路上に、前記フィルタAと直列に配置されたタンクを更に有する請求項1~11のいずれか一項に記載のろ過装置。
- 前記タンクに対して前記流通路の上流側に、
前記タンクと直列に配置された、孔径10nm以上のフィルタCを更に有する請求項12に記載のろ過装置。 - 前記タンクに対して前記流通路の上流側に、
前記タンクと直列に配置された、孔径20nm以上のフィルタCを更に有する請求項12に記載のろ過装置。 - 前記流通路上における、前記フィルタAの下流側から、前記フィルタAの上流側へと、
前記被精製液を返送可能な返送流通路を有する、請求項1~14のいずれか一項に記載のろ過装置。 - 前記被精製液のpHが0~9である、請求項1~15のいずれか一項に記載のろ過装置。
- 前記薬液が、洗浄液、エッチング液、リンス液、前処理液、及び、レジスト液からなる群より選択される少なくとも1種である、請求項1~16のいずれか一項に記載のろ過装置。
- 前記フィルタAの臨界湿潤表面張力が27×10-5N/cm以上である、請求項1~17のいずれか一項に記載のろ過装置。
- 前記フィルタAの臨界湿潤表面張力が30×10-5N/cm以上である、請求項1~18のいずれか一項に記載のろ過装置。
- 被精製液を精製して、半導体基板製造用の薬液を製造するためのろ過装置であって、
流入部と、流出部と、
フィルタAと、前記フィルタAとは異なる少なくとも1つのフィルタBと、を有し、
前記フィルタA及び前記フィルタBは、前記流入部及び前記流出部の間に直列に配置され、前記流入部から前記流出部にいたる流通路を有するろ過装置であって、
前記フィルタAは、
ポリテトラフルオロエチレン製の多孔質基材と、前記多孔質基材の少なくとも一部を覆うように形成されたペルフルオロスルホン酸ポリマーを含有する非架橋コーティングとを有する第1多孔質膜、及び、
ペルフルオロスルホン酸ポリマーとブレンドされたポリテトラフルオロエチレンを含有する第2多孔質膜、からなる群より選択される少なくとも1種を含む、ろ過装置。 - 請求項1~20のいずれか一項に記載のろ過装置と、
前記ろ過装置の前記流入部に接続された少なくとも1つの蒸留器と、
を有する精製装置。 - 前記少なくとも1つの蒸留器は、直列に接続された複数の蒸留器を含む、
請求項21に記載の精製装置。 - 被精製液を精製して薬液を得る、薬液の製造方法であって、請求項1~20のいずれか一項に記載のろ過装置を用いて、被精製液を精製して薬液を得る、ろ過工程を有する、薬液の製造方法。
- 前記ろ過工程の前に、前記フィルタA、及び、前記フィルタBを洗浄するフィルタ洗浄工程を更に有する、請求項23に記載の薬液の製造方法。
- 前記ろ過工程の前に、前記ろ過装置の接液部を洗浄する装置洗浄工程を更に有する、請求項23又は24に記載の薬液の製造方法。
- 被精製液を精製して薬液を得る、薬液の製造方法であって、
前記被精製液を、
ポリテトラフルオロエチレン製の多孔質基材と、前記多孔質基材の少なくとも一部を覆うように形成されたペルフルオロスルホン酸ポリマーを含有する非架橋コーティングとを有する第1多孔質膜、及び、ペルフルオロスルホン酸ポリマーとブレンドされたポリテトラフルオロエチレンを含有する第2多孔質膜、からなる群より選択される少なくとも1種を含むフィルタA、及び、
前記フィルタAとは異なるフィルタB、を用いてろ過して薬液を得る工程を有する、薬液の製造方法。
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