Filter, filter manufacturing method, filtration device, and chemical liquid manufacturing method

Abstract

To provide: a filter the allows manufacture of a chemical solution excellent in preventing defects; and a filter manufacturing method, a filtering device, and a chemical solution manufacturing method.SOLUTION: The filter is used for filtering and contains a filter body and one or more first organic compounds selected from the group consisting of: compounds represented by general formulas (I) to (V); alkanes represented by general formula (X); and alkenes represented by general formulas (XI) and (XII). The total content of the first organic compounds is 0.10 to 10000 ppt by mass with respect to the mass of the filter.SELECTED DRAWING: None

Description

[Technical field]

[0001] The present invention relates to a filter, a method for manufacturing a filter, a filtering device, and a method for manufacturing a chemical solution. [Background technology]

[0002] When manufacturing semiconductor devices, chemical liquids containing water and / or organic solvents are used as pre-wet liquids, resist liquids (resist compositions), developing liquids, rinsing liquids, stripping liquids, chemical mechanical polishing (CMP) slurries, and post-CMP cleaning liquids, or as diluting liquids for these liquids. In recent years, with the increasing sophistication of semiconductor products, the above-mentioned chemicals used in semiconductor manufacturing are required to have even greater defect suppression properties.

[0003] As for chemicals used in conventional semiconductor manufacturing processes, Patent Document 1 discloses a "manufacturing method for an organic processing liquid for patterning a chemically amplified resist film, capable of reducing particle generation in a pattern formation technique (paragraph

[0010] )," and in the manufacturing method, a "filter having a filtration membrane (claim 1)" is used. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] JP 2015-84122 A Summary of the Invention [Problem to be solved by the invention]

[0005] The present inventors have found that there is room for improvement in terms of defect suppression properties when using the organic processing liquid (chemical liquid) for patterning produced by the above-mentioned production method. In view of the above, an object of the present invention is to provide a filter capable of producing a chemical solution having excellent defect suppression properties, as well as a method for producing a filter, a filtering device, and a method for producing a chemical solution. [Means for solving the problem]

[0006] As a result of intensive research by the present inventors to solve the above problems, they have found that the above problems can be solved by the following configuration.

[0007] [1] A filter for filtration, A filter body; One or more first organic compounds selected from the group consisting of compounds represented by general formulas (I) to (V), alkanes represented by general formula (X), and alkenes represented by general formulas (XI) and (XII), A filter, wherein the total content of the first organic compounds is 0.10 to 10,000 ppt by mass relative to the mass of the filter. [2] The filter according to [1], further comprising at least one second organic compound selected from the group consisting of compounds represented by general formulas (VI) to (VIII). [3] The total content of the first organic compound is 5.0 ppt by mass or more relative to the mass of the filter, and The filter according to [2], wherein the total content of the compounds selected from the group consisting of the compounds represented by the general formulas (I) to (VIII), the alkanes represented by the general formula (X), and the alkenes represented by the general formulas (XI) and (XII) is 6,500 ppt by mass or less, relative to the mass of the filter. [4] The above filter, One or more compounds selected from Group A consisting of compounds represented by general formulas (I) to (VIII); The filter according to [2] or [3], comprising one or more compounds selected from Group B consisting of an alkane represented by general formula (X) and alkenes represented by general formulas (XI) and (XII). [5] The filter according to [4], wherein the total content of the compounds selected from the above Group A is 0.10 to 3200 mass ppt with respect to the mass of the above filter. [6] The filter according to [4] or [5], wherein the total content of the compounds selected from the above Group B is 1.0 to 1200 mass ppt with respect to the mass of the above filter. [7] Furthermore, the filter according to any one of [1] to [6], which contains a metal component selected from the group consisting of Al, Ca, Cr, Cu, Fe, K, Mg, Na, Ni, Zn, and Pb in an amount of 0.10 to 5000 mass ppt with respect to the mass of the above filter. [8] The above filter body contains nylon, The filter according to any one of [4] to [6], which contains one or more compounds selected from the above Group A and two or more compounds selected from the above Group B. [9] It contains an alkane represented by the general formula (X) and an alkene represented by the general formula (XI), For the filter according to [8], the content A of the alkane represented by the general formula (X), the content B of the alkene represented by the general formula (XI), and the content C of the alkene represented by the general formula (XII) are such that, on a mass basis, C < A and C < B.

[10] The above filter body contains polyethylene or polytetrafluoroethylene, The filter according to any one of [4] to [7], which contains one or more compounds selected from the above Group A and an alkane represented by the general formula (X).

[11] The filter according to any one of [1] to

[10] , wherein the pore diameter of the above filter is 10 nm or less.

[12] The filter according to any one of [1] to

[11] , wherein the above filter body contains an ion exchange group.

[13] The filter according to any one of [1] to

[12] , wherein the above filter body contains two or more layers made of different materials.

[14] The filter according to any one of [1] to

[13] , wherein the filter body contains an asymmetric porous membrane.

[15] The filter according to any one of [1] to

[14] , wherein the filter body is made of a material other than a fluorine-based material.

[16] A method for producing a filter according to any one of [1] to

[15] , A method for producing a filter, comprising a step of subjecting an untreated filter containing one or more compounds selected from the group consisting of compounds represented by general formulas (I) to (VIII), an alkane represented by general formula (X), and alkenes represented by general formulas (XI) and (XII) to a pretreatment using an organic cleaning solution.

[17] The organic cleaning liquid is propylene glycol monomethyl ether acetate, isopropanol, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, ethyl lactate, methyl methoxypropionate, cyclopentanone, cyclohexanone, γ-butyrolactone, diisoamyl ether, butyl acetate, isoamyl acetate, 4-methyl-2-pentanol, dimethyl sulfoxide, N-methylpyrrolidone, diethylene glycol, ethylene glycol, dipropylene glycol , propylene glycol, ethylene carbonate, propylene carbonate, sulfolane, cycloheptanone, 2-heptanone, butyl butyrate, isobutyl isobutyrate, undecane, pentyl propionate, isopentyl propionate, ethylcyclohexane, mesitylene, decane, 3,7-dimethyl-3-octanol, 2-ethyl-1-hexanol, 1-octanol, 2-octanol, ethyl acetoacetate, dimethyl malonate, methyl pyruvate, and dimethyl oxalate.

[18] The method for producing a filter according to

[16] or

[17] , wherein the pretreatment comprises a step of immersing the untreated filter in the organic cleaning solution for three days or more.

[19] The method for producing a filter according to any one of

[16] to

[18] , comprising a step of subjecting the untreated filter immersed in the organic cleaning solution to ultrasonic treatment to perform the pretreatment.

[20] The pretreatment includes a step of passing the organic cleaning liquid through the untreated filter having a hollow cylindrical shape, The method for producing a filter according to any one of

[16] to

[19] , wherein the organic cleaning liquid passed through the untreated filter is 10 kg or more per inch of cylindrical length of the untreated filter. 〔twenty one〕 Relative to the total content of the compounds selected from the group consisting of the compounds represented by the general formulas (I) to (VIII), the alkanes represented by the general formula (X), and the alkenes represented by the general formulas (XI) and (XII) in the untreated filter, The method for producing a filter according to any one of

[16] to

[20] , wherein a mass ratio of a total content of the compounds selected from the group consisting of the compounds represented by the general formulas (I) to (VIII), the alkane represented by the general formula (X), and the alkenes represented by the general formulas (XI) and (XII), in the filter after the pretreatment, is 0.5000 or less. 〔twenty two〕 The method for producing a filter according to any one of

[16] to

[21] , wherein the untreated filter before the pretreatment is packed in a packing material, at least a part of a contact portion with the untreated filter being made of a fluororesin or stainless steel. 〔twenty three〕 An inlet portion and an outlet portion, The filter according to any one of [1] to

[15] above, Two or more of the filters are disposed in series between the inlet and the outlet; A filtration device for purifying a liquid to be purified to obtain a liquid drug, the filtration device including a flow passage extending from the inlet portion to the outlet portion. 〔twenty four〕 The filtration device according to

[23] , wherein, among the two or more filters, the filter having the largest pore size has a pore size of 10 to 200 nm, and the filter having the smallest pore size has a pore size of 1 to 10 nm. 〔twenty five〕 The filtration device according to

[23] or

[24] , comprising the filter according to

[12] .

[26] The filtration device according to any one of

[23] to

[25] , comprising the filter according to [9].

[27] The filtration device according to any one of

[23] to

[26] , comprising the filter according to

[10] .

[28] A method for producing a chemical solution by purifying a liquid to be purified to obtain a chemical solution, comprising the steps of: A method for producing a chemical solution, comprising a step of filtering a liquid to be purified using the filter according to any one of [1] to

[15] to obtain a chemical solution.

[29] The liquid to be purified is propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, propylene glycol monopropyl ether, cyclohexanone, methyl methoxypropionate, butyl acetate, γ-butyrolactone, 4-methyl-2-pentanol, propylene glycol monoethyl ether, ethyl lactate, cyclopentanone, diisoamyl ether, isoamyl acetate, isopropanol, dimethyl sulfoxide, N-methylpyrrolidone, diethylene glycol, ethylene glycol, dipropylene glycol , propylene glycol, ethylene carbonate, propylene carbonate, sulfolane, cycloheptanone, 2-heptanone, butyl butyrate, isobutyl isobutyrate, undecane, pentyl propionate, isopentyl propionate, ethylcyclohexane, mesitylene, decane, 3,7-dimethyl-3-octanol, 2-ethyl-1-hexanol, 1-octanol, 2-octanol, ethyl acetoacetate, dimethyl malonate, methyl pyruvate, and dimethyl oxalate. Effect of the Invention

[0008] According to the present invention, it is possible to provide a filter that allows production of a chemical solution having excellent defect suppression properties, and also to provide a filter production method, a filtering device, and a chemical solution production method. [Brief description of the drawings]

[0009] [Figure 1] 1 is a schematic diagram illustrating a filtering device according to a first embodiment of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0010] The present invention will be described in detail below. The following description of the components may be based on a representative embodiment of the present invention, but the present invention is not limited to such an embodiment. In this specification, a numerical range expressed using "to" means a range that includes the numerical values ​​before and after "to" as the lower and upper limits. In the present invention, "ppm" stands for "parts-per-million (10 -6 ) and "ppb" stands for "parts-per-billion (10 -9 )" and "ppt" stands for "parts-per-trillion (10 -12 )" and "ppq" is "parts-per-quadrillion(10 -15 )". In addition, in the description of groups (atomic groups) in the present invention, descriptions that do not indicate whether they are substituted or unsubstituted include groups that do not contain a substituent as well as groups that contain a substituent, within the scope of the present invention. For example, a "hydrocarbon group" includes not only a hydrocarbon group that does not contain a substituent (unsubstituted hydrocarbon group), but also a hydrocarbon group that contains a substituent (substituted hydrocarbon group). This point is the same for each compound. In the present invention, "radiation" refers to, for example, far ultraviolet light, extreme ultraviolet light (EUV), X-rays, electron beams, etc. In the present invention, light refers to actinic light rays or radiation. Unless otherwise specified, "exposure" in the present invention includes not only exposure to far ultraviolet light, X-rays, EUV, etc., but also drawing with particle beams such as electron beams or ion beams.

[0011] [filter] The filter of the present invention is a filter for filtering liquids. The filter includes a filter body and a first organic compound. The first organic compound is a general term for compounds selected from the group consisting of compounds represented by general formulas (I) to (V) described below, alkanes represented by general formula (X), and alkenes represented by general formulas (XI) and (XII). The total content of the first organic compounds is 0.10 to 10,000 ppt by mass relative to the mass of the filter.

[0012] Although the mechanism by which the problem of the present invention is solved by using a filter having such a configuration is not necessarily clear, the inventor speculates that the mechanism is as follows. Note that the mechanism below is merely speculation, and even if the effect of the present invention is obtained through a different mechanism, it is still within the scope of the present invention. In semiconductor manufacturing processes, even trace amounts of impurities contained in chemicals can easily cause various defects. The various defects are defects that occur when the chemical liquid is applied to the manufacturing process of a semiconductor device. More specific examples are metal residue defects, particulate organic residue defects, and stain-like defects when the chemical liquid is used as a pre-wet liquid or a rinse liquid, and it is required to be able to suppress all of these defects. Another specific example is the above-mentioned defects that occur when the chemical liquid is used as a pipe cleaning liquid and then the pre-wet liquid or rinse liquid is transferred through the cleaned pipe and then pre-wet or rinse is performed, and it is required to be able to suppress all of these defects. Other specific examples are development failure defects, residue defects, and uniformity defects (one example of defects when a pattern is formed by ArF exposure) when the chemical liquid is used as a developer and / or rinse liquid for a pattern, as well as PLOT defects, which are protruding defects, BRIDGE defects, which are bridge-like defects between patterns, and GEL defects, which are defects based on film-like residues (one example of defects when a pattern is formed by EUV exposure), and it is required to be able to suppress all of these defects. Since the filter of the present invention contains the first organic compound in a predetermined amount or less, the chemical solution produced using the filter of the present invention is less likely to be contaminated with the first organic compound as an impurity, and the defect suppression properties of the chemical solution are improved. Furthermore, since the filter of the present invention contains a predetermined amount or more of the first organic compound, it is possible to prevent other trace components (especially impurities that are likely to cause defects) from adhering to the filter, and to prevent the other trace components from being mixed into the chemical solution produced using the filter of the present invention and causing defects in the pattern. The present inventors speculate that, based on this mechanism, the occurrence of defects in the final pattern can be suppressed in a resist process using a chemical solution produced using the filter of the present invention.

[0013] [Specified organic compounds] The filter of the present invention contains a first organic compound selected from the group consisting of compounds represented by the general formulas (I) to (V) described below, alkanes represented by the general formula (X), and alkenes represented by the general formulas (XI) and (XII). The first organic compound and the compounds represented by general formulas (VI) to (VIII) described later are also collectively referred to as specific organic compounds. The specific organic compound is usually liquid or solid at normal temperature and pressure.

[0014] <First organic compound> The first organic compound is at least one selected from the group consisting of compounds represented by general formulas (I) to (V), alkanes represented by general formula (X), and alkenes represented by general formulas (XI) and (XII). Each of the first organic compounds will be described below.

[0015] ·General formula (I) The compounds represented by general formula (I) are shown below.

[0016] [ka]

[0017] In general formula (I), R 1a and R 1c each independently represents an alkyl group which may contain a substituent. The alkyl group may be linear or branched, or may contain a cyclic structure. The number of carbon atoms in the alkyl group is preferably from 1 to 50, and more preferably from 10 to 20. The number of carbon atoms in the alkyl group does not include the number of carbon atoms contained in a substituent that the alkyl group may contain. R 1b represents an alkylene group which may contain a substituent. Note that the number of carbon atoms in the alkylene group does not include the number of carbon atoms contained in the substituent that the alkylene group may contain. The alkylene group may be linear or branched, and may contain a cyclic structure. The alkylene group preferably has 1 to 10 carbon atoms, and more preferably has 1 to 5 carbon atoms.

[0018] When the filter contains the compound represented by general formula (I), the content thereof is preferably 0.10 to 3000 mass ppt, more preferably 1.0 to 1000 mass ppt, further preferably 1.0 to 200 mass ppt, and particularly preferably 1.0 to 80 mass ppt, relative to the mass of the filter. Examples of compounds represented by general formula (I) are given below.

[0019] [ka]

[0020] ·General formula (II) The compound represented by the general formula (II) is shown below. The compound represented by the general formula (II) is a specific organic compound different from the compound represented by the general formula (I).

[0021] [ka]

[0022] In the general formula (II), a benzene ring group which may contain a substituent, a cyclohexene ring group which may contain a substituent, or a cyclohexane ring group which contains a cycloalkyloxy group as a substituent is represented. The cyclohexane ring group may further contain another substituent. Examples of the substituent that the benzene ring group may have include an alkyl group, an alkoxy group, and an arylcarbonyl group, each of which may have a substituent. Examples of the substituent that the cyclohexene ring group may contain include an alkenyloxy group and a cyclohexene ring group, each of which may contain a substituent.

[0023] When the filter contains the compound represented by general formula (II), the content thereof is preferably 0.10 to 6000 mass ppt, more preferably 1.0 to 2000 mass ppt, further preferably 1.0 to 400 mass ppt, and particularly preferably 1.0 to 160 mass ppt, relative to the mass of the filter. Examples of the compound represented by the general formula (II) are given below.

[0024] [ka]

[0025] [ka]

[0026] ·General formula (III) The compound represented by the general formula (III) is shown below. The compound represented by the general formula (III) is a specific organic compound different from the specific organic compounds described above.

[0027] [ka]

[0028] ·General formula (III) In general formula (III), R 3a ~R 3h each independently represents an alkyl group which may contain a substituent. R 3b and R 3e may be bonded to each other to form a ring, R 3b and R 3e The group formed by bonding with each other is -O-(-Si(R 3i )2-O-) a -It is. a represents an integer of 1 or more. There is no particular upper limit to a, but it is often 10 or less. R 3i represents an alkyl group which may contain a substituent. Multiple R's 3i may be the same or different. R 3a ~R 3i The alkyl group represented by the formula (I) may be linear or branched, or may contain a cyclic structure. The number of carbon atoms in the alkyl group is preferably 1 to 10, and more preferably 1 to 5. The number of carbon atoms in the alkyl group does not include the number of carbon atoms contained in a substituent that the alkyl group may contain. R 3a ~R 3i Each of the alkyl groups represented by the following formula (I) is preferably an unsubstituted alkyl group, and more preferably a methyl group. R 3g and R 3h It is also preferable that one of the groups is an alkyl group containing a substituent. The substituent is preferably a group containing one or more oxyalkylene groups (the alkylene group portion preferably has 2 to 4 carbon atoms, may be linear or branched, or may contain a cyclic structure).

[0029] When the filter contains the compound represented by general formula (III), the content thereof is preferably 0.10 to 5000 mass ppt, more preferably 1.0 to 1500 mass ppt, further preferably 1.0 to 400 mass ppt, and particularly preferably 1.0 to 110 mass ppt, relative to the mass of the filter. Examples of the compound represented by the general formula (III) are shown below.

[0030] [ka]

[0031] [ka]

[0032] ·General formula (IV) The compound represented by general formula (IV) is shown below. The compound represented by the general formula (IV) is a specific organic compound different from the specific organic compounds described above.

[0033] [ka]

[0034] In general formula (IV), R 4a is -N(R 4c )R 4d or -SR 4e Represents. R 4c , R 4d , and R 4e each independently represents a hydrogen atom or a substituent. R 4b represents -NH- or -S-. R 4e Examples of the aryl group include aromatic thio groups. The aromatic ring group in the aromatic thio group may or may not contain a heteroatom (such as a sulfur atom, a nitrogen atom, and / or an oxygen atom), but preferably contains one. The aromatic ring group may be a monocyclic or polycyclic ring, but preferably a polycyclic ring. The aromatic ring group is preferably a benzothiazole ring group.

[0035] When the filter contains the compound represented by general formula (IV), the content thereof is preferably 0.10 to 2000 ppt by mass, more preferably 1.0 to 1000 ppt by mass, and further preferably 1.0 to 600 ppt by mass, relative to the mass of the filter. Examples of the compound represented by the general formula (IV) are shown below.

[0036] [ka]

[0037] ·General formula (V) The compound represented by general formula (V) is shown below. The compound represented by the general formula (V) is a specific organic compound different from the specific organic compounds described above.

[0038] [ka]

[0039] In formula (V), Y represents a benzene ring group which may be substituted with an alkyl group, or a group represented by formula (A), in which * represents a bonding position.

[0040] [ka]

[0041] When Y represents a benzene ring group, s represents 1, L represents a single bond, and R 5a represents an alkyl group which may contain a substituent. The alkyl group may contain a heteroatom (preferably an oxygen atom). R 5a The alkyl group may be linear or branched, or may contain a cyclic structure. R 5a The number of carbon atoms in the alkyl group is preferably 1 to 20, and more preferably 1 to 10. 5a The number of carbon atoms in the alkyl group of R 5adoes not include the number of carbon atoms contained in any substituents that the alkyl group may contain. R 5a The substituent that the alkyl group may have preferably contains an aromatic ring group (preferably a benzene ring group, which may further contain a substituent).The substituent is more preferably an aromatic ester group. When the benzene ring group represented by Y is substituted with an alkyl group, the above alkyl group and R 5a may be bonded to each other to form a ring. When a plurality of alkyl groups are substituted on a benzene ring group represented by Y, the alkyl groups may be bonded to each other to form a ring.

[0042] When Y represents a group represented by formula (A), s represents 3, L represents a methylene group, and R 5a each independently represents an alkyl group. In this case, R 5a The alkyl group preferably has 1 to 15 carbon atoms, and more preferably has 1 to 10 carbon atoms.

[0043] When the filter contains the compound represented by general formula (V), the content thereof is preferably 0.10 to 2000 mass ppt, more preferably 1.0 to 1500 mass ppt, further preferably 5.0 to 250 mass ppt, and particularly preferably 5.0 to 60 mass ppt, relative to the mass of the filter. Examples of compounds represented by general formula (V) are given below.

[0044] [ka]

[0045] ·General formula (X) Alkanes represented by general formula (X) are shown below. The alkane represented by the general formula (X) is a specific organic compound different from the specific organic compounds described above.

[0046] [ka]

[0047] In the general formula (X), j represents an integer of 12 to 50. Two j's have the same value. The alkane may be linear or branched, but does not contain a cyclic structure, i.e., is not a cycloalkane.

[0048] When the filter contains the alkane represented by general formula (X), the content thereof is preferably 0.10 to 3000 mass ppt, more preferably 1.0 to 600 mass ppt, still more preferably 1.0 to 315 mass ppt, and particularly preferably 1.0 to 90 mass ppt, relative to the mass of the filter.

[0049] ·General formula (XI) Alkenes represented by general formula (XI) are shown below. The alkene represented by the general formula (XI) is a specific organic compound different from the specific organic compounds described above.

[0050] [ka]

[0051] In general formula (XI), k represents an integer of 12 to 50. Two k's have the same value. The alkene represented by general formula (XI) is an alkene containing one C=C double bond in the molecule. The alkene may be linear or branched, but does not contain a cyclic structure.

[0052] When the filter contains the alkene represented by general formula (XI), the content thereof is preferably 0.10 to 9000 mass ppt, more preferably 0.10 to 3000 mass ppt, further preferably 1.0 to 600 mass ppt, and particularly preferably 1.0 to 250 mass ppt, relative to the mass of the filter.

[0053] ·General formula (XII) Alkenes represented by general formula (XII) are shown below. The alkene represented by the general formula (XII) is a specific organic compound different from the specific organic compounds described above.

[0054] [ka]

[0055] n represents an integer of 30 to 50. m represents an integer of 20 to 90 and not more than 2n-2. The alkene represented by the general formula (XII) is an alkene containing two or more C=C double bonds in the molecule. When the alkene represented by general formula (XII) contains x C=C double bonds, m takes the value of "2n+2-2x". The alkene may be linear or branched, but does not contain a cyclic structure.

[0056] When the filter contains the alkene represented by general formula (XII), the content thereof is preferably 0.10 to 4000 mass ppt, more preferably 1.0 to 1000 mass ppt, further preferably 1.0 to 350 mass ppt, and particularly preferably 1.0 to 70 mass ppt, relative to the mass of the filter. Examples of the alkene represented by the general formula (XII) include squalene (C 30 H 50 ), Lycopene (C 40 H 56 ), Neurosporen (C 40 H 58 ), phytoene (C 40 H 64 ), or phytofluene (C 40 H 62 ) are mentioned.

[0057] The total content of the first organic compounds is 0.10 to 10000 mass ppt, preferably 1.0 to 8000 mass ppt, more preferably 5.0 to 2500 mass ppt, and particularly preferably 5.0 to 850 mass ppt, relative to the mass of the filter. If the total content of the first organic compounds is 1.0 ppt by mass or more (preferably 5.0 ppt by mass or more) relative to the mass of the filter, the filter is unlikely to excessively adsorb the second organic compounds described below from the environment (air, etc.), and the produced chemical solution is considered to have better defect suppression. If the total content of the first organic compounds is 8000 ppt by mass or less (preferably 2500 ppt by mass or less, more preferably 850 ppt by mass or less) relative to the mass of the filter, the produced chemical solution is unlikely to be contaminated with the second organic compounds derived from the filter, and the produced chemical solution is considered to have better defect suppression. When the filter contains multiple types of first organic compounds each represented by a different general formula, it is preferable that at least one of the first organic compounds represented by each general formula satisfies the above-mentioned preferred content range, and it is more preferable that two or more of the first organic compounds each satisfy the above-mentioned preferred content range.

[0058] <Second organic compound> Furthermore, the filter preferably contains, as the specific organic compound, at least one type of second organic compound selected from the group consisting of the compounds represented by the general formulas (VI) to (VIII). Each of the second organic compounds will be described below.

[0059] ·General formula (VI) The compound represented by general formula (VI) is shown below. The compound represented by the general formula (VI) is a specific organic compound different from the specific organic compounds described above.

[0060] [ka]

[0061] In general formula (VI), R 6a represents an optionally substituted alkyl group or a hydrogen atom. R 6b and R 6c each independently represents a hydrogen atom, -AL-OR 6d , -CO-R 6eor -C(OH)-R 6f Represents. AL represents an alkylene group (preferably having 1 to 6 carbon atoms) which may contain a substituent. R 6d , R 6e , or R 6f each independently represents a substituent (preferably an alkyl group which may further contain a substituent). R 6a , R 6d , R 6e , and R 6f The alkyl groups which may contain a substituent represented by the following formula (I) may each independently be linear or branched, or may contain a cyclic structure. The number of carbon atoms in the alkyl group is preferably from 1 to 50, and more preferably from 1 to 20. The number of carbon atoms in the alkyl group does not include the number of carbon atoms contained in a substituent that the alkyl group may contain. Examples of the substituent that the alkyl group may have include a hydroxyl group, an alkyl ester group, and an alkyl vinyl group (preferably an alkyl group portion having 3 to 12 carbon atoms). R 6d If there are multiple, there are multiple R 6d They may be the same or different. 6e If there are multiple, there are multiple R 6e They may be the same or different. 6f If there are multiple, there are multiple R 6f They may be the same or different. R 6a The substituent that may be contained in the alkyl group represented by the formula: 6d , R 6e , and R 6f Two combinations selected from the group consisting of two R 6d Two R's 6e Two R's 6f may be bonded to each other to form a ring. R 6a The substituent that may be contained in the alkyl group represented by the formula: 6d , R 6e , and R6f Two combinations selected from the group consisting of two R 6d Two R's 6e Two R's 6f The groups formed by bonding with each other are -O- and -NR 6g -(R 6g is a substituent), and -NHCO-. R 6a , R 6b , or R 6c At least one of these is other than a hydrogen atom.

[0062] When the filter contains the compound represented by general formula (VI), the content thereof is preferably 0.10 to 20,000 mass ppt, more preferably 1.0 to 4,000 mass ppt, still more preferably 1.0 to 1,000 mass ppt, and particularly preferably 1.0 to 300 mass ppt, relative to the mass of the filter. Examples of the compound represented by the general formula (VI) are shown below. In the following examples, AL represents an alkylene group having 1 to 10 carbon atoms which may contain a substituent, and q represents an integer of 4 to 6.

[0063] [ka]

[0064] [ka]

[0065] [ka]

[0066] ·General formula (VII) The compound represented by general formula (VII) is shown below. The compound represented by the general formula (VII) is a specific organic compound different from the specific organic compounds described above.

[0067] [ka]

[0068] In general formula (VII), R 7a and R 7b each independently represents an alkyl group which may contain a substituent. The alkyl group may be linear or branched, or may contain a cyclic structure. The number of carbon atoms in the alkyl group is preferably 1 to 20, and more preferably 2 to 10. The number of carbon atoms in the alkyl group does not include the number of carbon atoms contained in a substituent that the alkyl group may contain. The above-mentioned substituent is preferably, for example, an aromatic ring group (which may further contain a substituent, and is preferably a phenyl group).

[0069] When the filter contains the compound represented by general formula (VII), the content thereof is preferably 0.10 to 30,000 mass ppt, more preferably 1.0 to 5,000 mass ppt, still more preferably 1.0 to 395 mass ppt, and particularly preferably 1.0 to 90 mass ppt, relative to the mass of the filter. Examples of the compound represented by formula (VII) are shown below.

[0070] [ka]

[0071] ·General formula (VIII) The compound represented by the general formula (VIII) is shown below. The compound represented by the general formula (VIII) is a specific organic compound different from the specific organic compounds described above.

[0072] [ka] In general formula (VIII), R 8a ~R 8ceach independently represents a hydrogen atom, an alkyl group which may have a substituent, or a benzene ring group which may have a substituent. R 8a ~R 8c Among these, it is preferable that one or more (preferably two or more) are an alkyl group which may contain a substituent, or a benzene ring group which may contain a substituent. The alkyl group may be linear or branched, or may contain a cyclic structure. The number of carbon atoms in the alkyl group is preferably 1 to 20, and more preferably 1 to 5. The number of carbon atoms in the alkyl group does not include the number of carbon atoms contained in a substituent that the alkyl group may contain. The substituent is preferably an alkoxy group (preferably having 2 to 6 carbon atoms) or a halogen atom (such as a fluorine atom, a chlorine atom, a bromine atom, or an iodine atom). The substituent that the benzene ring group may have is preferably an alkyl group (preferably having a carbon number of 2 to 10).

[0073] When the filter contains the compound represented by general formula (VIII), the content thereof is preferably 0.10 to 20,000 mass ppt, more preferably 1.0 to 10,000 mass ppt, still more preferably 1.0 to 8,000 mass ppt, particularly preferably 1.0 to 1,000 mass ppt, and most preferably 1.0 to 300 mass ppt, relative to the mass of the filter. Examples of the compound represented by the general formula (VIII) are shown below.

[0074] [ka]

[0075] The total content of the second organic compounds is preferably from 0.10 to 200,000 ppt by mass, more preferably from 1.0 to 9,000 ppt by mass, particularly preferably from 1.0 to 3,000 ppt by mass, and most preferably from 1.0 to 750 ppt by mass, relative to the mass of the filter. When the filter contains a plurality of types of second organic compounds represented by different general formulas, it is preferable that at least one of the first organic compounds represented by each general formula satisfies the above-described preferable content range, and more preferably two or more satisfy the above-described preferable content range.

[0076] <Group A, Group B> The specific organic compound can also be classified into a specific organic compound of Group A and a specific organic compound of Group B separately from the classification of the first organic compound and the second organic compound. The specific organic compound of Group A is a compound selected from the group consisting of compounds represented by general formulas (I) to (VIII), and the specific organic compound of Group B is an alkane represented by general formula (X), and general formulas (XI) and (XII). It is a compound selected from the group consisting of alkenes represented by The filter preferably contains both one or more specific organic compounds of Group A and one or more specific organic compounds of Group B.

[0077] When the filter contains a specific organic compound of Group A, its total content is preferably 0.10 to 100,000 mass ppt, more preferably 0.10 to 10,000 mass ppt, still more preferably 0.1 to 3200 mass ppt, particularly preferably 1.0 to 1000 mass ppt, and most preferably 1.0 to 1200 mass ppt with respect to the mass of the filter. When the filter contains a specific organic compound of Group B, its total content is preferably 0.10 to 50,000 mass ppt, more preferably 0.10 to 10,000 mass ppt, still more preferably 1.0 to 1200 mass ppt, particularly preferably 1.0 to 1000 mass ppt, and particularly preferably 1.0 to 500 mass ppt with respect to the mass of the filter.

[0078] The total content of the specific organic compounds of group A and the specific organic compounds of group B in the filter (i.e., the total content of the compounds selected from the group consisting of the compounds represented by the general formulas (I) to (VIII), the alkanes represented by the general formula (X), and the alkenes represented by the general formulas (XI) and (XII)) is preferably 0.1 mass ppt or more, more preferably 1 mass ppt or more, and even more preferably 5 mass ppt or more, relative to the mass of the filter. The upper limit is preferably 1,000,000 mass ppt or less, more preferably 170,000 mass ppt or less, even more preferably 10,000 mass ppt or less, particularly preferably 6,500 mass ppt or less, and most preferably 1,600 mass ppt or less.

[0079] In this specification, the content of the specific organic compound in the filter is measured by the following method. First, the dried filter is immersed in PGMEA (propylene glycol monomethyl ether acetate) heated under reflux conditions for one hour, and specific organic compounds in the filter are dissolved into the PGMEA (dissolution treatment). In this case, the PGMEA to be immersed should be of high purity grade (and the amount of impurities contained in the filter is set as zero, based on the standard amount.) The amount (mass) of PGMEA to be immersed in the filter should be 10 to 30 times the mass of the filter to be measured. The amount and type of specific organic compounds contained in each PGMEA before and after the elution treatment are measured by GC / MS (gas chromatography mass spectrometry), and the amount of each specific organic compound in PGMEA increased by the elution treatment is defined as the amount of each specific organic compound contained in the filter being measured. More specifically, the content of each specific organic compound in the filter as defined in this application is "(the content of each specific organic compound in PGMEA after the treatment) - (the content of each specific organic compound in PGMEA before the treatment)".

[0080] [Metal Components] The filter may contain a metal component. In the present invention, the metal component includes metal particles and metal ions, and for example, the content of the metal component refers to the total content of the metal particles and metal ions. The filter may contain either metal particles or metal ions, or may contain both, and preferably contains both metal particles and metal ions.

[0081] Examples of the metal element in the metal component include Al (aluminum), B (boron), Ba (barium), Ca (calcium), Cd (cadmium), Co (cobalt), Cr (chromium), Cu (copper), Fe (iron), K (potassium), Li (lithium), Mg (magnesium), Mn (manganese), Mo (molybdenum), Na (sodium), Ni (nickel), P (phosphorus), Pb (lead), Sb (antimony), Si (silicon), Ti (titanium), V (vanadium), and Zn (zinc). Among them, the metal element in the metal component is preferably one or more selected from the group consisting of Al, Ca, Cr, Cu, Fe, K, Mg, Na, Ni, Zn, and Pb. Hereinafter, these metal elements are also particularly referred to as specific metal elements. In addition, metal components, metal particles, and metal ions containing specific metal elements are also referred to as specific metal components, specific metal particles, and specific metal ions, respectively.

[0082] The metal particles may be a simple substance or an alloy, or may be other metal compounds, and the metal (including metal compounds) may exist in a form associated with an organic substance. The metal components may be metal components that are inevitably contained in the filter, may be metal components that are inevitably contained during the production, storage, and / or transportation of the treatment liquid, or may be metal components that are intentionally added.

[0083] In order to provide a chemical solution with better defect suppression properties, when the filter contains a specific metal component, the content thereof is preferably 0.10 to 30,000 mass ppt, more preferably 0.10 to 5,000 mass ppt, still more preferably 1.0 to 5,000 mass ppt, particularly preferably 1.0 to 1,500 mass ppt, and most preferably 1.0 to 300 mass ppt, relative to the total mass of the chemical solution. If the content of the specific metal component is 0.1 ppt by mass or more, the metal forms coarse aggregates that are thrown off by centrifugal force, and as a result, the defect suppression property can be further improved. Furthermore, if the content of the specific metal component is less than 30,000 ppt by mass, it is easy to avoid an increase in the occurrence of defects resulting from the metal component.

[0084] In order to obtain a chemical solution with better defect suppression properties, when the filter contains a specific metal ion, the content thereof is preferably 0.10 to 20,000 mass ppt, more preferably 0.10 to 2,500 mass ppt, still more preferably 1.0 to 2,500 mass ppt, and particularly preferably 1.0 to 800 mass ppt, relative to the mass of the filter. In order to provide a chemical solution with better defect suppression properties, when the filter contains specific metal particles, the content thereof is preferably 0.10 to 5000 mass ppt, more preferably 0.10 to 1000 mass ppt, still more preferably 1.0 to 1000 mass ppt, and particularly preferably 1.0 to 400 mass ppt, relative to the mass of the filter.

[0085] The type and content of metal ions and metal particles in the filter are transferred to PGMEA using a process similar to that used for the elution process in which specific organic compounds in the filter are eluted into PGMEA. The PGMEA was measured before and after the treatment using a SNP-ICP / MS (single nano-particle inductively coupled plasma mass spectrometry, e.g., Agilent 8900) device, and the amount of each metal component in the PGMEA increased by the treatment was defined as the amount of each metal component contained in the filter being measured.

[0086] [Filter body structure] The filter contains a filter body, which is typically porous, and the liquid to be purified that is treated by the filter of the present invention passes through the pores contained in the filter body.

[0087] <Filter pore diameter (pore diameter of the filter body)> The pore size of the filter is not particularly limited, and a filter having a pore size that is generally used for filtering the product to be purified, as described below, can be used. In particular, the pore size of the filter is preferably 200 nm or less, more preferably 20 nm or less, and even more preferably 10 nm or less, in order to easily control the number of particles (metal particles, etc.) contained in the chemical solution within a desired range. The lower limit is not particularly limited, but generally, 1 nm or more is preferred from the viewpoint of productivity. When multiple filters are used, it is preferable that at least one of the filters satisfies the above range. In this specification, the pore size and pore size distribution of the filter refer to the pore size and pore size distribution determined by the bubble point of isopropanol (IPA) or HFE-7200 ("Novec 7200", manufactured by 3M, hydrofluoroether, C4F9OC2H5). Usually, the pore size of the filter body and the pore size of the filter are the same.

[0088] <Filter body material> The material components of the filter body are not particularly limited. In the case of a resin, the material contained in the filter body may be polyamide such as nylon (for example, 6-nylon and 6,6-nylon); polyolefin such as polyethylene and polypropylene; polystyrene; polyimide (including polyamideimide); poly(meth)acrylate; polytetrafluoroethylene, perfluoroalkoxyalkane, perfluoroethylenepropene copolymer, ethylene-tetrafluoroethylene copolymer, ethylene-chlorotrifluoroethylene copolymer, polychlorotrifluoroethylene, polyvinylidene fluoride, polyvinyl fluoride, and other polyfluorocarbons; polyvinyl alcohol; polyester; cellulose; cellulose acetate, and the like. Among them, it is preferable to contain at least one selected from the group consisting of nylon (among which 6,6-nylon is preferred), polyolefin (among which polyethylene is preferred), poly(meth)acrylate, and polyfluorocarbon (among which polytetrafluoroethylene (PTFE) and perfluoroalkoxyalkane (PFA) are preferred) in terms of having better solvent resistance and the resulting chemical solution having better defect suppression properties. These polymers may be used alone or in combination of two or more. In addition to resin, materials such as diatomaceous earth and glass may also be used.

[0089] The polyimide (including polyamideimide) that may be contained in the filter body preferably has an imidization ratio of 1.0, more preferably 1.4 or more. There is no particular upper limit, but it is generally preferably 2.0 or less. The "imidization ratio" is calculated by dividing the area of ​​the peak representing an imide bond measured by a Fourier transform infrared spectrometer (FT-IR) by the area of ​​the peak representing benzene measured by the same FT-IR.

[0090] The polyimide preferably has continuous pores having a B value of 15 nm or less, as determined by the method described below. In this specification, the "B value" refers to a number (unit: nm) calculated by the following method. First, adsorbed molecules are adsorbed and desorbed to polyimide to obtain an adsorption isotherm. Then, from the obtained adsorption isotherm, [P / {V a The equilibrium relative pressure (P / P) is calculated and plotted against the equilibrium relative pressure (P / P). This plot is then considered as a straight line, and the slope s (=[(C-1) / (V m C)]) and intercept i(=[1 / (V m Then, from the obtained slope s and intercept i, V is calculated based on equations (2-1) and (2-2). m and C are calculated. Furthermore, V m The specific surface area A is calculated based on formula (3). Next, the adsorption data of the obtained adsorption isotherm is linearly interpolated to obtain the adsorption amount at the relative pressure set as the pore volume calculation relative pressure, and the total pore volume V is calculated from this adsorption amount. This is based on the theory of a series of calculation methods for specific surface area generally known as the "BET (Brunauer, Emmett, Teller) method." When carrying out the above method, matters not described in this specification shall conform to JIS R 1626-1996 "Method for measuring specific surface area of ​​fine ceramic powder by gas adsorption BET method."

[0091] [P / {V a (P0-P)}] =[1 / (V m ·C)]+[(C-1) / (V m ·C)](P / P0) (1) V m =1 / (s+i) (2-1) C = (s / i) + 1 (2-2) A=(V m ·L·σ) / 22414 (3)

[0092] however, V a :Adsorption amount V m : Monolayer adsorption amount P: Pressure at equilibrium of adsorbed molecules P0: Saturation vapor pressure of the adsorbed molecule L: Avogadro's number σ: Adsorption cross section of the adsorbed molecule It is.

[0093] The B value (nm) is a value calculated from the formula [4V / A] based on the specific surface area A and the total pore volume V calculated based on the above-mentioned method. The B value (nm) has the meaning of a pore diameter estimated from the measurement results of the BET method.

[0094] It is also preferred that the filter body contains a copolymer containing repeat units based on tetrafluoroethylene and other repeat units. Copolymers containing repeating units based on tetrafluoroethylene and other repeating units include, but are not limited to, tetrafluoroethylene-perfluoro(alkyl vinyl ether) copolymers (Poly(PTFE-CO-PFVAE)), tetrafluoroethylene-hexafluoropropylene copolymers (FEP), and mixtures thereof. PFA Teflon (registered trademark) is an example of a tetrafluoroethylene-perfluoro(alkyl vinyl ether) copolymer in which the alkyl is mainly or completely propyl. FEP Teflon (registered trademark) is an example of a tetrafluoroethylene-hexafluoropropylene copolymer. Both are manufactured by DuPont. Neoflon (trademark) PFA (Daikin Industries) is a polymer similar to DuPont's PFA Teflon (registered trademark). U.S. Patent No. 5,463,006 describes a tetrafluoroethylene-perfluoro(alkyl vinyl ether) copolymer in which the alkyl is mainly methyl. Also preferred is Hyflon® Poly(PTFE-CO-PFVAE) 620, available from Ausimont USA, Inc., Thorofare, New Jersey.

[0095] A filter body containing a copolymer containing a repeating unit based on tetrafluoroethylene and another repeating unit has no particular limitation on the pore diameter, pore structure, etc., as long as it contains a copolymer containing a repeating unit based on tetrafluoroethylene and another repeating unit, and is preferably a membrane (hollow fiber membrane) formed using hollow fibers.

[0096] The outer or inner surface of the hollow fiber membrane can be skinned or non-skinned. The skin is a thin and dense surface layer integral with the membrane substrate. In the case of a skinned membrane, most of the flow resistance by the membrane is in the thin skin. The skin on the surface may contain pores that make the continuous porous structure of the substrate, or may be a non-porous complete film. Asymmetry relates to the uniformity of the pore diameter across the membrane thickness, and in the case of hollow fibers, this is in the porous wall of the fiber. An asymmetric membrane has a structure where the pore diameter is a function of the position in the cross-section. Another definition method of asymmetry is the ratio of the pore diameter on one surface to the pore diameter on the opposite surface. As a method for manufacturing a material component composed of a hollow fiber membrane using such a copolymer containing a repeating unit based on tetrafluoroethylene and another repeating unit, for example, reference can be made to the description in JP-A-2015-61727.

[0097] When the filter body contains nylon, the filter preferably contains one or more of the specific organic compounds in Group A described above and two or more of the specific compounds in Group B. In this case, the filter body preferably contains at least an alkane represented by the general formula (X) and an alkene represented by the general formula (XI). Further, in the filter, when the content of the alkane represented by the general formula (X) is A, the content of the alkene represented by the general formula (XI) is B, and the content of the alkene represented by the general formula (XII) is C, it is preferable to satisfy the relationship of C < A and C < B on a mass basis.

[0098] When the filter body contains polyethylene or PTFE, the filter preferably contains one or more of the specific organic compounds in Group A described above and an alkane represented by the general formula (X).

[0099] The filter body may be surface-treated. The method of surface treatment is not particularly limited, and any known method may be used. Examples of the surface treatment method include chemical modification, plasma treatment, hydrophobic treatment, coating, gas treatment, and sintering.

[0100] The plasma treatment is preferable because it makes the surface of the filter body hydrophilic. The water contact angle of the surface of the filter body that has been hydrophilized by the 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, and even more preferably 30° or less.

[0101] As the chemical modification treatment, a method of introducing an ion exchange group into the base material is preferable. That is, the filter body may have ion exchange groups introduced into the substrate, which is made of any of the materials listed above. Typically, the filter body is preferably a layer containing a substrate containing ion exchange groups on the surface of the substrate (such a form is also simply referred to as "the filter body contains ion exchange groups." The same applies hereinafter in the same expressions). There are no particular limitations on the surface-modified substrate, and it is preferable to introduce ion exchange groups into the polymer, which is easier to manufacture.

[0102] Examples of the ion exchange group include a sulfonic acid group, a carboxyl 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 includes a method in which a compound containing an ion exchange group and a polymerizable group is reacted with the polymer to typically perform grafting.

[0103] The method for introducing ion exchange groups is not particularly limited, but may be to irradiate the fibers of the above resin with ionizing radiation (alpha rays, beta rays, gamma rays, X-rays, electron beams, etc.) to generate active moieties (radicals) in the resin. The irradiated resin is immersed in a monomer-containing solution to graft polymerize the monomer onto the substrate. As a result, a polymer is generated in which the monomer is bonded to the polyolefin fiber as a graft-polymerized side chain. The resin containing the generated polymer as a side chain is contacted and reacted with a compound containing an anion exchange group or a cation exchange group, and the ion exchange group is introduced into the graft-polymerized side chain polymer to obtain the final product.

[0104] The filter body may also be constructed by combining a woven or nonwoven fabric on which ion exchange groups are formed by radiation graft polymerization with a conventional filtering material such as glass wool, woven or nonwoven fabric.

[0105] By using a filter body containing ion exchange groups, the content of particles containing metal atoms in the chemical solution can be easily controlled to a desired range. The material of the filter containing ion exchange groups is not particularly limited, but examples thereof include polyfluorocarbons and materials in which ion exchange groups are introduced into polyolefins, and materials in which ion exchange groups are introduced into polyfluorocarbons are more preferable. The pore size of the filter containing the filter body containing ion exchange groups is not particularly limited, but is preferably 1 to 30 nm, more preferably 5 to 20 nm. When multiple filters are used, the filter using the filter body containing ion exchange groups may also serve as the filter containing the smallest pore size, or may be used separately from the filter containing the smallest pore size. Among them, when multiple filters are used in the filtration step described below, a form using a filter using a filter body containing ion exchange groups and a filter using a filter body not containing ion exchange groups and containing the smallest pore size is preferred, since the resulting chemical solution has better defect suppression properties.

[0106] The material used for the filter body of the filter containing the smallest pore size is not particularly limited, but from the viewpoint of solvent resistance and the like, generally, at least one selected from the group consisting of polyfluorocarbons and polyolefins is preferred, and polyolefins are more preferred.

[0107] Therefore, when multiple filters are used, the filter bodies of the filters may be made of different materials. For example, two or more types of filters may be used, each of which has a filter body made of a material selected from the group consisting of polyolefin, polyfluorocarbon, polyamide, and materials having ion exchange groups introduced therein.

[0108] The filter (filter body) may contain a coating layer. An example of a filter body containing a coating layer is a filter body A containing a porous substrate made of polyfluorocarbon and a coating layer containing a resin containing a hydrophilic group arranged so as to cover the porous substrate. It is preferable that the entire surface of the porous substrate is covered with the coating layer, but there may be a region that is not covered with the coating layer. The surface also includes the surfaces of the holes in the porous substrate. Examples of polyfluorocarbons include polytetrafluoroethylene, perfluoroalkoxyalkane, perfluoroethylenepropene copolymer, ethylene-tetrafluoroethylene copolymer, ethylene-chlorotrifluoroethylene copolymer, polychlorotrifluoroethylene, polyvinylidene fluoride, and polyvinyl fluoride, and polytetrafluoroethylene (PTFE) is preferred. As the polyfluorocarbon, polyfluorocarbons commercially available as PTFE porous substrates can be appropriately used. The method for producing the filter body A is not particularly limited, but typically, a method is preferred in which a coating layer is formed on the surface of a porous substrate (including the surface inside the pores) by contacting (e.g., applying and / or spraying) a coating layer-forming composition containing a resin containing hydrophilic groups with a porous substrate made of polyfluorocarbon (e.g., PTFE).

[0109] The coating layer contains a resin containing a hydrophilic group. There are no particular limitations on the resin, and any known resin can be used. Among them, polynorbornene or a copolymer thereof is preferred from the viewpoint of solvent resistance and the like. The hydrophilic group is not particularly limited, but examples thereof include a hydroxyl group, an ether group, an oxyalkylene group, a polyoxyalkylene group, a carboxylic acid group, an ester group, a carbonate ester group, a thiol group, a thioether group, a phosphoric acid group, a phosphoric acid ester group, an amide group, an imide group, and a group combining these (for example, a group containing a thioether group and a hydroxyl group), and the like. In terms of obtaining better effects of the present invention, a polyoxyalkylene group is preferred. As for the manufacturing method of the filter body A, for example, the descriptions in JP-A-2016-194038 and JP-A-2016-199733 can be referred to.

[0110] The filter body containing a coating layer may be, for example, a filter body B containing a porous substrate made of polyfluorocarbon and a coating layer containing a resin containing an adsorptive group arranged so as to cover the porous substrate. It is preferable that the entire surface of the porous substrate is covered with the coating layer, but there may be a region that is not covered with the coating layer. The surface also includes the surfaces of the pores of the porous substrate. Examples of the polyfluorocarbon include the same as those mentioned above. The method for producing the filter body B is not particularly limited, but typically, a method is preferred in which a coating layer-forming composition containing a resin containing an adsorptive group is used on a porous substrate made of polyfluorocarbon (e.g., PTFE), and the coating layer-forming composition is brought into contact with the porous substrate (e.g., by coating and / or spraying) to form a coating layer on the surface of the porous substrate (including the surface inside the pores).

[0111] The coating layer contains a resin containing an adsorptive group. The resin is not particularly limited, and known resins can be used. The adsorptive group is not particularly limited, and examples thereof include ether groups, hydroxyl groups, thioether groups, thiol groups, quaternary ammonium groups (quaternary ammonium bases), carboxylic acid groups, sulfonic acid groups, phosphoric acid groups, sulfonium groups, diester groups, and groups containing these groups. Among these, a group containing at least one selected from the group consisting of ether groups, hydroxyl groups, thioether groups, thiol groups, quaternary ammonium groups, carboxylic acid groups, and sulfonic acid groups is preferred in terms of the superior effect of the present invention. Among these, a group containing a thioether group and further containing at least one selected from the group consisting of an ether group, a hydroxyl group, a thiol group, a quaternary ammonium group, a carboxylic acid group, and a sulfonic acid group is preferred. The resin may contain one type of adsorptive group alone, or may contain two or more types.

[0112] The adsorptive group is not particularly limited, but may be *-SL(R 1 ) m (R 2 ) n-m-1 In the above formula, L is a linking group having a valence of n (n is an integer of 2 or more), and R 1 is at least one group selected from the group consisting of a hydroxyl group, a thiol group, a quaternary ammonium group, a carboxylic acid group, and a sulfonic acid group; R 2 represents a hydrogen atom or a monovalent organic group, * represents a bonding position, and m represents an integer of 0 or more and n-1 or less. For the manufacturing method of the filter body B, reference can be made to the descriptions in, for example, JP 2017-002273 A, JP 2016-29146 A, JP 2016-196625 A, and JP 2016-194040 A.

[0113] The filter body containing a coating layer may be, for example, a filter body C that contains a porous substrate made of polytetrafluoroethylene and a coating layer containing a fluorinated ionomer arranged so as to cover the porous substrate, the fluorinated ionomer containing at least one type selected from the group consisting of at least two types of monomer units described below and iodine atoms and bromine atoms. The two types of monomer units are an ethylene group and a functional group that can be converted into a hydrophilic group selected from the group consisting of -SO2F, -COOR, -COF, and combinations thereof, and R is any one of C1 to C 20 Alkyl radical or C6-C 20 a fluorinated monomer unit containing a functional group which is an aryl radical; and a monomer unit derived from at least one bis-olefin selected from the group consisting of formula (OF-1), formula (OF-2), and formula (OF-3) below.

[0114] [ka]

[0115] In formula (OF-1), j is an integer of 2 to 10, and R1, R2, R3 and R4 may be the same or different and are H, F, or a C1 to C5 alkyl group, a perfluoroalkyl group or a fluoroalkyl group.

[0116] [ka] In formula (OF-2), the multiple A's may be the same or different from one another and are each independently selected from the group consisting of F, Cl, and H; the multiple B's may be the same or different from one another and are each independently selected from the group consisting of F, Cl, H, and ORB, where R is a branched or linear alkyl radical which may be at least partially fluorinated or chlorinated, and E is a divalent group containing 2 to 10 carbon atoms which may be inserted by an ether bond and which is optionally fluorinated.

[0117] [ka]

[0118] In formula (OF-3), E, ​​A, and B are the same as the definitions of the respective symbols in formula (OF-2), and R5, R6, and R7 may be the same or different and are H, F, or a C1 to C5 alkyl group, a perfluoroalkyl group, or a fluoroalkyl group. As for a method for manufacturing the filter body C, for example, the description in JP 2012-522882 A can be referred to.

[0119] The filter body containing a coating layer may be a filter body D containing a porous substrate made of PTFE and a non-crosslinked coating layer containing a perfluorosulfonic (PFSA) acid polymer formed so as to cover the porous substrate. The porous substrate contained in the filter body D may have areas that are not covered by the non-crosslinked coating layer, but it is preferable that the entire surface (including the surfaces of the pores communicating with the outermost surface of the porous membrane) is covered with the non-crosslinked coating layer.

[0120] The polytetrafluoroethylene porous substrate is not particularly limited, and a commercially available porous substrate made of PTFE can be appropriately used.

[0121] The PFSA polymer dispersion for forming the coating layer is not particularly limited, but is available from Solvay Specialty Polymers (Borger, Texas) as AQUIVION® PFSA (e.g., AQUIVION PFSA D83-24B, AQUIVION PFSA D83-06A, and AQUIVION PFSA D79-20BS), which is based on a short-chain (SSC) copolymer of tetrafluoroethylene and sulfonyl fluoride vinyl ether (SFVE) F2C=CF-O-CF2-CF2-SO2F. The ionomer dispersion contains the sulfonic acid form. As the PFSA polymer dispersion, DuPont® Nafion® PFSA polymer dispersion is also preferred.

[0122] When forming a coating, the content of the PFSA in the coating solution can be appropriately adjusted. In general, the content is preferably in the range of 0.10 to 3 mass % relative to the total mass of the coating solution, and more preferably in the range of 0.12 to 2.2 mass %.

[0123] The method for forming a coating on a substrate is not particularly limited, but examples thereof include a method of immersing the substrate in the coating liquid and a method of spraying the coating liquid onto the substrate.

[0124] It is also preferred that the filter body contains two or more layers, which may be the same or different. A specific example of a combination of two or more layers is a laminated structure containing a first layer made of a porous PTFE substrate containing a first hydrophilic group on its surface, and a second layer disposed on the first layer and made of a porous PTFE substrate containing a second hydrophilic group different from the first hydrophilic group on its surface.

[0125] The method for forming a PTFE porous substrate (membrane) containing hydrophilic groups on its surface is not particularly limited, and examples thereof include a method in which a first hydrophilic group and / or a second hydrophilic group is bonded to the surface of an unmodified PTFE porous membrane. The method for introducing hydrophilic groups into an unmodified PTFE porous substrate is not particularly limited, but a method in which unmodified PTFE is used as the substrate and hydrophilic groups are introduced into the substrate is preferred. Although there is no particular limitation on the method for introducing hydrophilic groups, a PTFE porous membrane is irradiated with ionizing radiation (alpha rays, beta rays, gamma rays, X-rays, electron beams, etc.) to generate active moieties (radicals) in the PTFE resin. The irradiated PTFE resin is immersed in a solution containing a compound containing a specific functional group to bond the compound to the substrate. In this case, when the resin is immersed in a monomer containing a functional group, the monomer containing a functional group is graft polymerized to the main chain of the resin. As a result, the monomer is bonded to the polyolefin fiber as a graft polymerized side chain.

[0126] In addition to the above, hydrophilic groups may also be introduced into the PTFE porous substrate by plasma treatment, flame treatment, or the like.

[0127] The first hydrophilic group and the second hydrophilic group are not particularly limited, and examples thereof include a hydroxyl group, a (poly)ether group, an oxyalkylene group, a polyoxyalkylene group, a carboxylic acid group, a boronic acid group, a phosphonic acid group, a sulfonic acid group, an amino group, a quaternary ammonium group, an imidazolium group, a pyridinyl group, an ester group, a carbonate ester group, a thiol group, a thioether group, a phosphoric acid group, a phosphoric acid ester group, an amide group, an imide group, a (per)fluoroalkyl group, and a group combining these. Among these, at least one selected from the group consisting of a polyether group, a hydroxyl group, a thioether group, a thiol group, a quaternary ammonium group, a carboxylic acid group, a sulfonic acid group, and a group combining these is preferable.

[0128] <Porous structure of the filter body> The pore structure of the filter body (in other words, the pore structure of the material components contained in the filter body) is not particularly limited and may be appropriately selected depending on the components in the product to be purified, which will be described later. In this specification, the pore structure of the filter body refers to the pore size distribution, the positional distribution of the pores in the filter body, the shape of the pores, etc., and can typically be controlled by the manufacturing method of the filter body (or the material components contained in the filter body). For example, porous membranes can be obtained by sintering powders of resins or the like, and fibrous membranes can be obtained by electrospinning, electroblowing, meltblowing, and other methods, each of which has a different pore structure.

[0129] By "porous membrane" is meant a membrane that retains components of a product, such as gels, particles, colloids, cells, and poly-oligomers, but allows components substantially smaller than the pores to pass through the pores. Retention of components of a product by a porous membrane can depend on operating conditions, such as face velocity, use of surfactants, pH, and combinations thereof, and can depend on the pore size, structure, and size and structure of the particles to be removed (such as hard particles or gels).

[0130] When the product to be purified contains negatively charged particles, polyamides act as non-sieving membranes to remove such particles. Exemplary non-sieving membranes include, but are not limited to, nylon membranes such as nylon-6 membranes and nylon-6,6 membranes. It is noted that "non-sieving" retention mechanisms, as used herein, refer to retention that occurs due to mechanisms such as obstruction, diffusion and adsorption that are not related to the pressure drop or pore size of the filter.

[0131] Non-sieving retention includes retention mechanisms such as obstruction, diffusion and adsorption that remove target particles in the product regardless of the pressure drop of the filter or the pore size of the filter. Particle adsorption to the surface of the material component can be mediated, for example, by intermolecular van der Waals and electrostatic forces. Obstruction effects occur when particles moving through a non-sieving membrane layer containing a tortuous path cannot be redirected quickly enough to avoid contact with the non-sieving membrane. Particle transport by diffusion results primarily from random or Brownian motion of small particles, which creates a certain probability of the particles colliding with the filter media. Non-sieving retention mechanisms can be active when there is no repulsive force between the particle and the filter.

[0132] The UPE (ultra-high molecular weight polyethylene) membrane that the filter body may contain is typically a sieving membrane, by which is meant a membrane that primarily captures particles via a sieving retention mechanism, or a membrane optimized for capturing particles via a sieving retention mechanism. Typical examples of sieving membranes include, but are not limited to, polytetrafluoroethylene (PTFE) membranes and UPE membranes. The "sieve retention mechanism" refers to the retention of particles that are larger than the pore size of the porous membrane. Sieve retention can be improved by forming a filter cake (an agglomeration of particles to be removed on the membrane surface). The filter cake effectively performs the function of a secondary filter.

[0133] The material of the fiber membrane is not particularly limited as long as it is a polymer capable of forming a fiber membrane. Examples of the polymer include polyamides. Examples of the polyamide include nylon 6 and nylon 6,6. The polymer forming the fiber membrane may be poly(ethersulfone). When the fiber membrane is on the primary side of the porous membrane, it is preferable that the surface energy of the fiber membrane is higher than that of the polymer that is the material of the porous membrane on the secondary side. An example of such a combination is when the fiber membrane is made of nylon and the porous membrane is made of polyethylene (UPE).

[0134] The method for producing the fiber membrane is not particularly limited, and any known method can be used, including, for example, electrospinning, electroblowing, and meltblowing.

[0135] The pore structure of the porous membrane (e.g., porous membranes containing UPE, PTFE, etc.) is not particularly limited, but examples of the pore shape include lace-like, string-like, and node-like. The distribution of the pore sizes 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 positions in the membrane may be symmetric. It is also preferable that the filter body contains a membrane having a larger size distribution and an asymmetric distribution position in the membrane (the above membrane is also called an "asymmetric porous membrane"). In the asymmetric porous membrane, the size of the pores changes in the membrane. In particular, the asymmetric porous membrane preferably has an asymmetric pore size distribution in the thickness direction (filtration direction). Typically, the pore size increases from one surface of the membrane to the other surface of the membrane. In this case, the surface on the side where there are many pores with a large pore size is called the "open side", and the surface on the side where there are many pores with a small pore size is also called the "tight side". Asymmetric porous membranes include, for example, membranes in which the pore size is smallest at a position within the thickness of the membrane (also called "hourglass shaped"). With an asymmetric porous membrane, the primary side has larger pore size, in other words the primary side is the open side, creating a pre-filtration effect.

[0136] The asymmetric porous membrane is preferably a membrane containing an asymmetric porous membrane made of UPE and graft chains bonded to the surface of the asymmetric porous membrane, and at least a part of the graft chains preferably contains a neutral group or an ion exchange group. For a membrane containing an asymmetric porous membrane made of UPE and graft chains bonded to the surface of the asymmetric porous membrane, for example, the description in JP-T-2017-536232 may be referred to.

[0137] The porous membrane may include a thermoplastic polymer such as PESU (polyethersulfone), PFA (perfluoroalkoxyalkane, a copolymer of tetrafluoroethylene and perfluoroalkoxyalkane), polyamide, and polyolefin, or may include polytetrafluoroethylene, etc. Among them, ultra-high molecular weight polyethylene is preferable as a material for the porous membrane. Ultra-high molecular weight polyethylene means a thermoplastic polyethylene containing an extremely long chain, and preferably has a molecular weight of at least one million, typically 2 to 6 million.

[0138] <Support layer> A material having the above-mentioned composition and structure, etc., preferably constitutes a member (also referred to as a "filtration layer") used to exert the filtering ability of the filter body, and the above-mentioned filter body preferably contains a support layer in addition to such a filtration layer. For example, when it is difficult to process a filter body consisting of only a filtration layer into a desired shape, the support layer is laminated with the filtration layer to impart appropriate rigidity to the filter and improve processability. The filter body may contain only one filtration layer or may contain two or more filtration layers. Similarly, the filter body may contain only one support layer or may contain two or more support layers. The support layer may be provided on only one side (the primary or secondary side of filtration) or on both sides of the filtration layer. When the filter body contains two or more filtration layers, the filtration layers and the support layers may be provided alternately. The material of the support layer may be, for example, polyolefin (polyethylene (including UPE), polypropylene, etc.), PTFE, PFA, or polyester.

[0139] The filter body also preferably contains two or more layers, each layer being made of a different material. An example of a filter body containing two or more layers made of different materials is a filter in which the filter body has a filtration layer and a support layer, and the filtration layer and the support layer are made of different materials. In addition, a filter body containing two or more layers each made of a different material may be a filter in which the filter body has a filtration layer and a support layer, both of which are made of the same material, and the surface of the filtration layer is grafted to form a graft layer that is a material different from both the filtration layer and the support layer. Alternatively, the filter body containing two or more layers each made of a different material may be a filter having a layer that serves both the functions of a filtration layer and a support layer, the surface of which is grafted to form a graft layer made of a material different from the layer that serves both the functions of the filtration layer and the support layer.

[0140] The filter body is also preferably made of a material other than a fluorine-based material. An example of the filter body being made of a material other than a fluorine-based material is one in which the filtration layer and support layer of the filter body are both made of a material other than a fluorine-based material (fluororesins such as PTFE, PFA, and PESU). In other words, in a filter body made of a material other than a fluorine-based material, for example, the filtration layer and the support layer are both preferably made of a material other than a fluorine-based material (polyolefin (polyethylene (including UPE), polypropylene, etc.), polyester, and / or polyamide (nylon 6, nylon 6,6, etc.)). The filtration layer of the filter body made of a material other than a fluorine-based material may be grafted (preferably using a non-fluorine-based repeating unit). A filter body made of a material other than a fluorine-based material tends to reduce the elution of components from the filter, and the resulting chemical solution has better defect suppression properties (especially pattern defect suppression properties when a pattern is formed by EUV exposure).

[0141] [Filter manufacturing method] The method for producing the filter of the present invention preferably includes, for example, a step of pretreating an untreated filter containing one or more specific organic compounds with an organic cleaning liquid. An untreated filter is, for example, a filter available on the market, and usually contains the first organic compound on the surface and / or inside of the untreated filter in a content exceeding the content permitted by the present invention. Hereinafter, a filter that is subjected to preprocessing (an unprocessed filter) is also referred to as a processed filter.

[0142] The treated filter may be obtained from the market as described above. When such a treated filter is put into circulation, it is often packaged in a packaging material, such as being placed in a packaging bag and sealed in order to prevent contamination. In this case, if the part of the packaging material that may come into contact with the treated filter in the packaged state (contact part) is polyolefin (polyethylene including high density polyethylene, etc.), the specific organic compounds and / or other impurity components described above are more likely to adhere to the treated filter, causing contamination, compared to when the contact part is a fluorine-based resin or stainless steel. Therefore, it is preferable that the filter to be treated before being subjected to pretreatment is packed in a packaging material in which at least a part of the contact area with the filter to be treated is made of a fluororesin or stainless steel, in order to reduce the cost required for pretreatment and / or to better suppress defects in the chemical solution produced using the final filter obtained. If at least a part of the contact area is made of fluororesin or stainless steel, contamination of the treated filter can be reduced, and the effects of the present invention achieved by the filter of the present invention obtained by pre-treating the treated filter that has been packaged in such packaging material will be even better. In other words, the filter of the present invention is preferably a filter obtained by performing pretreatment on a filter to be treated that is packed in a packaging material in which at least a portion of the contact portion with the filter to be treated is made of a fluorine-based material or stainless steel.

[0143] The fluororesin in the contact portion may be, for example, fluororesins such as PTFE and PFA. The stainless steel in the contact portion may be the stainless steel described below as a corrosion-resistant material, and among these, it is preferable that the contact portion be made of electrolytically polished stainless steel (EP-SUS). The area of ​​the contact portion which is the fluororesin and / or stainless steel is preferably 50 to 100%, more preferably 90 to 100%, and even more preferably 99 to 100%, of the total area of ​​the contact portion. The form of the packaging material is not particularly limited, and it may be in the form of a bag or a capsule. The packaging material only needs to have at least a part of the contact portion made of fluororesin and / or stainless steel, and may be entirely made of fluororesin and / or stainless steel, or may be a composite material with other materials. For example, it may be a composite material with a layer structure in which the contact portion is made of fluororesin and / or stainless steel and the other portion is made of fluororesin and / or stainless steel. In addition, even when the filter of the present invention (e.g., a treated filter after being subjected to pretreatment) is packed in a packaging material and stored or distributed, it is preferable that it is packed in a packaging material having a contact part configuration as described above. The filter to be treated packed in the packing material may be appropriately subjected to a cleaning process or the like before being packed.

[0144] The type of organic cleaning liquid used for the pretreatment is not particularly limited, and a known organic solvent can be used as the main component. In this specification, the main component means a component contained in the organic cleaning liquid at 99.9 mass% or more, more preferably 99.99 mass% or more, based on the total mass of the organic cleaning liquid. Examples of the organic solvent include alkylene glycol monoalkyl ether carboxylates, alkylene glycol monoalkyl ethers, alkyl lactates, alkyl alkoxypropionates, cyclic lactones (preferably having 4 to 10 carbon atoms), monoketone compounds which may contain a ring (preferably having 4 to 10 carbon atoms), alkylene carbonates, alkyl alkoxyacetates, alkyl pyruvates, dialkyl sulfoxides, cyclic sulfones, dialkyl ethers, monohydric alcohols, glycols, alkyl acetates, and N-alkylpyrrolidones.

[0145] Among them, organic cleaning solutions include propylene glycol monomethyl ether acetate, isopropanol, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, ethyl lactate, methyl methoxypropionate, cyclopentanone, cyclohexanone, gamma-butyrolactone, diisoamyl ether (isoamyl ether), butyl acetate, isoamyl acetate, 4-methyl-2-pentanol, dimethyl sulfoxide, N-methylpyrrolidone, diethylene glycol, ethylene glycol , dipropylene glycol, propylene glycol, ethylene carbonate, propylene carbonate, sulfolane, cycloheptanone, 2-heptanone, butyl butyrate, isobutyl isobutyrate, undecane, pentyl propionate, isopentyl propionate, ethylcyclohexane, mesitylene, decane, 3,7-dimethyl-3-octanol, 2-ethyl-1-hexanol, 1-octanol, 2-octanol, ethyl acetoacetate, dimethyl malonate, methyl pyruvate, and dimethyl oxalate.

[0146] The pretreatment preferably includes, for example, a step of immersing the filter to be treated in an organic cleaning liquid and / or a step of passing the organic cleaning liquid through the filter to be treated.

[0147] In the case where the pretreatment includes a step of immersing the filter to be treated in an organic cleaning liquid, the method of immersing the filter to be treated in the organic cleaning liquid may include a method of filling an immersion container with the organic cleaning liquid and immersing the filter to be treated in the organic cleaning liquid. As the immersion container, a housing contained in a filter unit in a filtration device described later can also be used. That is, a method can be used in which the filter to be treated (preferably contained in a filter cartridge described later) is housed in a housing contained in a filtration device, the housing is filled with the immersion liquid, and the housing is allowed to stand in this state. In addition to the above, there is also a method in which an immersion container is prepared separately from the housing contained in the purification apparatus (i.e., an immersion container is prepared outside the purification apparatus), the separately prepared immersion container is filled with the organic cleaning liquid, and the filter to be treated is immersed in the organic cleaning liquid. Among these, a method in which an immersion container prepared outside the filtration apparatus is filled with the organic cleaning solution and the filter to be treated is immersed in the organic cleaning solution is preferred, since impurities eluted from the filter to be treated are not mixed into the filtration apparatus.

[0148] The shape and size of the immersion container are not particularly limited and can be appropriately selected depending on the number and size of the filters to be immersed. The material of the immersion vessel is not particularly limited, but it is preferable that at least the liquid-contacting portion is made of a corrosion-resistant material described below. The material for the immersion container preferably contains at least one selected from the group consisting of polyfluorocarbons (PTFE, PFA: perfluoroalkoxyalkane, and PCTFE: polychlorotrifluoroethylene, etc.), PPS (polyphenylene sulfide), POM (polyoxymethylene), and polyolefins (PP, PE, etc.), more preferably contains at least one selected from the group consisting of polyfluorocarbons, PPS, and POM, even more preferably contains polyfluorocarbons, particularly preferably contains at least one selected from the group consisting of PTFE, PFA, and PCTFE, and most preferably contains PTFE. The immersion vessel is preferably washed before use, and is preferably washed with an organic washing liquid (so-called co-washing).

[0149] The immersion time is, for example, preferably one day or more, more preferably three days or more, even more preferably one week or more, and particularly preferably one month or more. There is no upper limit, but it is usually less than one year. The temperature of the organic cleaning solution during the immersion treatment is preferably at least room temperature (23° C.), more preferably at least 35° C. There is no particular upper limit, but it is usually below the boiling point of the organic cleaning solution used.

[0150] During the immersion, the treated filter may be subjected to ultrasonic treatment either continuously or temporarily. For example, when the filter body is used in the form of a hollow cylinder (for example, when the filter is used in a state where it is contained in a filter cartridge described below), the ultrasonic output is preferably 50 kW or more, more preferably 80 kW or more, and even more preferably 100 kW or more per inch of cylindrical length of the filter (filter to be treated) of the filter cartridge. There is no particular upper limit, but it is usually 200 kW. The duration of the ultrasonic treatment is, for example, preferably 5 minutes or more, more preferably 15 minutes or more, even more preferably 1 hour or more, and particularly preferably 3 hours or more. There is no particular upper limit, but it is usually less than 10 hours.

[0151] When the pretreatment includes a step of passing an organic cleaning liquid through the filter to be treated, for example, a method can be mentioned in which the filter (preferably contained in a cartridge with a filter) is housed in a housing of a filter unit of a filtration device described later, and an organic cleaning liquid is introduced into the housing to pass the organic cleaning liquid through the filter body to be treated.

[0152] During cleaning, the specific organic compounds contained in the filter to be treated are transferred (typically dissolved) into the organic cleaning liquid. Therefore, it is preferable that the organic cleaning liquid that has been passed through the filter once is not used again for cleaning, but is discharged outside the filtration device described below. In other words, it is preferable not to perform circulating cleaning.

[0153] Another embodiment of the method of passing an organic cleaning liquid through the filter to be treated for cleaning includes a method of cleaning the filter to be treated using a cleaning device. In this specification, the cleaning device means a device that is different from the filtration device and is provided outside the filtration device. The type of the cleaning device is not particularly limited, and a device with a similar configuration to the filtration device can be used.

[0154] When the pretreatment includes a step of passing an organic cleaning liquid through the filter body to be treated, the amount of the liquid passed is, for example, when the filter body to be treated has a hollow cylindrical shape (typically, when a filter cartridge containing the filter to be treated is contained in a housing of a filter unit and the organic cleaning liquid is passed through the filter body), preferably 10 kg or more, more preferably 50 kg or more, even more preferably 300 kg or more, and particularly preferably 500 kg or more per inch of the cylindrical length of the filter body to be treated. The temperature of the organic cleaning solution passed through is preferably at least room temperature (23° C.), more preferably at least 35° C. There is no particular upper limit, but it is usually below the boiling point of the organic cleaning solution used.

[0155] The pretreatment is preferably carried out so that the ratio of the content of specific organic compounds contained in the pretreated filter to the total content of specific organic compounds contained in the treated filter (untreated filter) (also called "cleanliness") is 0.5000 or less, more preferably 0.1000 or less, even more preferably 0.0300 or less, and particularly preferably 0.0100 or less. There is no particular lower limit, but it is usually 0.00001 or more.

[0156] [Filtration device] The filter of the present invention is preferably used by being installed in a filtration device. The above-mentioned filtering device preferably contains the filter of the present invention and is used for purifying a liquid to be purified to produce a liquid medicine. For example, the filtration device preferably contains an inflow section, an outflow section, and one or more (preferably two or more, more preferably 2 to 6, even more preferably 3 to 4, and particularly preferably 4) filters of the present invention, each filter being arranged in series between the inflow section and the outflow section, and containing a flow passage extending from the inflow section to the outflow section. The filtration device may have a plurality of filters arranged in parallel. In this case, it is preferable that the liquid to be purified passes through 1 or more (preferably 2 or more, more preferably 2 to 6, still more preferably 3 to 4, and particularly preferably 4) filters of the present invention regardless of which flow path the liquid to be purified takes from the inflow section to the outflow section. That is, the filtration device may combine both the parallel arrangement and the series arrangement of the plurality of filters.

[0157] In the filtration device, when two or more filters are arranged in series, among the two or more filters arranged in series, the pore diameter of at least one filter (preferably the filter with the largest pore diameter) is 10 to 200 nm, and the pore diameter of the filter with the smallest pore diameter is preferably 1 to 10 nm.

[0158] Further, among the two or more filters arranged in series, the filter body of at least one filter preferably contains an ion exchange group. Further, among the two or more filters arranged in series, the filter body of at least one filter is a filter body containing nylon, and the at least one filter contains at least an alkane represented by the general formula (X) and an alkene represented by the general formula (XI). It is also preferable that the content A of the alkane represented by the general formula (X), the content B of the alkene represented by the general formula (XI), and the content C of the alkene represented by the general formula (XII) satisfy C < A and C < B on a mass basis. Further, among the two or more filters arranged in series, the filter body of at least one filter contains polyethylene or polytetrafluoroethylene, and it is also preferable that the at least one filter contains one or more compounds selected from the above Group A and an alkane represented by the general formula (X). Further, among the two or more filters arranged in series, it is also preferable that the filter body of at least one filter (preferably more than half of the two or more filters, more preferably more than half of the two or more filters) is a filter body made of a material other than a fluorine-based material.

[0159] A filtration device including a filter of the present invention will be described below. In the following description, at least filter A is the filter of the present invention, and other filters (e.g., filter BU) may be filters other than the filter of the present invention. However, it is preferable that the filtration device has at least two or more filters of the present invention arranged in series between the inflow portion and the outflow portion, and it is more preferable that all of the filters in the filtration device are filters of the present invention.

[0160] First Embodiment FIG. 1 is a schematic diagram illustrating a filtering device according to a first embodiment of the present invention. The filtration device 100 is a filtration device in which a filter 103 (filter A) and a filter 104 (also referred to as filter BU) different from the filter 103 are arranged in series via a pipe 105 between an inflow section 101 and an outflow section . The inlet section 101, filter 104, piping 202, filter 103, and outlet section 102 are configured so that the liquid to be purified can flow therethrough, and the above components are connected to form a flow passage S1 (a path through which the liquid to be purified flows).

[0161] The inlet 101 and the outlet 102 are not particularly limited in form as long as they can introduce the liquid to be purified into the filtration device and discharge it, but typically include hollow cylindrical pipes (inlet and outlet) containing an inlet and an outlet. The following description will be given taking as an example a form in which the outlet and inlet are each pipes. The shapes of the inlet 101, the pipe 105, and the outlet 102 are not particularly limited, but typically include a hollow cylindrical shape formed to allow the purification liquid to flow therethrough. The materials for these are not particularly limited, but it is preferable that the liquid-contacting parts (parts that may come into contact with the purification liquid when filtering the purification liquid) contain the corrosion-resistant material described below as a material component (constituent component). In other words, it is preferable that they are formed using the corrosion-resistant material described below.

[0162] The liquid to be purified introduced from the inlet 101 of the filtration device 100 flows through the filtration device 100 along the flow path S1, during which it is filtered successively by a filter 103 (filter A) and a filter 104 (filter BU), and is discharged from the outlet 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 may include a pump, a damper, a valve, and the like (not shown) on the flow path S1 (e.g., the inlet (101), the pipe (105), the outlet (102), and the like) for the purpose of circulating the liquid to be purified. The method of circulating the liquid to be purified through the flow path in the filtration device 100 is not limited to the above, and may be a method of introducing pressurized liquid to be purified into the inlet.

[0163] The shape of the filter 103 (filter A) and the filter 104 (filter BU) is not particularly limited. Examples of the shape of the filter A and the filter BU include a planar shape, a pleated shape, a spiral shape, and a hollow cylindrical shape. Among them, in terms of superior handling properties, it is preferable to configure a cartridge with a filter (filter cartridge) that contains a core material formed of a material through which the liquid to be purified can permeate and / or has a structure through which the liquid to be purified can permeate, and a filter arranged on the core material in a form wound around the core material. In this case, the material of the core material is not particularly limited, but it is preferable that the core material is formed from a corrosion-resistant material described later. It should be noted that the core material is not a component of the filter.

[0164] Although there is no particular limitation on the method of arranging the filter, it is preferable to configure a filter unit arranged in a housing (not shown) that includes at least one inlet and at least one outlet, and has at least one flow passage formed between the inlet and the outlet. In this case, the filter is arranged to cross the flow passage in the housing. The flow passage formed in the housing forms a part of the flow passage S1, and the liquid to be purified is filtered by the filter arranged to cross the flow passage S1 when it flows through the flow passage S1.

[0165] The material of the housing can be any suitable rigid impermeable material, including, but not limited to, any impermeable thermoplastic material that is compatible with the liquid to be purified. For example, the housing can be made of a metal, such as stainless steel, or a polymer. In some embodiments, the housing is a polymer, such as polyacrylate, polypropylene, polystyrene, or polycarbonate. In order to obtain a filtration device having the excellent effect of the present invention, it is preferable that at least a part of the liquid-contacting part of the housing, preferably 90% of the surface area of ​​the liquid-contacting part, and more preferably 99% of the surface area of ​​the liquid-contacting part, is made of a corrosion-resistant material described below. In this specification, the liquid-contacting part means a part that may come into contact with the purified liquid (excluding the filter itself), and refers to the inner wall of a unit such as a housing.

[0166] (Filter BU) Filter BU is a filter disposed in series with filter A on the flow path. Filter BU is a filter disposed in series with filter A on the flow path, upstream of filter A. It is preferable that filter A and filter BU are different filters. In this specification, a filter different from filter A means a filter that is different from filter A in at least one selected from the group consisting of material, pore size, and pore structure. In particular, in order to obtain a filtration device having a more excellent effect of the present invention, it is preferable that filter BU differs from filter A in at least one selected from the group consisting of pore size and material, and it is preferable that at least the materials are different. In this specification, when filter A and filter BU are made of different materials, this typically includes a case where the components (material components) contained in each filter are different; and when the filter is made of resin, a case where the types of substituents arranged on the filter surface are different due to differences in surface treatment.

[0167] The pore size of the filter BU is not particularly limited, and may have any pore size as a filter used in a filtration device. In particular, the filter BU preferably has a pore size larger than that of the filter A, in that a chemical solution having a more excellent defect suppression property can be obtained. In particular, the pore size of the filter BU is preferably 200 nm or less, more preferably 10 nm or more, and more preferably 20 nm or more. According to the study by the present inventors, it has been found that when a filtration device is used in which a filter BU having a pore size of 20 nm or more is disposed on the flow path S1 upstream of the filter A, the filter A is less likely to become clogged, and the life of the filter A can be extended. As a result, a filtration device capable of stably providing a chemical solution having superior defect suppression properties can be obtained.

[0168] In particular, when the filtration device contains a plurality of filters BU, the pore size of the filter BU arranged at the most upstream side in the flow passage is preferably 20 nm or more, more preferably 50 nm or more, and preferably 200 nm or less. When the pore size of the filter BU arranged at the most upstream side in the flow passage (which may be filter C described later) is within the above range, the life of the filter is further improved, and as a result, a chemical solution having excellent defect suppression properties can be stably produced, which is preferable.

[0169] Although the filtration device in Fig. 1 includes one filter BU, the filtration device according to this embodiment may include multiple filters BU. In this case, the relationship between the pore sizes of the multiple filters BU is not particularly limited, but it is preferable that the pore size of the filter BU arranged most upstream on the flow path is the largest, since it is easier to obtain a chemical solution containing more excellent defect suppression properties. In this way, the life of the filters (including filter A) arranged downstream of the most upstream filter BU can be extended, and as a result, a filtration device that can stably provide a chemical solution containing more excellent defect suppression properties can be obtained.

[0170] When at least one of the filters BU contained in the filtration device contains a resin containing an ion exchange group as a material component, the filter BU has a stronger interaction with metal impurities (e.g., metal ions, etc.) contained in the liquid to be purified. As a result, the content of metal ions in the obtained chemical solution can be reduced, and the obtained chemical solution has better pattern width uniformity performance.

[0171] [Method of manufacturing chemical solution] The method for producing a chemical liquid according to an embodiment of the present invention is a method for producing a chemical liquid, in which a liquid to be purified is purified to obtain a chemical liquid, and includes a filtration step in which the liquid to be purified is filtered using the filter of the present invention (a filtration device containing the filter of the present invention) already described to obtain the chemical liquid.

[0172] <Liquid to be purified> The liquid to be purified to which the method for producing a chemical liquid according to the embodiment of the present invention can be applied is not particularly limited, but preferably contains a solvent. Examples of the solvent include organic solvents and water, and preferably contains an organic solvent. In the following, the liquid to be purified is divided into an organic solvent-based liquid to be purified in which the content of the organic solvent (the total content when multiple organic solvents are contained) exceeds 50 mass% relative to the total mass of the solvents contained in the liquid to be purified, and an aqueous liquid to be purified in which the content of water exceeds 50 mass% relative to the total mass of the solvents contained in the liquid to be purified.

[0173] (Organic solvent-based liquid to be purified) Organic solvents The organic solvent-based liquid to be purified contains a solvent, and the content of the organic solvent is more than 50 mass % based on the total mass of the solvent contained in the liquid to be purified. The organic solvent-based liquid to be purified contains an organic solvent. The content of the organic solvent in the organic solvent-based liquid to be purified is not particularly limited, but is generally preferably 99.0 mass% or more based on the total mass of the organic solvent-based liquid to be purified. The upper limit is not particularly limited, but is generally preferably 99.99999 mass% or less. The organic solvent may be used alone or in combination of two or more. When two or more organic solvents are used in combination, the total content is preferably within the above range.

[0174] In this specification, an organic solvent refers to a liquid organic compound contained in the above-mentioned purification target liquid at a content of more than 10,000 ppm by mass per component relative to the total mass of the above-mentioned purification target liquid. In other words, in this specification, a liquid organic compound contained in the above-mentioned purification target liquid at a content of more than 10,000 ppm by mass relative to the total mass of the above-mentioned purification target liquid corresponds to an organic solvent. In this specification, the term "liquid" means that the material is liquid at 25° C. and atmospheric pressure.

[0175] The organic solvent-based liquid to be purified (or the produced chemical liquid) may have a volume resistivity of 500,000,000 Ωm or more. The volume resistivity of the organic solvent-based liquid to be purified (or the produced chemical liquid) can be measured, for example, using a volume resistivity meter SME-8310 or a super insulation meter SM-8220 manufactured by Hioki Electric Corporation.

[0176] The type of organic solvent for the liquid to be purified is not particularly limited, and any known organic solvent can be used. Examples of the organic solvent include alkylene glycol monoalkyl ether carboxylate, alkylene glycol monoalkyl ether, alkyl lactate, alkyl alkoxypropionate, cyclic lactone (preferably having 4 to 10 carbon atoms), monoketone compound that may contain a ring (preferably having 4 to 10 carbon atoms), alkylene carbonate, alkyl alkoxyacetate, alkyl pyruvate, dialkyl sulfoxide, cyclic sulfone, dialkyl ether, monohydric alcohol, glycol, alkyl acetate, and N-alkylpyrrolidone. As the organic solvent, for example, organic solvents described in JP-A-2016-57614, JP-A-2014-219664, JP-A-2016-138219, and JP-A-2015-135379 may be used.

[0177] Examples of the organic solvent include propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, propylene glycol monopropyl ether, cyclohexanone, methyl methoxypropionate, butyl acetate, γ-butyrolactone, 4-methyl-2-pentanol, propylene glycol monoethyl ether, ethyl lactate, cyclopentanone, diisoamyl ether (isoamyl ether), isoamyl acetate, isopropanol, dimethyl sulfoxide, N-methylpyrrolidone, diethylene glycol, ethylene glycol Preferred is one or more selected from the group consisting of ethanol, dipropylene glycol, propylene glycol, ethylene carbonate, propylene carbonate, sulfolane, cycloheptanone, 2-heptanone, butyl butyrate, isobutyl isobutyrate, undecane, pentyl propionate, isopentyl propionate, ethylcyclohexane, mesitylene, decane, 3,7-dimethyl-3-octanol, 2-ethyl-1-hexanol, 1-octanol, 2-octanol, ethyl acetoacetate, dimethyl malonate, methyl pyruvate, and dimethyl oxalate.

[0178] The type and content of the organic solvent in the liquid to be purified can be measured using a gas chromatograph mass spectrometer.

[0179] The organic solvent to be purified has a Hansen solubility parameter distance for eicosene of, for example, 3 to 20 MPa. 0.5 (More preferably 5 to 20 MPa 0.5 ) is also preferred. When two or more organic solvents are used, it is preferable that at least one of them satisfies the above-mentioned range of Hansen solubility parameters. When two or more organic solvents are used, it is preferable that the weighted average value of the Hansen solubility parameters based on the molar ratio of the contents of the respective organic solvents satisfies the above-mentioned range of the Hansen solubility parameters.

[0180] For example, from the viewpoint of more excellent defect suppression of the chemical solution, it is also preferable that the organic solvent-based purification liquid contains substantially only organic solvents that satisfy the above-mentioned Hansen solubility parameter range. The organic solvent-based purification liquid contains substantially only organic solvents that satisfy the above-mentioned Hansen solubility parameter range means that the content of the organic solvents that satisfy the above-mentioned Hansen solubility parameter range is 99 mass% or more (preferably 99.9 mass% or more) with respect to the total mass of the organic solvents.

[0181] Also, for example, it is preferable that the organic solvent-based liquid to be purified is a mixed solvent containing both an organic solvent that satisfies the above-mentioned range of Hansen solubility parameters and an organic solvent that does not satisfy the above-mentioned range of Hansen solubility parameters. In this case, from the viewpoint of better defect suppression in the obtained chemical liquid, it is preferable that the organic solvent-based purified liquid (mixed solvent) contains 20 to 80 mass % (preferably 30 to 70 mass %) of an organic solvent satisfying the above-mentioned Hansen solubility parameter range, based on the total mass of the organic solvent-based purified liquid, and contains 20 to 80 mass % (preferably 30 to 70 mass %) of an organic solvent not satisfying the above-mentioned Hansen solubility parameter range, based on the total mass of the organic solvent-based purified liquid. When the content of the organic solvent satisfying the above-mentioned Hansen solubility parameter range and the content of the organic solvent not satisfying the above-mentioned Hansen solubility parameter range are each at a certain level or more, the affinity of the chemical solution for the metal-based material and the organic-based material can be adjusted to a suitable range, compared with the case where the organic solvent not satisfying the above-mentioned Hansen solubility parameter range is an amount outside a predetermined range (e.g., 1% by mass or more but less than 20% by mass or more or more than 80% by mass based on the total mass of the mixed solvent), and it is considered that the effect of the present invention is more excellent. In this case, the total content of the organic solvent satisfying the above-mentioned range of Hansen solubility parameters and the organic solvent not satisfying the above-mentioned range of Hansen solubility parameters is preferably 99.0 mass% or more based on the total mass of the organic solvent-based purified liquid. Although there is no particular upper limit, it is generally preferably 99.99999 mass% or less. In addition, the distance of the Hansen solubility parameter for eicosene in organic solvents that do not satisfy the above Hansen solubility parameter range is 0 MPa.0.5 More than 3MPa 0.5 Less than (preferably 0 MPa 0.5 Super 3MPa 0.5 less than 20MPa 0.5 More than (preferably 20MPa 0.5 Super 50MPa 0.5 (see below).

[0182] In this specification, the Hansen solubility parameters are intended to mean the Hansen solubility parameters described in "Hansen Solubility Parameters: A Users Handbook, Second Edition" (pages 1-310, CRC Press, published in 2007) etc. That is, the Hansen solubility parameters express solubility as a multidimensional vector (dispersion term (δd), dipole-dipole term (δp), and hydrogen bond term (δh)), and these three parameters are considered to be the coordinates of a point in a three-dimensional space called the Hansen space. The Hansen solubility parameter distance is the distance between two compounds in the Hansen space, and the Hansen solubility parameter distance can be calculated using the following formula: (Ra) 2 = 4(δd2-δd1) 2 +(δp2-δp1) 2 +(δh2-δh1) 2 Ra: Distance between the Hansen solubility parameters of the first and second compounds (unit: MPa 0.5 ) δd1: Dispersion term of the first compound (unit: MPa 0.5 ) δd2: Dispersion term of the second compound (unit: MPa 0.5 ) δp1: dipole-dipole term of the first compound (unit: MPa 0.5 ) δp2: dipole-dipole term of the second compound (unit: MPa 0.5 ) δh1: Hydrogen bond term of the first compound (unit: MPa 0.5 ) δh2: Hydrogen bond term of the second compound (unit: MPa 0.5 ) In this specification, the Hansen solubility parameter of a compound is specifically calculated using HSPiP (Hansen Solubility Parameter in Practice).

[0183] Other Ingredients The liquid to be purified may contain other components in addition to those described above, such as inorganic substances (metal ions, metal particles, metal oxide particles, etc.), resins, organic substances other than resins, and water.

[0184] ·Inorganic matter The liquid to be purified may contain inorganic substances. The inorganic substances are not particularly limited, and examples thereof include metal ions and metal-containing particles.

[0185] The metal-containing particles may contain metal atoms, and the form of the metal-containing particles is not particularly limited. For example, the metal-containing particles may be a single metal atom, a compound containing a metal atom (hereinafter also referred to as a "metal compound"), or a composite thereof. The metal-containing particles may contain a plurality of metal atoms.

[0186] The composite is not particularly limited, but examples thereof include so-called core-shell type particles containing a simple metal atom and a metal compound that covers at least a portion of the simple metal atom, solid solution particles containing a metal atom and other atoms, eutectic particles containing a metal atom and other atoms, aggregate particles of a simple metal atom and a metal compound, aggregate particles of different types of metal compounds, and metal compounds whose composition changes continuously or intermittently from the particle surface to the center.

[0187] The atoms other than the metal atom contained in the metal compound are 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.

[0188] The metal atom is not particularly limited, but may be Al (aluminum), B (boron), Ba (barium), Ca (calcium), Cd (cadmium), Co (cobalt), Cr (chromium), Cu (copper), Fe (iron), K (potassium), Li (lithium), Mg (magnesium), Mn (manganese), Mo (molybdenum), Na (sodium), Ni (nickel), P (phosphorus), Pb (lead), Sb (antimony), Si (silicon), Ti (titanium), V (vanadium), and Zn (zinc). The metal-containing particles may contain one type of the above metal atom alone or two or more types in combination.

[0189] The particle size of the metal-containing particles is not particularly limited, but is generally in the range of 1 to 100 nm.

[0190] The inorganic substance may be added to the liquid to be purified, or may be unintentionally mixed into the liquid to be purified during the manufacturing process. Examples of cases where the inorganic substance is unintentionally mixed during the manufacturing process of the chemical include cases where the inorganic substance is contained in a raw material (e.g., an organic solvent) used in the manufacturing of the chemical, and cases where the inorganic substance is mixed during the manufacturing process of the chemical (e.g., contamination), but are not limited to the above.

[0191] ··resin The liquid to be purified may contain a resin. The chemical solution may further contain a resin, preferably a resin P that contains a group that is decomposed by the action of an acid to generate a polar group.

[0192] The resin P is preferably a resin containing a repeating unit represented by formula (AI) described below, which is a resin whose solubility in a developer mainly composed of an organic solvent decreases under the action of an acid. The resin containing a repeating unit represented by formula (AI) described below contains a group that decomposes under the action of an acid to generate an alkali-soluble group (hereinafter, also referred to as an "acid-decomposable group"). The polar group may be an alkali-soluble group, such as a carboxy group, a fluorinated alcohol group (preferably a hexafluoroisopropanol group), a phenolic hydroxyl group, or a sulfo group.

[0193] In the acid-decomposable group, the polar group is protected by a group that is detached by an acid (acid-detachable group). Examples of the acid-detachable group include -C(R 36 )(R 37 )(R 38 ), -C(R 36 )(R 37 )(OR 39 ), and -C(R 01 )(R 02 )(OR 39 ) etc.

[0194] In the formula, R 36 ~R 39 R each independently represents an alkyl group, a cycloalkyl group, an aryl group, an aralkyl group, or an alkenyl group. 36 and R 37 may be bonded to each other to form a ring.

[0195] 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.

[0196] The resin P, the solubility of which in a developer mainly composed of an organic solvent decreases due to the action of an acid, will be described in detail below.

[0197] Formula (AI): Repeating unit containing an acid-decomposable group Resin P preferably contains a repeating unit represented by formula (AI).

[0198] [ka]

[0199] In formula (AI), Xa1 represents a hydrogen atom or an alkyl group which may contain a substituent. T represents a single bond or a divalent linking group. Ra1 to Ra3 each independently represent an alkyl group (straight-chain or branched-chain) or a cycloalkyl group (monocyclic or polycyclic). Two of Ra1 to Ra3 may be bonded to form a cycloalkyl group (monocyclic or polycyclic).

[0200] Examples of the alkyl group represented by Xa1, which may have a substituent, include a methyl group and -CH-R 11 Examples of the group represented by R 11 represents a halogen atom (such as a fluorine atom), a hydroxyl group, or a monovalent organic group. Xa1 is preferably a hydrogen atom, a methyl group, a trifluoromethyl group or a hydroxymethyl group.

[0201] Examples of the divalent linking group for T include an alkylene group, a -COO-Rt- group, and a -O-Rt- group, in which 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 -CH2- group, a -(CH2)2- group, or a -(CH2)3- group.

[0202] The alkyl groups Ra1 to Ra3 are preferably alkyl groups having 1 to 4 carbon atoms.

[0203] The cycloalkyl group of Ra1 to Ra3 is preferably a monocyclic cycloalkyl group such as a cyclopentyl group or a cyclohexyl group, or a polycyclic cycloalkyl group such as a norbornyl group, a tetracyclodecanyl group, a tetracyclododecanyl group, or an adamantyl group. The cycloalkyl group formed by combining two of Ra1 to Ra3 is preferably a monocyclic cycloalkyl group such as a cyclopentyl group or a cyclohexyl group, or a polycyclic cycloalkyl group such as a norbornyl group, a tetracyclodecanyl group, a tetracyclododecanyl group, an adamantyl group, etc. A monocyclic cycloalkyl group having 5 to 6 carbon atoms is more preferable.

[0204] The cycloalkyl group formed by combining two of Ra1 to Ra3 may have, for example, one of the methylene groups constituting the ring replaced with a heteroatom such as an oxygen atom, or a group containing a heteroatom such as a carbonyl group.

[0205] In the repeating unit represented by formula (AI), for example, Ra1 is a methyl group or an ethyl group, and Ra2 and Ra3 are bonded to form the above-mentioned cycloalkyl group.

[0206] Each of the above groups may contain a substituent. Examples of the substituent include an alkyl group (having 1 to 4 carbon atoms), a halogen atom, a hydroxyl group, an alkoxy group (having 1 to 4 carbon atoms), a carboxy group, and an alkoxycarbonyl group (having 2 to 6 carbon atoms), and the like, preferably having 8 or less carbon atoms.

[0207] The content of the repeating unit represented by formula (AI) is preferably from 20 to 90 mol %, more preferably from 25 to 85 mol %, and even more preferably from 30 to 80 mol %, based on all repeating units in the resin P.

[0208] Repeating units containing lactone structures Furthermore, the resin P preferably contains a repeating unit Q that contains a lactone structure.

[0209] The repeating unit Q containing a lactone structure preferably contains a lactone structure in the side chain, and is more preferably a repeating unit derived from a (meth)acrylic acid derivative monomer. The repeating unit Q containing a lactone structure may be used alone or in combination of two or more kinds, but it is preferable to use only one kind. The content of the repeating unit Q containing 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.

[0210] The lactone structure is preferably a 5- to 7-membered lactone structure, and more preferably a structure in which another ring structure is condensed with the 5- to 7-membered lactone structure to form a bicyclo structure or a spiro structure. The lactone structure preferably contains a repeating unit containing a lactone structure represented by any one of the following formulae (LC1-1) to (LC1-17). The lactone structure is preferably a lactone structure represented by formula (LC1-1), (LC1-4), (LC1-5), or (LC1-8), and more preferably a lactone structure represented by formula (LC1-4).

[0211] [ka]

[0212] The lactone structure portion may contain a substituent (Rb2). Preferred examples of the substituent (Rb2) 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, a carboxy group, a halogen atom, a hydroxyl group, a cyano group, and an acid-decomposable group. n2 represents an integer of 0 to 4. When n2 is 2 or more, the multiple substituents (Rb2) present may be the same or different, and the multiple substituents (Rb2) present may be bonded to each other to form a ring.

[0213] Repeating units containing phenolic hydroxyl groups Furthermore, the resin P may contain a repeating unit containing a phenolic hydroxyl group. An example of the repeating unit containing a phenolic hydroxyl group is a repeating unit represented by the following general formula (I).

[0214] [ka]

[0215] During the ceremony, 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. 42 may be bonded to Ar4 to form a ring, in which case R 42 represents a single bond or an alkylene group.

[0216] X4 is a single bond, -COO-, or -CONR 64 - represents R 64 represents a hydrogen atom or an alkyl group. L4 represents a single bond or an alkylene group. Ar4 represents an (n+1)-valent aromatic ring group; R 42 When it bonds with the ring, it represents an (n+2)-valent aromatic ring group. n represents an integer of 1 to 5.

[0217] R in general formula (I) 41 , R 42 and R 43 The alkyl group may have a substituent, and is preferably an alkyl group having 20 or less carbon atoms, such as a methyl group, an ethyl group, a propyl group, an isopropyl group, an n-butyl group, a sec-butyl group, a hexyl group, a 2-ethylhexyl group, an octyl group, or a dodecyl group, more preferably an alkyl group having 8 or less carbon atoms, and even more preferably an alkyl group having 3 or less carbon atoms.

[0218] R in general formula (I) 41 , R 42 and R 43The cycloalkyl group may be a monocyclic or polycyclic cycloalkyl group, and is preferably a monocyclic cycloalkyl group having 3 to 8 carbon atoms, such as a cyclopropyl group, a cyclopentyl group, or a cyclohexyl group, which may contain a substituent.

[0219] R in general formula (I) 41 , R 42 and R 43 Examples of the halogen atom include a fluorine atom, a chlorine atom, a bromine atom and an iodine atom, with a fluorine atom being preferred.

[0220] R in general formula (I) 41 , R 42 and R 43 The alkyl group contained in the alkoxycarbonyl group of R 41 , R 42 and R 43 The same groups as the alkyl group in the above formula are preferred.

[0221] Examples of the substituent in each of the above groups include an alkyl group, a cycloalkyl group, an aryl group, an amino group, an amido group, a ureido group, a urethane group, a hydroxy group, a carboxy group, a halogen atom, an alkoxy group, a thioether group, an acyl group, an acyloxy group, an alkoxycarbonyl group, a cyano group, and a nitro group, and the number of carbon atoms of the substituent is preferably 8 or less.

[0222] Ar4 represents an aromatic ring group having a valence of (n+1). When n is 1, the divalent aromatic ring group may contain a substituent, and examples thereof include arylene groups 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 a heterocycle, such as thiophene, furan, pyrrole, benzothiophene, benzofuran, benzopyrrole, triazine, imidazole, benzimidazole, triazole, thiadiazole, and thiazole.

[0223] Specific examples of the (n+1)-valent aromatic ring group when n is an integer of 2 or more include groups obtained by removing any (n-1) hydrogen atoms from the above-mentioned specific examples of the divalent aromatic ring group. The (n+1)-valent aromatic ring group may further contain a substituent.

[0224] Examples of the substituent that the above-mentioned 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 alkoxy groups such as a methoxy group, an ethoxy group, a hydroxyethoxy group, a propoxy group, a hydroxypropoxy group, and a butoxy group; and aryl groups such as a phenyl group.

[0225] -CONR represented by X4 64 -(R 64 represents a hydrogen atom or an alkyl group) 64 Examples of the alkyl group include alkyl groups having 20 or less carbon atoms, such as methyl, ethyl, propyl, isopropyl, n-butyl, sec-butyl, hexyl, 2-ethylhexyl, octyl, and dodecyl groups, which may have a substituent, and alkyl groups having 8 or less carbon atoms are more preferred.

[0226] X4 is preferably a single bond, -COO- or -CONH-, more preferably a single bond or -COO-.

[0227] The alkylene group in L4 is preferably 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, or an octylene group, which may contain a substituent.

[0228] Ar4 is preferably an aromatic ring group having 6 to 18 carbon atoms which may contain a substituent, and more preferably a benzene ring group, a naphthalene ring group or a biphenylene ring group.

[0229] The repeating unit represented by formula (I) preferably has a hydroxystyrene structure, i.e., Ar4 is preferably a benzene ring group.

[0230] The content of the repeating unit containing a phenolic hydroxyl group is preferably from 0 to 50 mol %, more preferably from 0 to 45 mol %, and even more preferably from 0 to 40 mol %, based on all repeating units in the resin P.

[0231] Repeating units containing organic groups that contain polar groups Resin P may further contain a repeating unit containing an organic group containing a polar group, in particular a repeating unit containing an alicyclic hydrocarbon structure substituted with a polar group, which improves the substrate adhesion and developer affinity. The alicyclic hydrocarbon structure substituted with a polar group is preferably an adamantyl group, a diamantyl group, or a norbornane group, and the polar group is preferably a hydroxyl group or a cyano group.

[0232] When the resin P contains a repeating unit containing an organic group containing a polar group, the content thereof is preferably 1 to 50 mol %, more preferably 1 to 30 mol %, still more preferably 5 to 25 mol %, and particularly preferably 5 to 20 mol %, based on the total repeating units in the resin P.

[0233] Repeating units represented by formula (VI) Resin P may contain a repeating unit represented by the following general formula (VI).

[0234] [ka]

[0235] In 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. 62may be bonded to Ar6 to form a ring, in which case R 62 represents a single bond or an alkylene group. X6 is a single bond, -COO-, or -CONR 64 - stands for R 64 represents a hydrogen atom or an alkyl group. L6 represents a single bond or an alkylene group. Ar6 represents an (n+1)-valent aromatic ring group; R 62 When it bonds with the ring, it represents an (n+2)-valent aromatic ring group. When n is 2 or more, Y2 each independently represents a hydrogen atom or a group which is eliminated by the action of an acid, provided that at least one of Y2 represents a group which is eliminated by the action of an acid. n represents an integer of 1 to 4.

[0236] As the group Y2 which is eliminated by the action of an acid, a structure represented by the following general formula (VI-A) is preferable.

[0237] [ka]

[0238] L1 and L2 each independently represent a hydrogen atom, an alkyl group, a cycloalkyl group, an aryl group, or a group formed by combining an alkylene group with an aryl group. M represents a single bond or a divalent linking group. Q represents an alkyl group, a cycloalkyl group which may contain a heteroatom, an aryl group which may contain a heteroatom, an amino group, an ammonium group, a mercapto group, a cyano group, or an aldehyde group. At least two of Q, M and L1 may be bonded to form a ring (preferably a 5- or 6-membered ring).

[0239] The repeating unit represented by the above general formula (VI) is preferably a repeating unit represented by the following general formula (3).

[0240] [ka]

[0241] In general formula (3), Ar3 represents an aromatic ring group. R3 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. M3 represents a single bond or a divalent linking group. Q3 represents an alkyl group, a cycloalkyl group, an aryl group or a heterocyclic group. At least two of Q3, M3 and R3 may be combined to form a ring.

[0242] The aromatic ring group represented by Ar3 is the same as Ar6 in the above general formula (VI) when n is 1, and is preferably a phenylene group or a naphthylene group, more preferably a phenylene group.

[0243] Repeating units containing silicon atoms in the side chain The resin P may further contain a repeating unit containing a silicon atom in the side chain. Examples of the repeating unit containing a silicon atom in the side chain include a (meth)acrylate repeating unit containing a silicon atom and a vinyl repeating unit containing a silicon atom. The repeating unit containing a silicon atom in the side chain is typically a repeating unit containing a group containing a silicon atom in the side chain, and examples of the group containing a silicon atom include a trimethylsilyl group, a triethylsilyl group, a triphenylsilyl group, a tricyclohexylsilyl group, a tristrimethylsiloxysilyl group, a tristrimethylsilylsilyl group, a methylbistrimethylsilylsilyl group, a methylbistrimethylsiloxysilyl group, a dimethyltrimethylsilylsilyl group, a dimethyltrimethylsiloxysilyl group, and the following cyclic or linear polysiloxanes, or cage, ladder, or random silsesquioxane structures. In the formula, R and R 1 each independently represents a monovalent substituent. * represents a bond.

[0244] [ka]

[0245] Preferred examples of the repeating unit containing the above group include a repeating unit derived from an acrylate compound or methacrylate compound containing the above group, or a repeating unit derived from a compound containing the above group and a vinyl group.

[0246] When the resin P contains the repeating unit containing a silicon atom in the side chain, the content thereof is preferably 1 to 30 mol %, more preferably 5 to 25 mol %, and even more preferably 5 to 20 mol %, based on the total repeating units in the resin P.

[0247] The weight average molecular weight of the resin P, as calculated as a polystyrene equivalent by GPC (gel permeation chromatography), is preferably 1,000 to 200,000, more preferably 3,000 to 20,000, and even more preferably 5,000 to 15,000. By setting the weight average molecular weight to 1,000 to 200,000, deterioration of heat resistance and dry etching resistance can be prevented, and deterioration of developability and deterioration of film formability due to an increase in viscosity can be prevented.

[0248] The dispersity (molecular weight distribution) is usually 1 to 5, preferably 1 to 3, more preferably 1.2 to 3.0, and even more preferably 1.2 to 2.0.

[0249] Other components contained in the chemical solution (for example, an acid generator, a basic compound, a quencher, a hydrophobic resin, a surfactant, a solvent, and the like) may all be known components.

[0250] (Water-based liquid to be purified) The aqueous liquid to be purified contains water in an amount of more than 50 mass %, preferably 51 to 95 mass %, based on the total mass of the solvent contained in the aqueous liquid to be purified. The water is not particularly limited, but is preferably ultrapure water used in semiconductor manufacturing, and more preferably water obtained by further purifying the ultrapure water to reduce inorganic anions and metal ions. The purification method is not particularly limited, but purification using a filtration membrane or an ion exchange membrane, and purification by distillation are preferred. In addition, purification is preferably performed by the method described in JP-A-2007-254168, for example.

[0251] Oxidizing agents The aqueous solution to be purified may contain an oxidizing agent, but the oxidizing agent is not particularly limited and any known oxidizing agent can be used. Examples of the oxidizing agent include hydrogen peroxide, peroxide, nitric acid, nitrates, iodates, periodates, hypochlorites, chlorites, chlorates, perchlorates, persulfates, dichromates, permanganates, ozone water, silver (II) salts, and iron (III) salts.

[0252] The content of the oxidizing agent is not particularly limited, but is preferably 0.1% by mass or more and 99.0% by mass or less based on the total mass of the aqueous liquid to be purified. The oxidizing agent may be used alone or in combination of two or more. When two or more oxidizing agents are used in combination, the total content is preferably within the above range.

[0253] ·Inorganic acid The aqueous purification liquid may contain an inorganic acid. There is no particular limitation on the inorganic acid, and any known inorganic acid may be used. Examples of inorganic acids include sulfuric acid, phosphoric acid, and hydrochloric acid. Note that inorganic acids are not included in the above-mentioned oxidizing agents. The content of inorganic acid in the aqueous liquid to be purified is not particularly limited, but is preferably 0.01% by mass or more and 99.0% by mass or less based on the total mass of the aqueous liquid to be purified. The inorganic acid may be used alone or in combination of two or more. When two or more inorganic acids are used in combination, the total content is preferably within the above range.

[0254] ·Corrosion inhibitor The aqueous solution to be purified may contain a corrosion inhibitor. The corrosion inhibitor is not particularly limited, and known corrosion inhibitors can be used. Examples of the corrosion inhibitor 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, and 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-mercaptobenzothiazole (2-MBT), 1-phenyl-2-tetrazoline-5-thione, 2-mercaptobenzimidazole (2-MBI), 4-methyl-2-phenylimidazole, 2-mercaptothiazoline, 2,4-diamino-6-methyl-1,3,5-triazine, thiazole, imide dazole, benzimidazole, triazine, methyltetrazole, bismuthiol I, 1,3-dimethyl-2-imidazolidinone, 1,5-pentamethylenetetrazole, 1-phenyl-5-mercaptotetrazole, diaminomethyltriazine, imidazolinethione, 4-methyl-4H-1,2,4-triazole-3-thiol, 5-amino-1,3,4-thiadiazole-2-thiol, benzothiazole, tritolyl phosphate, indazole, adenine, cytosine Synthin, guanine, thymine, phosphate inhibitors, amines, pyrazoles, propanethiol, silanes, secondary amines, benzohydroxamic acids, heterocyclic nitrogen inhibitors, ascorbic acid, thiourea, 1,1,3,3-tetramethylurea, urea, urea derivatives, uric acid, potassium ethylxanthate, glycine, dodecylphosphonic acid, iminodiacetic acid, boric acid, malonic acid, succinic acid, nitrilotriacetic acid, sulfolane, 2,3,5-trimethylpyrazine, 2-ethyl-3,5-Dimethylpyrazine, quinoxaline, acetylpyrrole, pyridazine, histadine, pyrazine, glutathione (reduced form), cysteine, cystine, thiophene, mercaptopyridine N-oxide, thiamine HCl, tetraethylthiuram disulfide, 2,5-dimercapto-1,3-thiadiazole ascorbic acid, ascorbic acid, catechol, t-butylcatechol, phenol, and pyrogallol.

[0255] Examples of the anticorrosive agent that may be used include aliphatic carboxylic acids such as dodecanoic acid, palmitic acid, 2-ethylhexanoic acid, and cyclohexanoic acid; and carboxylic acids having a chelating ability such as citric acid, malic acid, oxalic acid, malonic acid, succinic acid, itaconic acid, maleic acid, glycolic 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, 1-aminoanthraquinone-2-carboxylic acid, tannic acid, and gallic acid.

[0256] Examples of the anticorrosive agent include anionic surfactants such as coconut fatty acid salts, castor sulfate oil salts, lauryl sulfate salts, polyoxyalkylene allyl phenyl ether sulfate salts, alkylbenzene sulfonic acid, alkylbenzene sulfonate salts, alkyl diphenyl ether disulfonate salts, alkyl naphthalene sulfonate salts, dialkyl sulfosuccinate salts, isopropyl phosphate, polyoxyethylene alkyl ether phosphate salts, and polyoxyethylene allyl phenyl ether phosphate salts; cationic surfactants such as oleylamine acetate, lauryl pyridinium chloride, cetyl pyridinium chloride, lauryl trimethyl ammonium chloride, stearyl trimethyl ammonium chloride, behenyl trimethyl ammonium chloride, and didecyl dimethyl ammonium chloride; amphoteric surfactants such as coconut alkyl dimethyl amine oxide, fatty acid amidopropyl dimethyl amine oxide, alkyl polyaminoethyl glycine hydrochloride, amido betaine type surfactants, alanine type surfactants, and lauryl imino dipropionic acid. Surfactants: nonionic surfactants of polyoxyalkylene primary alkyl ethers or polyoxyalkylene secondary alkyl ethers, such as polyoxyethylene octyl ether, polyoxyethylene decyl ether, polyoxyethylene lauryl ether, polyoxyethylene laurylamine, polyoxyethylene oleylamine, polyoxyethylene polystyrylphenyl ether, polyoxyalkylene polystyrylphenyl ether, other polyoxyalkylene-based nonionic surfactants, such as polyoxyethylene dilaurate, polyoxyethylene laurate, polyoxyethylenated castor oil, polyoxyethylenated hydrogenated castor oil, sorbitan laurate, polyoxyethylene sorbitan laurate, and fatty acid diethanolamide; fatty acid alkyl esters, such as octyl stearate and trimethylolpropane tridecanoate; and polyether polyols, such as polyoxyalkylene butyl ether, polyoxyalkylene oleyl ether, and trimethylolpropane tris(polyoxyalkylene)ether, may also be used. Examples of the commercially available products include Newkalgen FS-3PG (manufactured by Takemoto Yushi Co., Ltd.) and Hosten HLP-1 (manufactured by Nikko Chemicals Co., Ltd.).

[0257] Moreover, a hydrophilic polymer may be used as the anticorrosive agent. Examples of hydrophilic polymers include polyglycols such as polyethylene glycol, alkyl ethers of polyglycols, polyvinyl alcohol, polyvinylpyrrolidone, polysaccharides such as alginic acid, polymethacrylic acid, carboxylic acid-containing polymers such as polyacrylic acid, polyacrylamide, polymethacrylamide, and polyethyleneimine, etc. 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.

[0258] Moreover, a cerium salt may be used as the anticorrosive agent. The cerium salt is not particularly limited, and any known cerium salt can be used. Examples of cerium salts include trivalent cerium salts such as cerium acetate, cerium nitrate, cerium chloride, cerium carbonate, cerium oxalate, and cerium sulfate, and examples of tetravalent cerium salts include cerium sulfate, ammonium cerium sulfate, ammonium cerium nitrate, diammonium cerium nitrate, and cerium hydroxide.

[0259] The corrosion inhibitor may include substituted or unsubstituted benzotriazoles. Suitable substituted benzotriazoles include, but are not limited to, benzotriazoles substituted with alkyl, aryl, halogen, amino, nitro, alkoxy, or hydroxyl groups. Substituted benzotriazoles also include compounds fused with one or more aryl (e.g., phenyl) or heteroaryl groups.

[0260] The content of the corrosion inhibitor in the aqueous solution to be purified is preferably adjusted to 0.01 to 5 mass% based on the total mass of the solution. The corrosion inhibitor may be used alone or in combination of two or more. When two or more types of corrosion inhibitors are used in combination, the total content is preferably within the above range.

[0261] Organic solvents The aqueous liquid to be purified may contain an organic solvent. The organic solvent is not particularly limited, but is as already explained as the organic solvent contained in the organic solvent-based liquid to be purified. When the aqueous liquid to be purified contains an organic solvent, the content of the organic solvent is preferably 5 to 35% by mass relative to the total mass of the solvent contained in the aqueous liquid to be purified.

[0262] <Filtration process> The method for producing a chemical solution according to this embodiment includes a filtration step of filtering the liquid to be purified using a filter of the present invention (typically, a filtration device equipped with a filter of the present invention) to obtain a chemical solution. In the above filtration device, the supply pressure of the purified liquid to each filter is not particularly limited, but generally, it is preferably 0.00010 to 1.0 MPa. Among these, in terms of obtaining a chemical solution having superior defect suppression properties, the supply pressure P2 is preferably 0.00050 to 0.090 MPa, more preferably 0.0010 to 0.050 MPa, and further preferably 0.0050 to 0.040 MPa. In addition, since the filtration pressure affects the filtration accuracy, it is preferable that the pressure pulsation during filtration is as small as possible.

[0263] The filtration rate is not particularly limited, but is preferably 1.0 L / min / m because it is easy to obtain a chemical solution having superior defect suppression properties. 2 More than 0.75 L / min / m is preferable. 2 More preferably, 0.6 L / min / m 2 The above is more preferable. Filters have a pressure tolerance that ensures filter performance (the filter will not break), and if this value is large, the filtration pressure can be increased to increase the filtration speed. In other words, the upper limit of the filtration speed usually depends on the pressure tolerance of the filter, but is usually 10.0 L / min / m 2 The following is preferred:

[0264] The temperature at which the liquid to be purified is passed through the filter is not particularly limited, but is generally preferably below room temperature.

[0265] The filtration step is preferably carried out in a clean environment. Specifically, the filtration step is preferably carried out in a clean room that satisfies Class 1000 (Class 6 in ISO14644-1:2015) of the US Federal Standards (Fed.Std.209E), more preferably a clean room that satisfies Class 100 (Class 5 in ISO14644-1:2015), even more preferably a clean room that satisfies Class 10 (Class 4 in ISO14644-1:2015), and particularly preferably a clean room that has a cleanliness of Class 1 (Class 3 in ISO14644-1:2015) or higher (Class 2 or Class 1). Each step described below is also preferably carried out in the above-mentioned clean environment.

[0266] In addition, when the filtration device includes a return flow passage, the filtration step may be a circulation filtration step in which the purified liquid is filtered at least through filter A, and the purified liquid after filtration through filter A is returned to the flow passage upstream of filter A and filtered again through filter A. The number of times of circulating filtration is not particularly limited, but is generally preferably 2 to 10 times. In the circulating filtration, the purified liquid may be returned upstream of filter A so as to repeatedly filter through filter A. In this case, the return flow passage may be adjusted so that filtration through a filter other than filter A is also repeated in addition to filter A.

[0267] <Other processes> The method for producing the chemical solution according to the present embodiment may include other steps than those described above. Examples of the other steps include an apparatus cleaning step and a static electricity removal step. Each step will be described in detail below.

[0268] (Equipment cleaning process) The device washing step is a step of washing the liquid-contacting parts of the filtration device before the filtration step. There is no particular limitation on the method of washing the liquid-contacting parts of the filtration device before the filtration step, but the following will be described using as an example a filtration device in which a filter is contained in a filter cartridge, and the filter cartridge is housed in a housing arranged on a flow path.

[0269] The device cleaning step preferably includes a step A of cleaning the liquid-contacting parts of the filtration device with a cleaning liquid with the filter cartridge removed from the housing, and a step B of storing the filter cartridge in the housing after step A, and further cleaning the liquid-contacting parts of the filtration device with a cleaning liquid.

[0270] ·Process A Step A is a step of cleaning the liquid-contacting parts of the filtration device with a cleaning liquid in a state where the filter cartridge is removed from the housing. "In a state where the filter is removed from the housing" means cleaning the liquid-contacting parts of the filtration device with a cleaning liquid before removing the filter cartridge from the housing or before storing the filter cartridge in the housing. There is no particular limitation on the method for cleaning the liquid-contacting part of the filtration device with the cleaning liquid when the filter has been removed from the housing (hereinafter also referred to as "without the filter"), except for a method in which the cleaning liquid is introduced from the inlet and collected from the outlet.

[0271] Among them, a method of cleaning the liquid-contacting part of a filtration device not housing a filter using a cleaning liquid, which can provide a more excellent effect of the present invention, is to fill the inside of the filtration device not housing a filter with the cleaning liquid. The inside of the filtration device not housing a filter is filled with the cleaning liquid, and the liquid-contacting part of the filtration device not housing a filter comes into contact with the cleaning liquid. As a result, impurities adhering to the liquid-contacting part of the filtration device are transferred (typically eluted) into the cleaning liquid. Then, the cleaning liquid after cleaning can be discharged outside the filtration device (typically from the outlet).

[0272] Cleaning solution The cleaning liquid is not particularly limited, and any known cleaning liquid can be used. In particular, 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 more excellent effects of the present invention can be obtained. In this specification, the main component means a component contained in the cleaning liquid at 99.9 mass% or more, and more preferably contains 99.99 mass% or more, based on the total mass of the cleaning liquid.

[0273] The organic solvent is not particularly limited, and for example, water and organic solvents already described as organic solvents contained in the chemical solution can be used. As the organic solvent, at least one selected from the group consisting of PGMEA, cyclohexanone, ethyl lactate, butyl acetate, MIBC (4-methyl-2-pentanol), MMP (3-methylmethoxypropionate), MAK (2-heptanone), n-pentyl acetate, ethylene glycol, isopentyl acetate, PGME (propylene glycol monoethyl ether), MEK (methyl ethyl ketone), 1-hexanol, and decane is preferable, since it provides a more excellent effect of the present invention.

[0274] ·Process B Step B is a method of cleaning the filtration device with a cleaning liquid while the filter is stored in the housing. As a method for cleaning the filtration device using a cleaning liquid, in addition to the cleaning method in step A already described, a method of passing a cleaning liquid through the filtration device can also be used. There is no particular limitation on the method for passing a cleaning liquid through the filtration device, but it is sufficient to introduce the cleaning liquid from the inlet and discharge it from the outlet. There is no particular limitation on the cleaning liquid that can be used in this step, and the cleaning liquid described in step A can be used.

[0275] (static elimination process) The charge removal step is a step of removing charge from the liquid to be purified to reduce the charged potential of the liquid to be purified. The charge removal method is not particularly limited, and any known charge removal method can be used. For example, the charge removal method includes a method of contacting the liquid to be purified 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 even more preferably 0.01 to 0.1 seconds. Examples of the conductive material include stainless steel, gold, platinum, diamond, and glassy carbon. One method for bringing the liquid to be purified into contact with a conductive material is, for example, to place a grounded mesh made of a conductive material across the flow path and allow the liquid to be purified to flow through it.

[0276] [Corrosion-resistant material] Next, the corrosion-resistant material will be described. In the filtering device and the purification device according to the embodiments of the present invention described above, at least a part of the liquid contacting part is preferably made of a corrosion-resistant material, more preferably 90% or more of the liquid contacting part is made of a corrosion-resistant material, and further preferably 99% or more of the liquid contacting part is made of a corrosion-resistant material.

[0277] There are no particular limitations on the state in which the liquid-contacting parts are formed from a corrosion-resistant material, but typical examples include a state in which each component (e.g., the tanks described above) is formed from a corrosion-resistant material, and a state in which each component contains a base material and a coating layer disposed on the base material, and the coating layer is formed from a corrosion-resistant material.

[0278] The corrosion-resistant material is a non-metallic material and an electrolytically polished metallic material. The non-metallic material is not particularly limited, but may be, for example, a polyethylene resin, a polypropylene resin, a polyethylene-polypropylene resin, a tetrafluoroethylene resin, a tetrafluoroethylene-perfluoroalkylvinyl ether copolymer, a tetrafluoroethylene-hexafluoropropylene copolymer resin, a tetrafluoroethylene-ethylene copolymer resin, a trifluorochloroethylene-ethylene copolymer resin, a vinylidene fluoride resin, a trifluorochloroethylene copolymer resin, and a vinyl fluoride resin.

[0279] The above-mentioned metal material is not particularly limited, but may be, for example, a metal material in which the total content of Cr and Ni is more than 25 mass% based on the total mass of the metal material, and more preferably 30 mass% or more. The upper limit of the total content of Cr and Ni in the metal material is not particularly limited, but is generally preferably 90 mass% or less. Examples of the metal material include stainless steel and Ni-Cr alloy.

[0280] The stainless steel is not particularly limited, and known stainless steels can be used. Among them, an alloy containing 8% or more of Ni by mass is preferable, and an austenitic stainless steel containing 8% or more of Ni by mass is more preferable. Examples of austenitic stainless steel include SUS (Steel Use Stainless) 304 (Ni content 8% by mass, Cr content 18% by mass), SUS304L (Ni content 9% by mass, Cr content 18% by mass), SUS316 (Ni content 10% by mass, Cr content 16% by mass), and SUS316L (Ni content 12% by mass, Cr content 16% by mass).

[0281] The Ni-Cr alloy is not particularly limited, and any known Ni-Cr alloy can be used. Among them, a NiCr alloy having a Ni content of 40 to 75 mass % and a Cr content of 1 to 30 mass % is preferable. Examples of Ni-Cr alloys include Hastelloy (trade name, the same applies below), Monel (trade name, the same applies below), and Inconel (trade name, the same applies below), etc. More specifically, examples include 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. Furthermore, the Ni-Cr alloy may further contain B, Si, W, Mo, Cu, Co, and the like in addition to the above-mentioned alloy, if necessary.

[0282] The method for electrolytically polishing the metal material is not particularly limited, and any known method can be used, such as those described in paragraphs 0011 to 0014 of JP 2015-227501 A and paragraphs 0036 to 0042 of JP 2008-264929 A.

[0283] It is presumed that the Cr content in the surface passive layer of a metallic material is higher than the Cr content in the parent phase due to electrolytic polishing, and therefore, it is presumed that the use of a refining device with a liquid-contacting part formed from an electrolytically polished metallic material makes it difficult for metal impurities containing metal atoms to flow out into the purified liquid. The metal material may be buffed. The method of buffing is not particularly limited, and known methods can be used. The size of the polishing grains used for the buffing is not particularly limited, but #400 or less is preferable because it tends to reduce the unevenness of the surface of the metal material. The buffing is preferably performed before the electrolytic polishing.

[0284] [Chemical Uses] The chemical solution produced using the filter of the present invention (preferably a filtration device containing the filter) is preferably used for manufacturing semiconductor substrates, and more preferably for forming fine patterns with a node of 10 nm or less (for example, a process including pattern formation using extreme ultraviolet light). In other words, the filtration apparatus is preferably used for producing chemical solutions for use in manufacturing semiconductor substrates, and more specifically, for producing chemical solutions used to treat inorganic and / or organic substances after completion of each step or before moving to the next step in the manufacturing process for semiconductor devices, which includes a lithography step, an etching step, an ion implantation step, and a peeling step, etc. Specifically, the above-mentioned filtration device is preferably used for producing at least one kind (chemical liquid obtained by purifying an organic liquid to be purified) selected from the group consisting of a developing solution, a rinsing solution, a wafer cleaning solution, a line cleaning solution (e.g., a piping cleaning solution), a pre-wet solution, a wafer rinsing solution, a resist solution, a solution for forming an underlayer film, a solution for forming an upper layer film, and a solution for forming a hard coat. In another embodiment, the filtration device is preferably used for producing at least one kind (chemical liquid obtained by purifying an aqueous liquid to be purified) selected from the group consisting of a water-based aqueous developing solution, a water-based rinsing solution, a stripping solution, a remover, an etching solution, an acidic cleaning solution, phosphoric acid, and a phosphoric acid-hydrogen peroxide mixture (SPM: Sulfuric acid-Hydrogen Peroxide Mixture).

[0285] The filter of the present invention (preferably a filtering device containing the filter) can also be used to produce a chemical solution used for rinsing the edge line of a semiconductor substrate before or after resist coating. The filter of the present invention (preferably a filtering device containing a filter) can also be used in producing a dilution liquid for a resin contained in a resist liquid, and a solvent contained in a resist liquid.

[0286] Furthermore, the filter of the present invention (preferably a filtration device containing the filter) can be used for producing chemical solutions used for purposes other than the production of semiconductor substrates, and can also be used for producing developers for polyimide, sensor resists, lens resists, etc., and rinse solutions, etc. The filter of the present invention (preferably a filtration device containing the filter) can also be used to produce solvents for medical or cleaning applications, particularly for the production of chemical solutions for cleaning containers, piping, and substrates (e.g., wafers, glass, etc.). In particular, the filter of the present invention (preferably a filtration device containing a filter) is preferably used in the production of at least one liquid selected from the group consisting of a pre-wet liquid, a developer, a rinsing liquid, and a pipe cleaning liquid for cleaning an apparatus that transports these liquids in pattern formation.

[0287] When the produced chemical solution contains an organic solvent as a main component (for example, when the content of the organic solvent is 80 mass% or more (preferably 99 mass% or more, more preferably 99.9 mass% or more; the upper limit is, for example, 100 mass% or less) relative to the total mass of the chemical solution), the chemical solution has a Hansen solubility parameter distance for eicosene of 3 to 20 MPa. 0.5 (More preferably 5 to 20 MPa 0.5 ) is preferably included. When two or more organic solvents are used, it is preferable that at least one of them satisfies the above-mentioned range of Hansen solubility parameters. When two or more organic solvents are used, it is preferable that the weighted average value of the Hansen solubility parameters based on the molar ratio of the contents of the respective organic solvents satisfies the above-mentioned range of the Hansen solubility parameters. As the organic solvent, for example, the same organic solvents as those exemplified as the organic solvent for the liquid to be purified can be used.

[0288] For example, from the viewpoint of more excellent defect suppression, it is also preferable that the chemical solution is substantially only an organic solvent satisfying the above-mentioned Hansen solubility parameter range. The chemical solution is substantially only an organic solvent satisfying the above-mentioned Hansen solubility parameter range means that the content of the organic solvent satisfying the above-mentioned Hansen solubility parameter range is 99 mass% or more (preferably 99.9 mass% or more) based on the total mass of the organic solvent.

[0289] Also, for example, it is preferable that the chemical solution is a mixed solvent containing both an organic solvent that satisfies the above-mentioned range of Hansen solubility parameters and an organic solvent that does not satisfy the above-mentioned range of Hansen solubility parameters. In this case, in order to obtain a chemical solution having better defect suppression properties, it is preferable that the chemical solution (mixed solvent) contains 20 to 80 mass % (preferably 30 to 70 mass %) of an organic solvent satisfying the above-mentioned Hansen solubility parameter range relative to the total mass of the chemical solution, and contains 20 to 80 mass % (preferably 30 to 70 mass %) of an organic solvent not satisfying the above-mentioned Hansen solubility parameter range relative to the total mass of the chemical solution. When the content of the organic solvent satisfying the above-mentioned Hansen solubility parameter range and the content of the organic solvent not satisfying the above-mentioned Hansen solubility parameter range are each at a certain level or more, the affinity of the chemical solution for the metal-based material and the organic-based material can be adjusted to a suitable range, compared with the case where the organic solvent not satisfying the above-mentioned Hansen solubility parameter range is an amount outside a predetermined range (e.g., 1% by mass or more but less than 20% by mass or more or more than 80% by mass based on the total mass of the mixed solvent), and it is considered that the effect of the present invention is more excellent. In this case, the total content of the organic solvent satisfying the above-mentioned range of Hansen solubility parameters and the organic solvent not satisfying the above-mentioned range of Hansen solubility parameters is preferably 99.0 mass% or more based on the total mass of the drug solution. Although there is no particular upper limit, it is generally preferably 99.99999 mass% or less. In addition, the distance of the Hansen solubility parameter for eicosene in organic solvents that do not satisfy the above Hansen solubility parameter range is 0 MPa. 0.5 More than 3MPa 0.5 Less than (preferably 0 MPa 0.5 Super 3MPa 0.5 less than 20MPa 0.5 More than (preferably 20MPa 0.5 Super 50MPa 0.5 (see below).

[0290] [Drug solution container] The liquid medicine produced by the above-mentioned filtration device may be stored in a container until it is used. Such a container and the liquid medicine stored in the container are collectively referred to as a liquid medicine container. The liquid medicine is taken out from the stored liquid medicine container and used.

[0291] The container for storing the above-mentioned chemical solution is preferably a container for manufacturing semiconductor substrates, which has a high degree of cleanliness within the container and is unlikely to leach impurities into the chemical solution during storage. Usable containers are not particularly limited, and examples thereof include the "Clean Bottle" series manufactured by Aicello Chemical Co., Ltd. and the "Pure Bottle" manufactured by Kodama Resin Industry Co., Ltd., but are not limited to these.

[0292] As the container, it is also preferable to use a multi-layer bottle whose inner wall has a six-layer structure made of six types of resin, or a multi-layer bottle whose inner wall has a seven-layer structure made of six types of resin, in order to prevent impurities from being mixed in (contaminated) with the drug solution. Examples of such containers include the containers described in JP 2015-123351 A.

[0293] At least a part of the liquid-contacting portion of the container is preferably made of the corrosion-resistant material already described. In order to obtain a more excellent effect of the present invention, it is preferable that 90% or more of the area of ​​the liquid-contacting portion is made of the above material. EXAMPLES

[0294] The present invention will be described in more detail below based on examples. The materials, amounts, ratios, processing contents, processing procedures, etc. shown in the following examples can be appropriately changed without departing from the spirit of the present invention. Therefore, the scope of the present invention should not be interpreted as being limited by the following examples.

[0295] In addition, in preparing the chemical solutions in the Examples and Comparative Examples, handling of containers, preparation, filling, storage, and analysis and measurement were all performed in clean rooms that met ISO class 2 or 1. In order to improve measurement accuracy, when measuring the content of organic compounds and the content of metal components, when components below the detection limit in normal measurements were measured, the chemical solutions were concentrated before measurement, and the content was calculated by converting it into the concentration of the solution before concentration. Unless otherwise specified, the equipment used in the tests had been thoroughly cleaned beforehand.

[0296] [Filter Creation] [Filter packaging material] The treated filters were obtained packaged in the packaging materials shown below. The abbreviations for the packaging materials for the treated filters are as follows:

[0297] HDPE: The part that comes into contact with the filter to be treated is made of HDPE (high density polyethylene) Fluorine resin: A fluororesin bag in which the part that comes into contact with the filter to be treated is made of fluororesin EP-SUS: A capsule made of stainless steel, the part that comes into contact with the filter to be treated being electropolished stainless steel.

[0298] [Filter to be processed] A filter containing a filter body including a filtration layer and a support layer containing the materials shown below was subjected to pretreatment as a filter to be treated. The abbreviations for the materials of the filter body of each filter (filter to be treated) are as follows:

[0299] PP: Polypropylene IEX(PTFE): PTFE with cation exchange groups ·PTFE: Polytetrafluoroethylene Nylon: ·UPE: Ultra-high molecular weight polyethylene PFA: Perfluoroalkoxyalkane Polyester: Grafted Nylon: Nylon grafted with a nylon-based polymer

[0300] A1: First, a pre-crosslinker of the formula CH2CH-CF 12 TFE and vinyl ether of formula CF2=CF-O-CF2CF2-SO2F were emulsion polymerized using a bis-olefin of -CHCH2, I-C4F8-I as a chain transfer agent, and potassium persulfate as a radical initiator. The emulsion polymerization conditions were in accordance with those in Table 2 of paragraph 0121 of JP2012-522882A, and copolymer C1 in Table 2 above was synthesized. Next, the fluorocarbon composition S1 described in paragraphs 0123 to 0125 (particularly Table 3 in paragraph 0123) of JP2012-522882A was prepared. Next, the fluorocarbon composition was adjusted so that the content of the ionomer was 1.3 mass%. The prepared fluorocarbon composition contained a crosslinking agent and a radical initiator. A film was formed by forming a coating layer on the surface of a PTFE porous substrate using the prepared fluorocarbon composition.

[0301] A2: Referring to the description in paragraph 0058 of JP 2015-61727 A, hollow fibers of a tetrafluoroethylene-perfluoro(alkyl vinyl ether) copolymer were prepared, and a membrane was produced using the fibers.

[0302] A3: A membrane comprising: a first layer containing a porous substrate made of polytetrafluoroethylene and sulfonic acid groups bonded to the surface of the porous substrate; and a second layer disposed on the first layer, the second layer containing a porous substrate made of polytetrafluoroethylene and amide groups bonded to the surface of the porous substrate.

[0303] Anion exchange group: A grafted ultra-high molecular weight polyethylene membrane (containing a quaternary ammonium group as an anion exchange group) as described in paragraph 0099 of JP2017-536232A. This membrane is an asymmetric porous membrane.

[0304] Cation exchange group: Ultra-high molecular weight polyethylene membrane grafted with reference to the description in paragraphs 0130 to 0132 of JP2017-536232A (containing sulfonic acid groups as cation exchange groups). This membrane is an asymmetric porous membrane.

[0305] Neutral grafted UPE1: A grafted ultra-high molecular weight polyethylene membrane (containing a hydroxy group derived from hydroxymethylacrylamide as a neutral group) as described in paragraphs 0058 to 0059 of JP2017-536232A. This membrane is an asymmetric porous membrane.

[0306] Neutral grafted UPE2: An ultra-high molecular weight polyethylene membrane (containing a hydroxy group derived from hydroxymethylacrylamide as a neutral group) prepared in the same manner as above, except that in paragraphs 0058 to 0059 of JP2017-536232A, vinylbenzyltrimethylammonium chloride monomer was not used. This membrane is an asymmetric porous membrane.

[0307] PFSA / PTFE: Commercially available Fluoroguard AT manufactured by Entegris, Inc. was immersed in a polymer solution prepared by dissolving 0.25% PFSA solution (Aquivion PFSA 24: D83-24B Solvay Plastics) in methanol-water solvent until it was sufficiently wet, then drained, dried, and washed with ultrapure water for 24 hours.

[0308] ·PTFE-a1: A membrane in which a coating layer of poly(M8-b-NPF6) is formed on the surface of a PTFE porous membrane, with reference to the description in paragraphs 0124 and 0125 of JP 2016-194038 A. The pore size was adjusted by the amount of poly(M8-b-NPF6) coated. The resin forming the coating layer of PTFE-1 contains a polyoxyalkylene group as a hydrophilic group.

[0309] PTFE-a2: Poly(M8-b-NPF6)-S(CH2)SO3Na described in paragraph 0023 of JP 2016-194038 A was synthesized. Specifically, the above copolymer was synthesized with reference to the description in paragraphs 0103 to 0109 of JP 2016-194038 A. A porous PTFE membrane containing a coating layer was produced using the synthesized copolymer in the same manner as PTFEa-1. The resin forming the coating layer of PTFE-2 contains a polyoxyalkylene group and a sulfonic acid (salt) group as hydrophilic groups.

[0310] ·PTFE-a3: Poly(M8-b-NPF6)-S-CH2COOH described in paragraph 0023 of JP 2016-194038 A was synthesized. Specifically, the above copolymer was synthesized with reference to the description in paragraphs 0103 to 0109 of JP 2016-194038 A. A porous PTFE membrane containing a coating layer was produced using the synthesized copolymer in the same manner as PTFE-a1. The resin forming the coating layer of PTFE-a3 contains a polyoxyalkylene group and a carboxylic acid (salt) group as a hydrophilic group.

[0311] ·PTFE-a4: Poly(NTEG-b-NPF6) / thioglycerol was synthesized as described in paragraph 0014 of JP 2016-199733 A. Specifically, the copolymer was synthesized with reference to the description in paragraphs 0106-0108 of JP 2016-199733 A. A porous PTFE membrane containing a coating layer was produced using the synthesized copolymer in the same manner as PTFE-a1. The resin forming the coating layer of PTFE-a4 contains a polyoxyalkylene group as a hydrophilic group, and a group containing a thioether group and a hydroxyl group.

[0312] PTFE-b1: Grubbs' second generation catalyst (3.0 mg, 0.004 mmol), 2-butene-1,4-diol (10.0 mg, 0.12 mmol), and 1,5-cyclooctadiene (490 mg, 4.54 mmol) were combined in a 50 mL round bottom flask equipped with a stir bar, degassed with argon for 5 min, and transferred to a 40° C. oil bath. Heating was continued for 1 h, and the remaining 1,5-cyclooctadiene (4.5 mg, 4.2 mmol) in 5 mL of DCM was added to the mixture and heating was continued for an additional 6 h. The hydroxyl-terminated polymer (PCOD) was isolated by precipitation in methanol. 1 H-NMR (300MHz, CDCl3): δ (ppm) 5.3~5.5 (s, wide, 1H), 1.75~2.5 (s, wide).

[0313] The above PCOD homopolymer was post-functionalized with 1H,1H,2H,2H-perfluorodecanethiol in the presence of a photoinitiator under UV irradiation to obtain fluorinated PCOD. The porous PTFE membrane is coated with fluorinated PCOD, modified via a thiol-ene reaction, by immersing the membrane in a solution containing fluorinated PCOD (1-10% mass concentration) in THF, photoinitiator (Irgacure, 1-15% mass), 3-mercaptoethanesulfonic acid sodium salt (1-15% mass, neutralized with an aqueous solution of THF and dilute hydrochloric acid (1N) until a homogeneous THF solution is obtained), and the membrane is crosslinked with this mixture using UV irradiation (300-480 nm, 150-250 mW, 60 s-180 s). The membrane is then washed with water and dried at 100 °C for 10 min to obtain the membrane.

[0314] PTFE-b1 obtained by the above method contained a coating layer of a copolymer having PCOD as a main chain and containing a thioether group (-SCH2CH2(CF2)7CF3) as an adsorptive group, which was arranged on a porous PTFE substrate so as to cover the porous substrate.

[0315] PTFE-b2: A coating resin having a carboxylic acid group introduced into a side chain was obtained by a thiol-ene reaction between mercaptoacetic acid and an allyl group, with reference to the description in paragraphs 0018 to 0032 of JP 2017-002273 A. Furthermore, a coating layer of the above resin was formed on a PTFE porous membrane with reference to the description in paragraphs 0070 to 0071 of JP 2017-002273 A to obtain a membrane.

[0316] PTFE-b2 obtained by the above method contained a coating layer of a copolymer of formula (I) that contained a thioether group and a group containing a carboxylic acid group (-SCH2COOH) as an adsorptive group, disposed on a porous PTFE substrate so as to cover the porous substrate.

[0317] [ka]

[0318] The copolymer of formula (I) is a random copolymer or a block copolymer, Rf is a perfluoro substituent, Rh is an adsorptive group, Ra is a methyl group or an ethyl group, m and n are independently 10 to 1000, X is an alkyl group, and Y is a reactive functional group.

[0319] ·PTFE-b3: Referring to the description in paragraphs 0018 to 0032 of JP 2017-002273 A, an aminoethyl group was introduced by a thiol-ene reaction between mercaptoethyldiethylamine and an allyl group, and then a quaternary ammonium group was introduced to the side chain by a quaternary reaction with ethyl bromide to obtain a coating resin. Furthermore, referring to the description in paragraphs 0070 to 0071 of JP 2017-002273 A, a coating layer was formed from the above resin on a PTFE porous membrane to obtain a membrane.

[0320] PTFE-b3 obtained by the above method contained a coating layer of a copolymer of formula (I) that contained a thioether group and a group containing a quaternary ammonium group as an adsorptive group, and was disposed on a porous PTFE substrate so as to cover the porous substrate.

[0321] PTFE-b4: A coating resin having a thioether group introduced therein was obtained by a thiol-ene reaction between 2-ethylhexylthiopropyl mercaptan and an allyl group, with reference to the description in paragraphs 0018 to 0032 of JP 2017-002273 A. A coating layer of the resin was formed on a PTFE porous membrane, with reference to the description in paragraphs 0070 to 0071 of JP 2017-002273 A, to obtain a membrane.

[0322] PTFE-b4 obtained by the above method contained a coating layer of a copolymer of formula (I) containing a group containing a thioether group as an adsorptive group, which was disposed on a porous PTFE substrate so as to cover the porous substrate.

[0323] ·PTFE-b5: A coating resin having a phosphoricoxy group introduced therein was obtained by a thiol-ene reaction between tripropyloxyphosphoricoxypropyl mercaptan and an allyl group, with reference to the description in paragraphs 0018 to 0032 of JP 2017-002273 A. A coating layer of the resin was formed on a PTFE porous membrane, with reference to the description in paragraphs 0070 to 0071 of JP 2017-002273 A, to obtain a membrane.

[0324] PTFE-b5 obtained by the above method contained a coating layer of a copolymer of formula (I) that was disposed on a porous PTFE substrate so as to cover the porous substrate and contained a thioether group and a group containing a phosphate group as an adsorptive group.

[0325] ·PTFE-b6: A PTFE porous membrane coated with PFDT-PG-AGE having perfluorodecanethiol bonded thereto, with reference to the description in paragraphs 0068 to 0082 of JP 2016-29146 A.

[0326] PTFE-b6 obtained by the above method contained a coating layer of a fluorinated polymer containing the structure of "PFDT-PG-AGE" and a copolymer containing a group containing a thioether group as an adsorptive group, which was arranged on a porous PTFE substrate so as to cover the porous substrate.

[0327] PTFE-b7: A PTFE porous membrane coated with poly(SZNB-b-NPF6)-2, with reference to the description in paragraphs 0085 to 0088 of JP 2016-194040 A. The PTFE-7 obtained by the above method was a fluorinated polymer containing the structure of "poly(SZNB-b-NPF6)-2" arranged on a porous PTFE substrate so as to cover the porous substrate, and contained a coating layer made of a copolymer containing a sulfonic acid group as an adsorptive group and a group containing a quaternary ammonium group.

[0328] ·PTFE-b8 Poly(C2 diacid-r-NPF6) was synthesized with reference to the description in paragraphs 0110 to 0112 of JP 2016-196625 A, and a coating layer was formed on a PTFE porous membrane with reference to the description in paragraph 0109 of the same publication, to obtain a membrane.

[0329] The PTFE-b8 obtained by the above method contained a "poly(C2 diacid-r-NPF6)" structure arranged on a PTFE porous substrate so as to cover the porous substrate, and contained a coating layer made of a copolymer containing a carboxylic acid group and an oxyalkylene group as an adsorptive group.

[0330] ·PTFE-b9: Poly(C4-r-NPF6-r-NHS) was synthesized with reference to the description in paragraphs 0120 to 0124 of JP 2016-196625 A, and a coating layer was formed on a PTFE porous membrane with reference to the description in paragraph 0109 of the same publication, to obtain a membrane. 1H-NMR (300 MHz, CDCl3): δ (ppm) 6 (s broad), 5.9-5.0 (m broad), 5.1-4.6 (m broad), 4.6-4.1 (m broad), 4.0-3.0 (m broad), 3.0-2.4 (m broad), 2.3-1.4 (m broad), 1.25 (s broad).

[0331] The PTFE-9 obtained by the above method contained a “poly(C4-r-NPF6-r-NHS)” structure arranged on a PTFE porous substrate so as to cover the porous substrate, and contained a coating layer made of a copolymer containing a thioether group and a group containing a diester group as an adsorptive group.

[0332] Filter Y1: A porous film containing a polyimide resin produced with reference to the description in paragraphs 0223 and 0234 to 0239 of JP 2017-68262 A. The pore size was controlled by adjusting the particle size of the fine particles used, and the imidization rate was controlled by adjusting the baking temperature and / or re-baking temperature. The imidization rate was set to 1.85. The pore size is shown in the table below.

[0333] Filters Y2~Y6: A membrane prepared in the same manner as for filter Y1, except that the particle size of the microparticles used, and the baking temperature and / or re-baking temperature, etc. were adjusted so that the pore size and imidization rate would be the desired values. The imidization rates are 1.82, 1.60, 1.93, 1.68, and 0.88, starting from filter Y2. The pore sizes are shown in the table below.

[0334] R: A porous film containing a polyimide resin, produced with reference to the description in paragraphs 0019 to 0027 of JP2016-538122A. The imidization ratio was 1.45. The porous film had a structure in which the imidization ratio differed in the thickness direction, but the imidization ratio was calculated as the average value for the entire porous film.

[0335] S: A porous film containing a polyimide resin produced with reference to the description in paragraphs 202 to 203 of JP 2018-20301 A. The produced porous membrane is the membrane described in Example 1 of JP 2018-20301 A. The B value and imidization rate were 8 nm and 1.43, respectively.

[0336] T: A porous film containing a polyimide resin produced with reference to the description in paragraphs 202 to 203 of JP 2018-20301 A. The produced porous membrane is the membrane described in Example 2 of JP 2018-20301 A. The B value and imidization rate were 10 nm and 1.54, respectively.

[0337] [Organic cleaning solution] The organic cleaning solutions used in the pretreatment are shown below. All of the organic cleaning solutions were of high purity grade. ·PGMEA: Propylene glycol monomethyl ether acetate IPA: Isopropanol ·CyHe: Cyclohexane nBA: Butyl acetate

[0338] [Pretreatment] The filter to be treated was pretreated using the cleaning method described below. The filter to be treated was subjected to pretreatment in a state in which it was contained in a filter cartridge with a filter tube length of 1 inch, and was then subjected to the test described below.

[0339] <Immersion treatment> The filter to be treated was immersed in 20 liters of organic cleaning solution. The type of organic cleaning solution, the temperature, and the immersion time are shown in the table below.

[0340] <Ultrasonic treatment> The filter was sonicated while immersed in 20 liters of organic cleaning solution (PGMEA). The sonication lasted for 1 hour. The ultrasonic output is shown in the table below.

[0341] <Liquid passing process> An organic cleaning liquid was passed through a filter unit in which a filter cartridge containing a filter to be treated was housed and installed. The type and amount of organic cleaning liquid passed are shown in the table below.

[0342] When the pretreatment included two or more treatments, the treatments were carried out in the order of immersion treatment, ultrasonic treatment, and liquid passing treatment, and immediately after one treatment was completed, the next treatment was carried out. The filter (filter cartridge) after the pretreatment was placed in a housing to be used in the test of [Production of chemical solution] described later. In addition, when the organic cleaning liquid that had been last contacted was different from the liquid to be purified used in [Production of chemical liquid], 400 kg of the liquid to be purified was passed through before being used in the test in [Production of chemical liquid].

[0343] 〔analysis〕 After pretreatment, the filters were analyzed. In addition, in order to prevent the content of specific organic compounds in the filters from being affected by the processing for the analysis (e.g., elution processing), two filters were prepared for each filter in addition to the filter used for the production of the chemical solution described below, and these filters were used for the analysis before and after the pretreatment, respectively. Specifically, when producing Filter 1 shown in the table below, a treated filter used for a manufacturing test of a chemical solution after pretreatment was prepared, and two more filters (treated filters) with the same configuration, obtained on the same occasion, and distributed and stored under the same conditions were prepared. One of the two filters was analyzed before pretreatment, and the content, etc. of the specific organic compounds analyzed was determined to be the content, etc. of the specific organic compounds contained in Filter 1 before pretreatment. The other of the two filters was analyzed after the same pretreatment as Filter 1, and the content, etc. of the specific organic compounds analyzed was determined to be the content, etc. of the specific organic compounds contained in Filter 1 obtained by pretreatment of the treated filter.

[0344] <Specific organic compounds> The content of the specific organic compound in each filter was measured by the method described above in the specification. The compounds detected as specific organic compounds are as follows:

[0345] A compound represented by the general formula (I)

[0346] [ka]

[0347] A compound represented by the general formula (II)

[0348] [ka]

[0349] [ka]

[0350] A compound represented by the general formula (III)

[0351] [ka]

[0352] [ka]

[0353] A compound represented by the general formula (IV)

[0354] [ka]

[0355] A compound represented by the general formula (V)

[0356] [ka]

[0357] A compound represented by the general formula (VI)

[0358] [ka]

[0359] [ka]

[0360] [ka]

[0361] A compound represented by the general formula (VII)

[0362] [ka]

[0363] A compound represented by the general formula (VIII)

[0364] [ka]

[0365] A compound represented by the general formula (X) When applied to general formula (X), compounds in which j is 12 to 50 were detected.

[0366] A compound represented by the general formula (XI) When applied to general formula (XI), compounds with k of 12 to 50 were detected.

[0367] A compound represented by the general formula (XII) Squalene was detected.

[0368] <Specific metal components> The contents of specific metal components (specific metal ions and specific metal particles) in each filter were measured using an Agillent 8900 by the method described above in the specification.

[0369] Table 1 below shows the pretreatment conditions and the contents of specific organic compounds and specific metal components in the filter after treatment.

[0370] [Table 1]

[0371] [Table 2]

[0372] [Table 3]

[0373] [Table 4]

[0374] [Table 5]

[0375] [Table 6]

[0376] [Table 7]

[0377] [Table 8]

[0378] [Table 9]

[0379] [Table 10]

[0380] [Table 11]

[0381] [Table 12]

[0382] [Table 13]

[0383] [Table 14]

[0384] [Table 15]

[0385] [Production of drug solutions] Four filters that had undergone pretreatment were selected and designated as the first to fourth filters. A filtration device was fabricated in which the first to fourth filters were arranged in series between the inflow section and the outflow section in this order. Each filter was contained in a filter cartridge and housed in a housing to form a filter unit. The liquid to be purified was purified using the above-mentioned filtration device. The names of the chemicals mentioned below correspond to the numbers of each example. For example, the chemical produced and tested in Example A001 described later is referred to as Chemical A001.

[0386] [Liquid to be purified] The liquids used for purification are shown below. All of the liquids used for purification are of high purity grade. The values ​​in parentheses indicate the distance (MPa) between the Hansen solubility parameters of each liquid (organic solvent) and eicosene. 0.5 ). PGMEA: Propylene glycol monomethyl ether acetate (9.5) PGME: Propylene glycol monoethyl ether (11.0) PGMEA / PGME (v / v=7 / 3): A mixture of PGMEA and PGME in a ratio of 7:3 (by volume) (10.2) · PGMP: Propylene glycol monopropyl ether (10.6) MPM: Methyl methoxypropionate (8.8) CHN: Cyclohexanone (5.1) nBA: Butyl acetate (4.6) ·γBL: γ-butyrolactone (8.5) ·MIBC: 4-Methyl-2-pentanol (12.1) · iAA: Isoamyl acetate (6.0) Butyl butyrate (4.6) Isobutyl isobutyrate (3.6) Isoamyl ether (2.1) Undecane (1.8) Dimethyl malonate / isoamyl ether = 9 / 1 (a mixture of dimethyl malonate and isoamyl ether at a ratio of 9:1 (by mass)) (9.4) Dimethyl malonate / isoamyl ether = 5 / 5 (a 5:5 mixture of dimethyl malonate and isoamyl ether by mass) (5.9) Dimethyl malonate / isoamyl ether = 1 / 9 (a 1:9 mixture of dimethyl malonate and isoamyl ether (by mass)) (2.7) In addition, the Hansen solubility parameter distance for eicosene when dimethyl malonate is used alone is 10.3MPa. 0.5 It is.

[0387] [test] [Pre-wet liquid, rinsing liquid] The prepared chemical solutions were evaluated for their defect suppression properties when used as a pre-wet solution and a rinsing solution by the method described below. First, the chemicals were spin-discharged onto a silicon substrate with a diameter of 300 mm, and while the substrate was rotating, 0.5 cc of each chemical was discharged onto the surface of the substrate. The substrate was then spin-dried. Next, the number of defects present on the substrate after the chemicals were applied was counted using a wafer inspection device "SP-5" manufactured by KLA-Tencor. Next, using EDAX (energy-dispersive X-ray spectroscopy), the particulate foreign matter on the wafer was classified into "metal residue defects" mainly composed of metal and "particulate organic residue defects" mainly composed of organic matter, and then measured. Furthermore, non-particulate stain-like defects were counted as "stain-like defects." In addition, if the evaluation of metal residue defects, particulate organic residue defects, and stain-like residue defects is a grade of C or higher, the liquid can be suitably used as a pre-wet liquid and a rinse liquid.

[0388] <Metal residue defects, particulate organic residue defects, stain-like residue defects> A: The corresponding number of defects was 20 or less per wafer. B: The corresponding defect count was greater than 20 / wafer and less than or equal to 50 / wafer. C: The corresponding number of defects was greater than 50 / wafer and less than 100 / wafer. D: The corresponding number of defects exceeds 100 / wafer.

[0389] [Pipe cleaning fluid] The produced chemical solution was evaluated for its defect suppression performance when used as a pipe cleaning solution by the method described below. Immediately after purchase, piping (liquid contact part: made of PTFE, φ: 50 mm, length: 5 m) was cleaned by passing 5000 ml of the chemical solution to be evaluated through it at 500 ml / min. Next, the chemical liquid A021 (chemical liquid obtained by the purification process of Example A021) was discharged onto the wafer through this pipe, and the same test was performed as for the evaluation of the performance as a pre-wet liquid or a rinse liquid described above, and the evaluation was performed with the same criteria. If the chemical liquid A021 that passed through the pipe after cleaning can be suitably used as a pre-wet liquid or a rinse liquid, it can be determined that the occurrence of defects can be suppressed when such a pipe cleaning liquid is applied to the resist process to clean the equipment.

[0390] [Developer / Rinse] The prepared chemical solutions were evaluated for their defect suppression properties when used as developing solutions or rinsing solutions by the method described below.

[0391] <Test 1 (ArF exposure)> First, a resist pattern was formed by the following procedure. An organic anti-reflective coating composition ARC29SR (manufactured by Nissan Chemical Industries, Ltd.) was applied to a silicon substrate having a diameter of 300 mm and baked at 205° C. for 60 seconds to form an anti-reflective coating having a thickness of 78 nm. To improve the coatability, a pre-wetting liquid (chemical solution A021 was used) was dropped onto the surface of the silicon wafer on which the anti-reflective coating was formed, and spin coating was performed. Next, an actinic ray-sensitive or radiation-sensitive resin composition (actinic ray-sensitive or radiation-sensitive resin composition 1 described below) was applied onto the antireflective film after the prewetting process, and prebaked (PB) at 100°C for 60 seconds to form a resist film with a thickness of 150 nm.

[0392] (Actinic ray-sensitive or radiation-sensitive resin composition 1) Acid-decomposable resin (resin represented by the following formula (weight average molecular weight (Mw): 7500): the numerical value written for each repeating unit means mol %): 100 parts by mass

[0393] [ka]

[0394] Photoacid generator as shown below: 8 parts by weight

[0395] [ka]

[0396] Quencher shown below: 5 parts by mass (the mass ratio, from left to right, was 0.1:0.3:0.3:0.2). Of the quenchers shown below, the polymer type quencher has a weight average molecular weight (Mw) of 5000. The numerical values ​​shown for each repeating unit indicate the molar ratio.

[0397] [ka]

[0398] Hydrophobic resin shown below: 4 parts by mass (the mass ratio, from left to right, was 0.5:0.5.) Of the hydrophobic resins shown below, the hydrophobic resin on the left has a weight average molecular weight (Mw) of 7000, and the hydrophobic resin on the right has a weight average molecular weight (Mw) of 8000. In each hydrophobic resin, the numerical value given for each repeating unit means the molar ratio.

[0399] [ka]

[0400] solvent: PGMEA (propylene glycol monomethyl ether acetate): 3 parts by mass Cyclohexanone: 600 parts by mass γ-BL (γ-butyrolactone): 100 parts by mass

[0401] The wafer on which the resist film was formed was scanned with an ArF excimer laser scanner (Numerical Aperture: 0.75) at 25 mJ / cm 2The wafer was exposed to light at 100° C. for 60 seconds. The wafer was then developed by puddling in a developer for 30 seconds, and then developed by puddling in a rinse solution for 30 seconds. The wafer was then rotated at 4000 rpm for 30 seconds to form a negative resist pattern. The resulting negative pattern was then heated at 200° C. for 300 seconds. Through the above steps, an L / S pattern with a line / space ratio of 1:1 (average pattern width: 45 nm) was obtained. Evaluations of developability and defect suppression were performed for each pattern. Here, when evaluating the developer, the developer to be evaluated was used as the developer, and chemical solution B049 (chemical solution obtained by the purification treatment of Example B049) was used as the rinsing solution. When evaluating the rinse solution, the developing solution used was chemical solution B018, and the rinse solution to be evaluated was used.

[0402] <Defect suppression> The formed wafer patterns were observed using a pattern defect measurement device (Hitachi High-Technologies Corporation's Multipurpose SEM (Scanning Electron Microscope) "Inspago" RS6000 series) and the number of the following defects was measured. · Poor development defect: A defect in which the space is not formed to the bottom of the pattern Residue defect: A defect where a foreign object exists on the pattern. Uniformity defect: A defect in which the pattern width is 3 nm or more larger than the target (45 nm). In addition, if the evaluation of each of the poor development defect, residue defect, and uniformity defect is C or higher, the liquid can be suitably used as a pre-wet liquid and a rinse liquid.

[0403] <Development defects, residue defects, uniformity defects> A: The corresponding number of defects was 5 or less per wafer. B: The corresponding defect count was greater than 5 / wafer and less than or equal to 10 / wafer. C: The corresponding defect count was greater than 10 / wafer and less than or equal to 30 / wafer. D: The corresponding number of defects exceeds 30 / wafer.

[0404] <Test 2 (EUV exposure)> (Actinic ray-sensitive or radiation-sensitive resin composition (resist composition 1)) First, resist composition 1 was obtained by mixing the components in the following ratio. ·Resin (A-1): 0.77g Photoacid generator (B-1): 0.03g Basic compound (E-3): 0.03g PGMEA (commercially available, high purity grade): 67.5g Ethyl lactate (commercial product, high purity grade): 75g

[0405] ·resin The following resins were used.

[0406] [ka]

[0407] Photoacid generator As the photoacid generator, the following compound was used.

[0408] [ka]

[0409] Basic compounds As the basic compound, the following compounds were used.

[0410] [ka]

[0411] (Pattern formation and evaluation) The chemicals were evaluated for their ability to suppress residue defects, bridge defects, and stain defects by the following methods. 3S " was used. First, AL412 (manufactured by Brewer Science) was applied onto a silicon wafer with a diameter of 300 mm, and baked at 200°C for 60 seconds to form a resist underlayer film with a thickness of 20 nm. A pre-wet liquid (chemical solution A021) was applied thereon, and a resist composition was applied thereon, and baked at 100°C for 60 seconds (PB: Prebake) to form a resist film with a thickness of 30 nm.

[0412] This resist film was exposed through a reflective mask using an EUV exposure machine (manufactured by ASML; NXE3350, NA 0.33, Dipole 90°, outer sigma 0.87, inner sigma 0.35). Then, it was baked at 85°C for 60 seconds (PEB: Post Exposure Bake). Next, the developer was sprayed for 30 seconds by the spray method to develop, and the rinse solution was discharged onto the silicon wafer for 20 seconds by the spin coating method to rinse. Next, the silicon wafer was rotated at a rotation speed of 2000 rpm for 40 seconds to form a line-and-space pattern with a space width of 20 nm and a pattern line width of 15 nm. Here, when evaluating the developer, the developer to be evaluated was used as the developer, and chemical solution B049 (chemical solution obtained by the purification treatment of Example B049) was used as the rinsing solution. When evaluating the rinse solution, the developing solution used was chemical solution B018, and the rinse solution to be evaluated was used.

[0413] The above patterns were observed using a pattern defect measurement device (Hitachi High-Technologies Corporation's Multipurpose SEM (Scanning Electron Microscope) "Inspago" RS6000 series) to count the number of "PLOT defects", which are protrusion-like defects, "BRIDGE defects", which are defects that bridge between patterns, and "GEL defects", which are film-like residue defects, and evaluated according to the following criteria.

[0414] (PLOT defect evaluation criteria) A: The number of defects was less than 20 per wafer. B: The number of defects was 21 or more / wafer and 50 or less / wafer. C: The number of defects was 51 or more / wafer and 100 or less / wafer. D: The number of defects was 101 or more per wafer.

[0415] (BRIDGE defect evaluation criteria) A: The number of defects was less than 20 per wafer. B: The number of defects was 21 or more / wafer and 50 or less / wafer. C: The number of defects was 51 or more / wafer and 100 or less / wafer. D: The number of defects was 101 or more per wafer.

[0416] (GEL defect evaluation criteria) A: The number of defects was less than 20 per wafer. B: The number of defects was 21 or more / wafer and 50 or less / wafer. C: The number of defects was 51 or more / wafer and 100 or less / wafer. D: The number of defects was 101 or more per wafer.

[0417] [result] The following Tables 2 and 3 show the types of purified liquid and filters used in the purification process, as well as the evaluation results of the resulting chemical liquid. In Table 2, "P / R" in the "Use" column indicates that the defect suppression was evaluated when the chemical was used as a pre-wet liquid and rinse liquid using the method shown in the "Pre-wet liquid, rinse liquid" section. "Pipe" indicates that the defect suppression was evaluated when the chemical was used as a pipe cleaning liquid using the method shown in the "Pipe cleaning liquid" section. Table 3 shows the results of evaluation of defect suppression when the chemicals are used as a developer or rinse, using the method shown in the [Developer / Rinse] section. Tables 3a1 and 3a2 show the processing conditions of the purified liquid (the purified liquid and filter used) and the test results using the produced chemicals, respectively, in the same example. The relationship between Table 3a1 and Table 3a2 is also the same.

[0418] [Table 16]

[0419] [Table 17]

[0420] [Table 18]

[0421] [Table 19]

[0422] [Table 20]

[0423] [Table 21]

[0424] [Table 22]

[0425] From the results shown in the table, it was confirmed that by using the filter of the present invention, a chemical solution having excellent defect suppression properties can be produced.

[0426] Furthermore, it was confirmed that when the pore size of the filter is 10 nm or less, the produced chemical solution tends to have better defect suppression properties (comparison between Examples A003 and A019, etc.).

[0427] A filter containing less than 5.0 ppt by mass of the first organic compound was likely to adsorb the second organic compound during the cleaning process and in the environment, etc. Therefore, it was confirmed that a chemical solution produced using a filter containing 5.0 ppt by mass or more of the first organic compound tended to be more excellent in suppressing stain defects when the chemical solution was used as a pre-wet solution or a rinsing solution, and in suppressing uniformity defects when the chemical solution was used as a developer (Comparison between Example A013 and Examples A003, A012, and A018; Comparison between Example B008 and Examples B001, B007, and B013, etc.).

[0428] It was confirmed that a chemical solution produced using a filter having a total content of first organic compounds of 5.0 ppt by mass or more relative to the mass of the filter, and a total content of compounds selected from the group consisting of compounds represented by general formulas (I) to (VIII), alkanes represented by general formula (X), and alkenes represented by general formulas (XI) and (XII) of 6,500 ppt by mass or less relative to the mass of the filter, tends to have better stain defect suppression properties when the chemical solution is used as a pre-wet liquid or a rinsing liquid, and better uniformity defect suppression properties when the chemical solution is used as a developer (Comparison between Example A013 and Examples A003, A012, A018; Comparison between Examples A014, A015, A017 and Examples A012, A018; Comparison between Example B008 and Examples B001, B007, B013, etc.; Comparison between Examples B009, B010, B012 and Examples B007, B013, etc.).

[0429] It was confirmed that a chemical solution produced using a filter in which the total content of compounds selected from Group A is 0.10 to 3200 mass ppt relative to the mass of the filter tends to be more excellent in suppressing stain defects when the chemical solution is used as a pre-wet liquid or a rinsing liquid, and in suppressing uniformity defects when the chemical solution is used as a developer (Compare Example A013 with Examples A003, A012, A018; Compare Examples A014, A015, A017 with Examples A012, A018; Compare Example B008 with Examples B001, B007, B013, etc.; Compare Examples B009, B010, B012 with Examples B007, B013, etc.).

[0430] It was confirmed that a chemical solution produced using a filter in which the total content of compounds selected from Group B is 1.0 to 1200 mass ppt relative to the mass of the filter tends to be more excellent in suppressing stain defects when the chemical solution is used as a pre-wet liquid or a rinsing liquid, and in suppressing uniformity defects when the chemical solution is used as a developer (Comparison between Example A013 and Examples A003, A012, A018; Comparison between Examples A014, A015, A017 and Examples A012, A018; Comparison between Example B008 and Examples B001, B007, B013, etc.; Comparison between Examples B009, B010, B012 and Examples B007, B013, etc.).

[0431] It was confirmed that a chemical solution produced using a filter containing a specific metal component in an amount of 0.10 to 5000 ppt by mass relative to the mass of the filter tends to have better defect suppression properties (results of Example A016, etc.).

[0432] It was confirmed that when the filter body contains an ion exchange group, the produced chemical solution tends to have better defect suppression properties (eg, comparison of Examples A023 to A027).

[0433] It was confirmed that when the filter body was made of a material other than a fluorine-based material, the produced chemical solution tended to have better defect suppression properties (results of Examples B018 and 019, etc.).

[0434] The chemical solution produced is an organic solvent, and the Hansen solubility parameter range for eicosene is 3 to 20 MPa. 0.5 In the case of an organic solvent, it has been confirmed that the effects of the present invention (particularly, the defect suppression effect when a pattern is formed by EUV exposure and the chemical solution is used as a rinsing liquid) are more excellent (e.g., comparison of Examples B048, B051, B054, and B057).

[0435] In addition, the distance between the Hansen solubility parameters of the manufactured liquid and eicosene is 3 to 20 MPa. 0.5 The distance between the Hansen solubility parameters of organic solvents and eicosene is 3 to 20 MPa. 0.5 When the chemical solution contains an organic solvent other than the above, it has been confirmed that the effects of the present invention (particularly, the defect suppression effect when a pattern is formed by EUV exposure and the chemical solution is used as a rinsing liquid) are more excellent if the mixing ratio (mass ratio) is 20 / 80 to 80 / 20 (results of Examples B060, B063, B066, etc.).

[0436] Furthermore, similar filters to those used to produce "Filter 79, Filter 80, Filter 81, Filter 82" were prepared except that the packaging material was a fluororesin, and these were subjected to the same pretreatment as "Filter 79, Filter 80, Filter 81, Filter 82" to obtain "Filter 79b, Filter 80b, Filter 81b, Filter 82b." The analysis results of the contents of specific organic compounds and specific metal compounds in "Filter 79b, Filter 80b, Filter 81b, and Filter 82b" were equivalent to those of "Filter 79, Filter 80, Filter 81, and Filter 82," respectively. The obtained "Filter 79b, Filter 80b, Filter 81b, Filter 82b" were used to conduct tests similar to those conducted using "Filter 79, Filter 80, Filter 81, Filter 82," and results equivalent to those of the tests conducted using "Filter 79, Filter 80, Filter 81, Filter 82" were obtained. Comparing these results with the results of Examples B045 and B046, it was confirmed that the effects of the present invention are superior when a filter of the present invention is obtained by pre-treating a filter to be treated that is packed in a packaging material whose contact portion with the filter to be treated is a fluororesin or stainless steel. [Explanation of symbols]

[0437] 100 Filtration Equipment 101 Inlet 102 Outlet 103, 104 Filter 105 Piping

Claims

1. A method for producing a medicinal liquid, comprising purifying a liquid to be purified to obtain a medicinal liquid, the method comprising the step of filtering the liquid to be purified using a filter to obtain the medicinal liquid, The filter comprises a filter body and One or more first organic compounds selected from the group consisting of compounds represented by general formulas (I) to (V), alkanes represented by general formula (X), and alkenes represented by general formulas (XI) and (XII), The total content of the first organic compounds is 0.10 to 10,000 ppt by mass relative to the mass of the filter; The method for producing a chemical solution, wherein the chemical solution is a developer or a rinse solution. 【Chemistry 1】 In general formula (I), R １ａ and R １ｃ each independently represents an alkyl group which may contain a substituent. R １ｂ represents an alkylene group which may contain a substituent. 【Chemistry 2】 In the general formula (II), X represents a benzene ring group which may contain a substituent, a cyclohexene ring group which may contain a substituent, or a cyclohexane ring group which contains a cycloalkyloxy group as a substituent. The cyclohexane ring group may further contain another substituent. 【Chemistry 3】 In general formula (III), R ３ａ ~R ３ｈ each independently represents an alkyl group which may contain a substituent. R ３ｂ and R ３ｅ may be bonded to each other to form a ring. R ３ｂ and R ３ｅ The group formed by bonding with each other is -O-(-Si(R ３ｉ ) ２ -O-) ａ -It is. a represents an integer of 1 or more. R ３ｉ represents an alkyl group which may contain a substituent. Multiple R's ３ｉ may be the same or different. 【Chemistry 4】 In general formula (IV), R ４ａ is -N(R ４ｃ ) R ４ｄ Or -SR ４ｅ Represents. R ４ｃ , R ４ｄ , and R ４ｅ each independently represents a hydrogen atom or a substituent. R ４ｂ represents -NH- or -S-. 【Chemistry 5】 In formula (V), Y represents a benzene ring group which may be substituted with an alkyl group, or a group represented by formula (A). 【Chemistry 6】 When Y represents a benzene ring group, s represents 1, L represents a single bond, R ５ａ represents an alkyl group which may contain a substituent. The alkyl group may contain a heteroatom. When the benzene ring group is substituted with an alkyl group, the alkyl group and R ５ａ may be bonded to each other to form a ring. When a plurality of alkyl groups are substituted on the benzene ring group, the alkyl groups may be bonded to each other to form a ring. When Y represents a group represented by formula (A), s represents 3, L represents a methylene group, R ５ａ each independently represents an alkyl group. 【Chemistry 7】 In the general formula (X), j represents an integer of 12 to 50. Two j's have the same value. 【Chemistry 8】 In formula (XI), k represents an integer of 12 to 50. Two k's have the same value. 【Chemistry 9】 n represents an integer of 30 to 50. m represents an integer of 20 to 90 and not more than 2n-2.

2. The liquid to be purified is propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, propylene glycol monopropyl ether, cyclohexanone, methyl methoxypropionate, butyl acetate, γ-butyrolactone, 4-methyl-2-pentanol, propylene glycol monoethyl ether, ethyl lactate, cyclopentanone, diisoamyl ether, isoamyl acetate, isopropanol, dimethyl sulfoxide, N-methylpyrrolidone, diethylene glycol, ethylene glycol, dipropylene glycol , propylene glycol, ethylene carbonate, propylene carbonate, sulfolane, cycloheptanone, 2-heptanone, butyl butyrate, isobutyl isobutyrate, undecane, pentyl propionate, isopentyl propionate, ethylcyclohexane, mesitylene, decane, 3,7-dimethyl-3-octanol, 2-ethyl-1-hexanol, 1-octanol, 2-octanol, ethyl acetoacetate, dimethyl malonate, methyl pyruvate, and dimethyl oxalate.

3. A step of filtering the liquid to be purified using a filter to obtain a chemical solution; forming a resist film using an actinic ray-sensitive or radiation-sensitive resin composition; exposing the resist film obtained; forming a resist pattern on the exposed resist film by using the chemical solution as a developer or a rinse solution, The filter comprises a filter body and One or more first organic compounds selected from the group consisting of compounds represented by general formulas (I) to (V), alkanes represented by general formula (X), and alkenes represented by general formulas (XI) and (XII), The pattern forming method, wherein the total content of the first organic compounds is 0.10 to 10,000 ppt by mass relative to the mass of the filter. 【Chemistry 10】 In formula (I), R 1a and R 1c each independently represent an alkyl group which may contain a substituent. R 1b represents an alkylene group which may contain a substituent. 【Chemistry 11】 In the general formula (II), X represents a benzene ring group which may contain a substituent, a cyclohexene ring group which may contain a substituent, or a cyclohexane ring group which contains a cycloalkyloxy group as a substituent. The cyclohexane ring group may further contain another substituent. 【Chemistry 12】 In formula (III), R 3a to R 3h each independently represent an alkyl group which may contain a substituent. R 3b and R 3e may be bonded to each other to form a ring. The group formed by combining with R 3b and R 3e is —O—(—Si(R 3i ) 2 —O—) a —. a represents an integer of 1 or more. R 3i represents an alkyl group which may contain a substituent. A plurality of R 3i may be the same or different. 【Chemistry 13】 In formula (IV), R 4a represents -N(R 4c )R 4d or -SR 4e . R 4c , R 4d and R 4e each independently represent a hydrogen atom or a substituent. R 4b represents —NH— or —S—. 【Chemistry 14】 In formula (V), Y represents a benzene ring group which may be substituted with an alkyl group, or a group represented by formula (A). 【Chemistry 15】 When Y represents a benzene ring group, s represents 1, L represents a single bond, and R 5a represents an alkyl group which may contain a substituent. The alkyl group may contain a heteroatom. When the benzene ring group is substituted with an alkyl group, the alkyl group and R 5a may be bonded to each other to form a ring. When the benzene ring group is substituted with a plurality of alkyl groups, the alkyl groups may be bonded to each other to form a ring. When Y represents a group represented by formula (A), s represents 3, L represents a methylene group, and each R 5a independently represents an alkyl group. 【Chemistry 16】 In the general formula (X), j represents an integer of 12 to 50. Two j's have the same value. 【Chemistry 17】 In formula (XI), k represents an integer of 12 to 50. Two k's have the same value. 【Chemistry 18】 n represents an integer of 30 to 50. m represents an integer of 20 to 90 and not more than 2n-2.

4. The pattern forming method described in claim 3, further comprising a step of exposing the resist film using ArF exposure or EUV exposure.

5. The pattern forming method described in claim 3 or 4, wherein the actinic ray-sensitive or radiation-sensitive resin composition contains a resin having a repeating unit having a lactone structure.

6. The pattern forming method described in any one of claims 3 to 5, wherein the actinic ray-sensitive or radiation-sensitive resin composition contains a resin having a repeating unit based on hydroxystyrene.

7. The pattern forming method described in any one of claims 3 to 6, wherein the actinic ray-sensitive or radiation-sensitive resin composition further contains a hydrophobic resin.

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