WO2017217320A1 - 液体組成物が収容された収容容器及び液体組成物の保管方法 - Google Patents
液体組成物が収容された収容容器及び液体組成物の保管方法 Download PDFInfo
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Images
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- Y02W30/80—Packaging reuse or recycling, e.g. of multilayer packaging
Definitions
- the present invention relates to a container that contains a liquid composition used for surface modification in a semiconductor device manufacturing process and the like, and a method for storing the liquid composition.
- This pattern collapse occurs when the wafer is pulled up from the cleaning liquid or the rinse liquid. This is said to be caused by a difference in residual liquid height between a portion where the aspect ratio of the pattern is high and a portion where the aspect ratio is low, thereby causing a difference in capillary force acting on the pattern.
- the magnitude of the capillary force is the absolute value of P obtained by the following formula. From this formula, it is expected that the capillary force can be reduced by reducing ⁇ or cos ⁇ .
- the present invention relates to a container containing a liquid composition used for surface modification such as imparting water repellency in a manufacturing process of a semiconductor device and the like, and a storage method of the liquid composition, the surface being stored It is an object of the present invention to provide a storage container in which a liquid composition is stored, and a storage method for the liquid composition, in which deterioration of the reforming performance is suppressed.
- the present invention also accommodates a liquid composition excellent in recyclability that can suppress deterioration of surface modification performance due to storage even when used repeatedly as a container for the liquid composition. It is an object to provide a storage container and a method for storing a liquid composition.
- the part to be stored is a container having a contact angle ⁇ with respect to water of 10 degrees or more and 150 degrees or less.
- [3] is the container according to [2], wherein the surface treatment agent is a silylating agent.
- the liquid composition contains one or more metal atoms selected from the metal species consisting of Cu, Fe and Zn, and the total content of the particulate metal containing at least one of the metal atoms is
- the container according to any one of [1] to [10], which is 0.01 to 100 mass ppt based on the total mass of the liquid composition.
- At least a part of a portion of the inner wall of the housing portion that contacts the liquid composition is formed of a material containing at least one selected from polytetrafluoroethylene, perfluoroalkoxyalkane, polyethylene, and polypropylene.
- X 1 is a monovalent substituent in which an atom bonded to a silicon atom is a nitrogen atom, a monovalent substituent in which an atom bonded to a silicon atom is an oxygen atom, a halogen atom, a nitrile group, and —CO—NH Represents a group or atom selected from the group consisting of —Si (CH 3 ) 3 ; When a plurality of X 1 are present, they may be the same or different.
- a is an integer of 1 to 3
- b is an integer of 0 to 2
- the sum of a and b is 1 to 3.
- a method for storing a liquid composition comprising an organic solvent having a water concentration of 400 mass ppm or less and a surface treatment agent, wherein at least a part of the inner wall has a contact angle ⁇ with respect to water of 10 degrees or more and 150 degrees or less.
- a storage method for a liquid composition comprising storing the liquid composition in a storage container having a storage portion made of a member.
- the portion of the inner wall of the container that contacts the liquid composition has a contact angle with water before contacting the liquid composition as ⁇ A and a contact angle with water after contact with the liquid composition as ⁇
- the liquid composition contains one or more metal atoms selected from the metal species consisting of Cu, Fe and Zn, and the total content of the particulate metal containing at least one of the metal atoms is The method for storing a liquid composition according to any one of [16] to [25], wherein the liquid composition is 0.01 to 100 mass ppt based on the total mass of the liquid composition.
- At least a part of a portion in contact with the liquid composition on the inner wall of the housing portion is formed of a material containing at least one selected from polytetrafluoroethylene, perfluoroalkoxyalkane, polyethylene, and polypropylene.
- a storage method for the liquid composition according to any one of [27] to [27].
- X 1 is a monovalent substituent in which an atom bonded to a silicon atom is a nitrogen atom, a monovalent substituent in which an atom bonded to a silicon atom is an oxygen atom, a halogen atom, a nitrile group, and —CO—NH Represents a group or atom selected from the group consisting of —Si (CH 3 ) 3 ; When a plurality of X 1 are present, they may be the same or different.
- a is an integer of 1 to 3
- b is an integer of 0 to 2
- the sum of a and b is 1 to 3.
- a container containing a liquid composition used for surface modification such as imparting water repellency in a manufacturing process of a semiconductor device and the like and a storage method for the liquid composition. It is possible to provide a storage container in which a liquid composition is stored, and a storage method for the liquid composition, in which deterioration of the surface modification performance due to is suppressed.
- the container is repeatedly used as a container for the liquid composition, it is possible to suppress deterioration of surface modification performance due to storage, and a liquid composition having excellent recyclability can be stored. And a storage method of the liquid composition can be provided.
- FIG. 1 is a conceptual diagram for explaining a contact angle.
- the notation that does not indicate substitution and non-substitution includes not only a substituent but also a substituent.
- the “alkyl group” includes not only an alkyl group having no substituent (unsubstituted alkyl group) but also an alkyl group having a substituent (substituted alkyl group).
- active light beam or “radiation” in the present specification refers to, for example, an emission line spectrum of a mercury lamp, far ultraviolet rays represented by excimer laser, extreme ultraviolet (EUV) rays, X rays or electron rays ( Electron Beam (EB).
- light means actinic rays or radiation.
- the term “exposure” in the present specification is not limited to exposure with far-ultraviolet rays such as mercury lamps and excimer lasers, X-rays and EUV light, but also with particle beams such as electron beams and ion beams, unless otherwise specified. Drawing is also included in the exposure.
- “(meth) acrylate” in the present specification means “at least one of acrylate and methacrylate”.
- “(Meth) acrylic acid” means “at least one of acrylic acid and methacrylic acid”.
- a numerical range expressed using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.
- the liquid composition filled in the container according to the present invention is a liquid composition used for surface modification such as imparting water repellency in the manufacturing process of a semiconductor device or the like (hereinafter also referred to as “treatment liquid”). It contains a surface treatment agent and an organic solvent.
- This organic solvent is an organic solvent having a moisture concentration of 400 ppm by mass (parts per million) or less (hereinafter also referred to as “non-aqueous organic solvent”).
- the present invention relates to a specific storage container in which the liquid composition is stored, and the present invention also relates to a storage method in which the liquid composition is stored in a specific storage container.
- the specific storage container will be described in detail later, but at least the part of the inner wall of the storage part in which the liquid composition is stored is in contact with the liquid composition has a contact angle ⁇ with respect to water of 10 degrees or more and 150 degrees or less. It is a storage container.
- the liquid composition will be described, and then the container will be described.
- the liquid composition of the present invention is used for surface modification such as imparting water repellency in the manufacturing process of a semiconductor device, and contains a surface treatment agent and a non-aqueous organic solvent.
- the liquid composition of the present invention may further contain an acid or a base.
- the liquid composition of the present invention is preferably a composition that does not substantially contain water.
- substantially free of water means that, in addition to water that can exist in an equilibrium state such as adsorbed water, it does not include raw materials to which water is intentionally added. It means that it was prepared without adding.
- the water concentration in the liquid composition of the present invention is preferably 400 ppm by mass or less with respect to the total mass of the liquid composition.
- the amount is preferably 200 ppm by mass or less, more preferably 100 ppm by mass or less, and still more preferably 50 ppm by mass or less.
- the water concentration is 0 ppm by mass, but it may be, for example, 0.01 mass ppt (parts per trillion) or more.
- the liquid composition of the present invention is preferably used, for example, for forming a water-repellent protective film.
- the water-repellent protective film is a film that is formed on the wafer surface to lower the wettability of the wafer surface, that is, a film that imparts water repellency.
- the water repellency means that the surface energy of the article surface is reduced and the interaction (for example, hydrogen bond, intermolecular force) between water or other liquid and the article surface is reduced. It is.
- the effect of reducing the interaction with water is great, but it has the effect of reducing the interaction with a mixed liquid of water and a liquid other than water or a liquid other than water. By reducing the interaction, the contact angle of the liquid with the article surface can be increased.
- the water-repellent protective film may be simply referred to as “protective film”.
- the cleaning liquid is removed from the concave portion of the concave / convex pattern of the wafer, that is, when dried, the protective film is formed on at least the concave portion surface. , Capillary force on the surface of the recess is reduced, and pattern collapse is less likely to occur.
- the liquid composition of the present invention has a concavo-convex pattern on the surface, and a water-repellent protective film is formed on at least the concave surface of the concavo-convex pattern when cleaning a wafer in which at least a part of the concavo-convex pattern contains silicon atoms. Used to form.
- Nonaqueous organic solvent As the organic solvent (non-aqueous organic solvent) having a water concentration of 400 ppm by mass or less, contained in the liquid composition of the present invention, for example, it is preferable to use a grade having very little water and metal impurities. It is preferable to use a non-aqueous organic solvent that has been further dehydrated and purified.
- the liquid composition comprises a non-aqueous organic solvent after this dehydration step (more preferably after the dehydration and purification step), a surface treatment agent, and, where applicable, for example, an acid or a base. It is obtained by mixing arbitrary components such as (mixing step).
- the dehydration step when the water concentration in the non-aqueous organic solvent is 400 mass ppm or less, the non-aqueous organic solvent, the surface treatment agent, and, if applicable, the acid or base are mixed in the subsequent mixing step.
- the surface treatment agent due to hydrolysis or the like, and if applicable, the acid or base activity is less likely to decrease.
- excellent water repellency can be imparted to the concave surface of the wafer.
- the pot life of the liquid composition is excellent.
- the water concentration in the non-aqueous organic solvent is preferably 200 ppm by mass or less, more preferably 100 ppm by mass or less, and further preferably 50 ppm by mass or less. This is because the water repellency imparting effect and pot life of the liquid composition are more excellent.
- the water concentration in the non-aqueous organic solvent in the dehydration step is ideally 0 mass ppm, but may be, for example, 0.01 mass ppt (parts per trillion) or more.
- the moisture concentration can be measured, for example, by measurement with a Karl Fischer moisture meter.
- the dehydration step can be performed by a known method.
- the nonaqueous organic solvent is purified by distillation, or an insoluble water adsorbent (for example, molecular sieve) is added to the nonaqueous organic solvent. It is preferably at least one method selected from the group consisting of removing water, aeration replacement with a dry inert gas, heating or vacuum heating.
- the water adsorbent insoluble in the non-aqueous organic solvent is at least one selected from the group consisting of zeolite, phosphorus pentoxide, silica gel, calcium chloride, sodium sulfate, magnesium sulfate, anhydrous zinc chloride, fuming sulfuric acid, and soda lime. It is preferable that
- hydrocarbons such as toluene, benzene, xylene, hexane, heptane, and octane, ethyl acetate, propyl acetate, butyl acetate, and acetoacetic acid.
- Esters such as ethyl, ethers such as diethyl ether, dipropyl ether, dibutyl ether, tetrahydrofuran, dioxane, acetone, acetylacetone, methyl ethyl ketone, methyl propyl ketone, methyl butyl ketone, cyclohexanone, ketones such as isophorone, perfluorooctane, Perfluorocarbons such as perfluorononane, perfluorocyclopentane, perfluorocyclohexane, hexafluorobenzene, 1, 1, 1, 3, 3-pentafluorobutane, octafluorocyclopentane, 2 Hydrofluorocarbons such as 3-dihydrodecafluoropentane, Zeolora H (manufactured by Nippon Zeon), methyl perfluoroisobutyl ether, methyl perfluor
- Fluorocarbon 1,1-dichloro-2,2,3,3,3-pentafluoropropane, 1,3-dichloro-1,1,2,2,3
- hydrochlorofluorocarbons such as pentafluoropropane, 1-chloro-3,3,3-trifluoropropene, 1,2-dichloro-3,3,3-trifluoropropene, perfluoroether, perfluoropolyether, etc.
- Halogen-containing solvents such as dimethyl sulfoxide, ⁇ -butyrolactone, ⁇ -valerolactone, ⁇ -hexanolactone, ⁇ -heptanolactone, ⁇ -octanolactone, ⁇ -nonanolactone, ⁇ -decanolactone, ⁇ -unde Canolactone, ⁇ -dodecanolactone, ⁇ -valerolactone, ⁇ -hexanolactone, ⁇ -octanolactone, ⁇ -nonanolactone, ⁇ -decanolactone, ⁇ -undecanolactone, ⁇ -dodecanolactone, ⁇ -hexano Lactone solvents such as lactone, dimethyl carbonate, Carbonate solvents such as methyl carbonate, diethyl carbonate, propylene carbonate, methanol, ethanol, propanol, butanol, ethylene glycol, diethylene glycol,
- the non-aqueous organic solvent includes hydrocarbons, esters, ethers, ketones, halogen-containing solvents, sulfoxide solvents, It is preferably at least one selected from the group consisting of a lactone solvent, a carbonate solvent, a derivative of a polyhydric alcohol having no OH group, and a nitrogen element-containing solvent having no NH group.
- the silylating agent easily reacts with a non-aqueous organic solvent containing an OH group or an NH group, when a non-aqueous organic solvent containing an OH group or an NH group is used as the non-aqueous organic solvent, There is a possibility that the reactivity of the silylating agent may be reduced, and as a result, water repellency may not be easily developed in a short time.
- the silylating agent hardly reacts with a non-aqueous organic solvent that does not contain OH groups or NH groups, a non-aqueous organic solvent that does not contain OH groups or NH groups is used as the non-aqueous organic solvent.
- the non-aqueous organic solvent containing no OH group or NH group includes both a non-aqueous polar solvent containing no OH group or NH group and a non-aqueous non-polar solvent containing no OH group or NH group. That is.
- non-flammable solvent for part or all of the non-aqueous organic solvent, the chemical solution for forming the protective film becomes non-flammable or the flash point becomes high, and the risk of the chemical solution is reduced. This is preferable.
- Many halogen-containing solvents are nonflammable, and the nonflammable halogen-containing solvent can be suitably used as a nonflammable organic solvent.
- a solvent having a flash point exceeding 70 ° C. is preferable to use as the non-aqueous organic solvent from the viewpoint of safety in the Fire Service Act.
- a solvent having a flash point of 93 ° C. or lower is defined as “flammable liquid”. Therefore, even if it is not a non-flammable solvent, if a solvent having a flash point of more than 93 ° C. is used as the non-aqueous organic solvent, the flash point of the protective film-forming chemical solution tends to exceed 93 ° C., and the chemical solution is “flammable. This is more preferable from the viewpoint of safety.
- lactone solvents those having no OH group are preferred because they have a high flash point and can reduce the risk of the protective film-forming chemical.
- ⁇ -butyrolactone, ⁇ -valerolactone, ⁇ -hexanolactone, ⁇ -heptanolactone, ⁇ -octanolactone, and ⁇ -nonanolactone having a flash point exceeding 70 ° C.
- the surface treatment agent contained in the liquid composition of the present invention is not particularly limited as an application, it is used, for example, for an application for controlling hydrophilicity / hydrophobicity of a substance surface.
- the surface treatment agent include alkylating agents, silane compounds, aluminum coupling agents, titanate coupling agents, zirconate coupling agents, tin coupling agents, and zirconium aluminate coupling agents.
- a silane compound for the surface treatment use in the manufacturing process of a semiconductor device.
- the silane compound is a compound having a hydrogen-silicon bond or a carbon-silicon bond in the molecule, and specific examples include a silylating agent and a silane coupling agent.
- a silylating agent and a silane coupling agent.
- two or more surface treatment agents may be used in combination.
- the alkylating agent is preferably a compound represented by, for example, R 7 -X.
- R 7 represents a hydrogen atom, an alkyl group having 1 to 20 carbon atoms, an allyl group or a benzyl group
- X represents a fluorine atom, a chlorine atom, a bromine atom, an iodine atom, a mesyloxy group, a tosyloxy group or Represents a trifluoromethylsulfonyloxy group.
- alkylating agent examples include trialkyloxonium tetrafluoroborate, alkyl triflate, dialkyl sulfate, alkyl tosylate, alkyl mesylate, alkyl iodide, alkyl bromide, alkyl chloride, alkyl fluoride, etc. Can do.
- the silylating agent is preferably at least one selected from the group consisting of silicon-containing compounds represented by the following general formula [1].
- R 1 represents a monovalent organic group containing a hydrocarbon group having 1 to 18 carbon atoms in which some or all of the hydrogen atoms may be replaced by fluorine atoms. When a plurality of R 1 are present, they may be the same or different.
- X 1 is a monovalent substituent in which an atom bonded to a silicon atom is a nitrogen atom, a monovalent substituent in which an atom bonded to a silicon atom is an oxygen atom, a halogen atom, a nitrile group, and —CO—NH Represents a group or atom selected from the group consisting of —Si (CH 3 ) 3 ; When a plurality of X 1 are present, they may be the same or different.
- a is an integer of 1 to 3
- b is an integer of 0 to 2
- the sum of a and b is 1 to 3.
- R 1 in the general formula [1] reduces the surface energy of the protective film formed using the liquid composition of the present invention, and is between the surface of the protective film and the surface of water or other liquid (interface). It has the effect of reducing the interaction. For example, interactions such as hydrogen bonds and intermolecular forces are reduced. In particular, the effect of reducing the interaction with water is great, but it has the effect of reducing the interaction with a mixed liquid of water and a liquid other than water or a liquid other than water. Thereby, the contact angle of the liquid with respect to the article
- X 1 in the general formula [1] is a reactive site having reactivity with a silanol group that is a reaction site of a silicon wafer, and the reactive site reacts with the silanol group of the wafer to form a silylating agent.
- the monovalent substituent in which the atom bonded to the silicon atom which is an example of X 1 in the general formula [1] is nitrogen includes not only hydrogen, carbon, and nitrogen, but also oxygen, silicon, sulfur, halogen, and the like. An atom may be included.
- substituents examples include isocyanate groups, amino groups, dialkylamino groups, isothiocyanate groups, azide groups, acetamide groups, —N (CH 3 ) C (O) CH 3 , —N (CH 3 ) C (O ) CF 3 , —N ⁇ C (CH 3 ) OSi (CH 3 ) 3 , —N ⁇ C (CF 3 ) OSi (CH 3 ) 3 , —NHC (O) —OSi (CH 3 ) 3 , —NHC ( O) —NH—Si (CH 3 ) 3 , imidazole ring (formula [7]), oxazolidinone ring (formula [8]), morpholine ring (formula [9]), —NH—C (O) — Si (CH 3 ) 3 , —N (H) 2 -h (Si (H) i R 9 3-i ) h (R 9 may be partially or entirely replaced with flu
- X 1 in the general formula [1] is oxygen, not only hydrogen, carbon, and oxygen, but also nitrogen, silicon, sulfur, halogen, and the like May be included.
- substituents examples include an alkoxy group, —OC (CH 3 ) ⁇ CHCOCH 3 , —OC (CH 3 ) ⁇ N—Si (CH 3 ) 3 , —OC (CF 3 ) ⁇ N—Si (CH 3 3 , —O—CO—R 10 (R 10 is a monovalent hydrocarbon group having 1 to 18 carbon atoms in which some or all of the hydrogen elements may be substituted with fluorine atoms or the like), part Alternatively, there is an alkyl sulfonate group in which all hydrogen atoms may be substituted with fluorine atoms or the like.
- halogen atom examples include a chloro atom, a bromo atom, and an iodo atom.
- Examples of the silylating agent represented by the general formula [1] include CH 3 Si (OCH 3 ) 3 , C 2 H 5 Si (OCH 3 ) 3 , C 3 H 7 Si (OCH 3 ) 3 , C 4 H 9 Si (OCH 3 ) 3 , C 5 H 11 Si (OCH 3 ) 3 , C 6 H 13 Si (OCH 3 ) 3 , C 7 H 15 Si (OCH 3 ) 3 , C 8 H 17 Si (OCH 3 ) 3 , C 9 H 19 Si (OCH 3 ) 3 , C 10 H 21 Si (OCH 3 ) 3 , C 11 H 23 Si (OCH 3 ) 3 , C 12 H 25 Si (OCH 3 ) 3 , C 13 H 27 Si (OCH 3) 3 , C 14 H 29 Si (OCH 3) 3, C 15 H 31 Si (OCH 3) 3, C 16 H 33 Si (OCH 3) 3, C 17 H 35 Si (OCH 3 ) 3 , C 18 H 37 Si (OCH 3 )
- the number of X 1 represented by 4-ab in the general formula [1] is 1 because the protective film can be formed uniformly.
- m 1 to 12
- n 1 to 8 because a protective film can be formed on the surface of the concavo-convex pattern in a short time.
- Silane coupling agent is preferably at least one selected from the group consisting of silicon-containing compounds represented by the following general formula [2].
- R 1 represents a monovalent organic group containing a hydrocarbon group having 1 to 18 carbon atoms in which some or all of the hydrogen atoms may be replaced by fluorine atoms. When a plurality of R 1 are present, they may be the same or different.
- Y 1 is an unsubstituted monovalent hydrocarbon group such as an alkyl group having 1 to 12 carbon atoms (particularly preferably, 1 to 10 carbon atoms), a cycloalkyl group, an alkenyl group, an aryl group, an aralkyl group, or the like.
- halogen atoms chlorine, fluorine, bromine atoms, etc.
- cyano groups oxyalkylene groups such as oxyethylene groups, polyoxyalkylene groups such as polyoxyethylene groups, (meth) acryl groups
- Substituted monovalent hydrocarbon groups substituted with functional groups such as (meth) acryloxy group, acryloyl group, methacryloyl group, mercapto group, amino group, amide group, ureido group, and epoxy group, these unsubstituted or substituted monovalent hydrocarbons in the group, an oxygen atom, NH group, NCH 3 group, NC 6 H 5 group, C 6 H 5 NH- group, such as H 2 NCH 2 CH 2 NH- group is interposed Group, and the like was.
- a is an integer of 1 to 3
- NC 6 H 5 group, C 6 H 5 NH- group such as H 2 NCH 2 CH 2 NH- group is interposed Group, and the like was.
- a is an
- vinyl silane such as vinyltrichlorosilane, vinyltris ( ⁇ -methoxyethoxy) silane, vinyltriethoxysilane, vinyltrimethoxysilane; ⁇ -methacryloxypropyltrimethoxysilane; ⁇ - (3,4-epoxycyclohexyl) )
- Epoxy silanes such as ethyltrimethoxysilane, ⁇ -glycidoxypropyltrimethoxysilane, ⁇ -glycidoxypropylmethyldiethoxysilane; N- ⁇ - (aminoethyl) - ⁇ -aminopropyltrimethoxysilane, N- aminosilanes such as ⁇ - (aminoethyl) - ⁇ -aminopropylmethyldimethoxysilane, ⁇ -aminopropyltrimethoxysilane, N-phenyl- ⁇ -aminopropyltrimethoxysilane, N
- titanate coupling agent examples include amine-based, phosphorous acid type, pyrophosphoric acid type, and carboxylic acid type titanate coupling agents.
- isopropyl triisostearoyl titanate isopropyl tridodecyl benzene sulfonyl titanate
- isopropyl tris (dioctyl pyrophosphate) titanate isopropyl tris (dioctyl pyrophosphate) titanate
- tetraoctyl bis (ditridecyl phosphite) titanate Tetra (2,2-diallyloxymethyl) bis (ditridecyl) phosphite titanate
- Aluminum coupling agent examples include aluminum isopropylate, mono sec-butoxyaluminum diisopropylate, aluminum sec-butyrate, aluminum ethylate, ethylacetoacetate aluminum diisopropylate, aluminum tris (ethyl Acetoacetate), alkyl acetoacetate aluminum diisopropylate, aluminum monoacetylacetonate bis (ethylacetoacetate), aluminum tris (acetylacetoacetate) and the like.
- zirconate coupling agent examples include tetra-n-propoxyzirconium, tetra-butoxyzirconium, zirconium tetraacetylacetonate, zirconium dibutoxybis (acetylacetonate), zirconium tributoxyethyl acetoacetate, zirconium butoxyacetylacetonate. Examples thereof include bis (ethyl acetoacetate).
- tin coupling agents include tin halide compounds such as dichlorotin, monomethyldichlorotin, dimethyldichlorotin, monoethyldichlorotin, diethyldichlorotin, methyltrichlorotin, monobutyldichlorotin, dibutyldibromotin, mono Hexyl dichlorotin, tetrachlorotin, etc. are used.
- tin halide compounds such as dichlorotin, monomethyldichlorotin, dimethyldichlorotin, monoethyldichlorotin, diethyldichlorotin, methyltrichlorotin, monobutyldichlorotin, dibutyldibromotin, mono Hexyl dichlorotin, tetrachlorotin, etc. are used.
- the liquid composition of the present invention may contain an acid or a base.
- the acid hydrogen chloride, sulfuric acid, perchloric acid, sulfonic acid represented by the following general formula [3] and anhydride thereof
- carboxylic acid represented by the following general formula [4] and anhydride thereof Alkyl borate ester, aryl borate ester, tris (trifluoroacetoxy) boron, trialkoxyboroxine, trifluoroboron, and at least one selected from the group consisting of silane compounds represented by the following general formula [5] Is preferred.
- R 2 S (O) 2 OH [3]
- R 2 is a monovalent hydrocarbon group having 1 to 18 carbon atoms in which some or all of the hydrogen atoms may be replaced by fluorine atoms.
- R 3 is a monovalent hydrocarbon group having 1 to 18 carbon atoms in which some or all of the hydrogen atoms may be replaced by fluorine atoms.
- R 4 is a monovalent hydrocarbon group having 1 to 18 carbon atoms in which some or all of the hydrogen atoms may be replaced with fluorine atoms. When a plurality of R 4 are present, they may be the same or different.
- X 2 is a chloro atom, —OCO—R 5 (R 5 is a monovalent hydrocarbon group having 1 to 18 carbon atoms in which some or all of the hydrogen atoms may be replaced by fluorine atoms), and , —OS (O) 2 —R 6 (R 6 is a monovalent hydrocarbon group having 1 to 18 carbon atoms in which some or all of the hydrogen atoms may be replaced by fluorine atoms) Represents at least one group selected. When a plurality of X 2 are present, they may be the same or different.
- C is an integer from 1 to 3
- d is an integer from 0 to 2
- the sum of c and d is 1 to 3.
- Examples of the sulfonic acid represented by the above general formula [3] and its anhydride include methanesulfonic acid, benzenesulfonic acid, p-toluenesulfonic acid, trifluoromethanesulfonic acid, trifluoromethanesulfonic anhydride, and the like.
- Examples of the carboxylic acid represented by [3] and its anhydride include acetic acid, trifluoroacetic acid, pentafluoropropionic acid, acetic anhydride, trifluoroacetic anhydride, pentafluoropropionic anhydride, and the above general formula [4].
- silane compound represented by the formula chlorosilane, alkylsilylalkyl sulfonate, and alkylsilyl ester are preferable, and trimethylsilyl trifluoroacetate, trimethylsilyl trifluoromethanesulfonate, dimethylsilyl trifluoroacetate, dimethylsilyl triflate.
- Oromethanesulfonate butyldimethylsilyl trifluoroacetate, butyldimethylsilyl trifluoromethanesulfonate, hexyldimethylsilyl trifluoroacetate, hexyldimethylsilyl trifluoromethanesulfonate, octyldimethylsilyl trifluoroacetate, octyldimethylsilyl trifluoromethanesulfonate, decyldimethylsilyltriflate
- fluoroacetate and decyldimethylsilyl trifluoromethanesulfonate examples include fluoroacetate and decyldimethylsilyl trifluoromethanesulfonate.
- the above bases are ammonia, N, N, N ′, N′-tetramethylethylenediamine, triethylenediamine, dimethylaniline, alkylamine, dialkylamine, trialkylamine, pyridine, piperazine, N-alkylmorpholine, At least one selected from the group consisting of silane compounds represented by [6] is preferred.
- R 7 is a monovalent hydrocarbon group having 1 to 18 carbon atoms in which some or all of the hydrogen atoms may be replaced by fluorine atoms. When a plurality of R 7 are present, they may be the same or different.
- X 3 is a monovalent substituent in which the atom bonded to the silicon atom is a nitrogen atom and may contain a fluorine atom or a silicon atom. When a plurality of X 3 are present, they may be the same or different.
- e is an integer of 1 to 3
- f is an integer of 0 to 2
- the sum of e and f is 1 to 3.
- the acid or base promotes the reaction between the silylating agent and a silanol group that is a reaction site on the concave / convex pattern surface of the silicon wafer. Therefore, excellent water repellency can be imparted to the wafer surface by the surface treatment with the liquid composition of the present invention.
- the acid or base may form part of the protective film.
- an acid is contained in the liquid composition, among which a strong acid such as hydrogen chloride and perchloric acid, such as Bronsted acid, trifluoromethanesulfonic acid and trifluoromethanesulfonic anhydride, Some or all of the hydrogen atoms are replaced by fluorine atoms, such as alkane sulfonic acids in which some or all of the hydrogen atoms are substituted with fluorine atoms, their anhydrides, trifluoroacetic acid, trifluoroacetic anhydride, pentafluoropropionic acid, etc.
- a strong acid such as hydrogen chloride and perchloric acid, such as Bronsted acid, trifluoromethanesulfonic acid and trifluoromethanesulfonic anhydride
- fluorine atoms such as alkane sulfonic acids in which some or all of the hydrogen atoms are substituted with fluorine atoms, their anhydrides, trifluoroacetic acid, triflu
- alkylsilyl ester is a silicon element in which an alkyl group and —O—CO—R ′ group (R ′ is an alkyl group) are bonded.
- the acid that can be contained in the liquid composition may be produced by a reaction, for example, by reacting an alkylchlorosilane with an alcohol and using the produced alkylalkoxysilane as a silylating agent, and the produced hydrochloric acid. It is also possible to obtain a chemical solution for forming a protective film in which the acid is an acid and the alcohol that has not been consumed in the reaction is a non-aqueous organic solvent.
- the content of the surface treatment agent is preferably 0.1 to 20% by mass relative to the total mass of the liquid composition, and when the acid or base is contained, the content is The content is preferably 0.0001 to 4% by mass relative to the total mass of the composition.
- liquid composition of the present invention include at least one non-aqueous organic solvent selected from the group consisting of hydrofluoroethers, hydrochlorofluorocarbons, polyhydric alcohol derivatives not having an OH group, and lactone solvents.
- a non-aqueous organic solvent selected from the group consisting of hydrofluoroethers, hydrochlorofluorocarbons, polyhydric alcohol derivatives not having an OH group, and lactone solvents.
- At least one non-aqueous organic solvent selected from the group consisting of hydrofluoroether, hydrochlorofluorocarbon, and a derivative of a polyhydric alcohol having no OH group is 76 to 99.8999% by mass, hexa Methyldisilazane, tetramethyldisilazane, 1,3-dibutyltetramethyldisilazane, 1,3-dihexyltetramethyldisilazane, 1,3-dioctyltetramethyldisilazane, 1,3-didecyltetramethyldisilazane, 0.1 to 20% by mass of at least one silylating agent selected from the group consisting of 1,3-didodecyltetramethyldisilazane, trifluoroacetic acid, trifluoroacetic anhydride, trifluoromethanesulfonic acid, trifluoroacetic anhydride Lomethane
- the liquid composition of the present invention contains one or more metal atoms selected from the metal species consisting of Cu, Fe and Zn, and has a particle property containing at least one of these metal atoms.
- the total metal content is preferably 0.01 to 100 mass parts per million (ppts) based on the total mass of the liquid composition.
- a metal element selected from a metal species consisting of Cu, Fe and Zn (hereinafter also referred to as “target metal”) is contained in the liquid composition as an impurity, and the liquid composition of the present invention is a semiconductor.
- target metal a metal element selected from a metal species consisting of Cu, Fe and Zn
- the liquid composition of the present invention is a semiconductor.
- particles containing these metal elements become defects and have a great influence on the formation of a fine resist pattern or a fine semiconductor element. For this reason, it was considered that the smaller the amount of metal atoms contained in the liquid composition, the better the occurrence of defects in semiconductor manufacturing.
- the present inventor has found that the amount of metal atoms contained in the liquid composition does not always correlate with the defect occurrence rate, and the defect occurrence rate varies.
- the amount of metal atoms present in the solution is divided into an ionic metal and a particulate metal (nonionic metal). It became possible to measure.
- the particulate metal is a metal component that does not dissolve in the solution and exists as a solid.
- the amount of metal atoms contained in a liquid composition has usually been analyzed by the ICP-MS method, and depending on the ICP-MS, an ionic metal and a particulate metal containing at least one kind of metal atoms are used. Since (nonionic metal) cannot be identified, the total mass of metal atoms, that is, the total mass of ionic metal and particulate metal (nonionic metal) (hereinafter also referred to as “total metal amount”). Quantified.
- the present inventor has developed an ionic metal and a particulate metal derived from metal atoms contained in a liquid composition that can be identified and quantified by SP-ICP-MS (Single-Particle ICP-MS) measurement.
- SP-ICP-MS Single-Particle ICP-MS
- the preferable content of the particulate metal described above is based on such new knowledge, and the content of the particulate metal in the liquid composition of the present invention is more preferably 0.01 to 50 mass ppt. Preferably, it is 0.01 to 10 mass ppt.
- the liquid composition of the present invention is preferably filtered with a filter for the purpose of removing foreign substances or reducing defects. If it is conventionally used for the filtration use etc., it can use without being specifically limited.
- a filter made of fluorine resin such as PTFE (polytetrafluoroethylene), polyamide resin such as nylon, polyolefin resin (including high density and ultra high molecular weight) such as polyethylene and polypropylene (PP), and the like can be given.
- PTFE polytetrafluoroethylene
- polyamide resin such as nylon
- polyolefin resin including high density and ultra high molecular weight
- polyethylene and polypropylene (PP) polypropylene
- nylon are preferable.
- the pore size of the filter is suitably about 0.001 to 1.0 ⁇ m, preferably about 0.02 to 0.5 ⁇ m, more preferably about 0.01 to 0.1 ⁇ m. By setting it as this range, it becomes possible to remove fine foreign matters, such as impurities or aggregates contained in the processing liquid, while suppressing filtration clogging.
- the filtering by the first filter may be performed only once or may be performed twice or more.
- the second and subsequent pore diameters are the same or larger than the pore diameter of the first filtering.
- the pore diameter here can refer to the nominal value of the filter manufacturer. As a commercially available filter, it can select from the various filters which Nippon Pole Co., Ltd., Advantech Toyo Co., Ltd., Japan Integris Co., Ltd. (former Japan Microlith Co., Ltd.), KITZ micro filter, etc. provide, for example.
- the second filter a filter formed of the same material as the first filter described above can be used.
- the pore size of the second filter is suitably about 0.01 to 1.0 ⁇ m, preferably about 0.1 to 0.5 ⁇ m. By setting it as this range, when the component particles are contained in the processing liquid, the foreign matters mixed in the processing liquid can be removed while the component particles remain.
- the filtering by the first filter is performed with a mixed solution containing a part of the components of the processing liquid, the remaining components are mixed with this to prepare the processing liquid, and then the second filtering is performed. Also good.
- the filter used before filtering a process liquid.
- the liquid used for this treatment is not particularly limited, but the metal content is preferably less than 0.001 mass ppt (parts per trillion), and other organic solvents can be purified in addition to the water described above, If the metal content is within the above range, or the treatment liquid of the present invention itself, a dilution of the treatment liquid, or a liquid containing a compound added to the treatment liquid, the desired effect of the present application is remarkably obtained. It is done.
- the liquid composition of the present invention preferably has an ion concentration of 1 ppm (parts per million) or less, such as Na, Ca, Al, Cr, Co, Pb, Li, Mg, Mn, Ni, K, and Ag. More preferably, it is 1 ppb (parts per billion) or less. In particular, it is more preferably in the order of ppt (all the above concentrations are based on mass), and it is particularly preferable that the concentration is not substantially contained.
- the adjustment of the metal content in the liquid composition of the present invention can be performed by, for example, distillation or at least one of the raw material stage used in producing the liquid composition and the stage after preparing the treatment liquid. Filter filtration, filtration using an ion exchange resin, adsorption purification, etc. may be repeated for sufficient purification.
- the method for adjusting the metal content rate (hereinafter, also referred to as “metal concentration reducing method”) is not particularly limited, but silicon carbide described in International Publication No. WO12 / 043396 is used. Adsorption purification etc. are mentioned, Furthermore, the example which combines distillation, filter filtration, and filtration using an ion exchange resin, and fully refine
- the method for adjusting the metal content is particularly preferably performed at the stage of raw materials used when producing a liquid composition from the viewpoint of obtaining the effects of the present invention.
- a container for containing raw materials used in the production of a liquid composition
- impurities described as for a container for containing the liquid composition of the present invention to be described later will be described.
- a container with little elution may be used.
- the liquid composition of this invention does not contain a coarse particle substantially.
- the coarse particles contained in the liquid composition are particles such as dust, dust, organic solids, and inorganic solids contained as impurities in the raw material, and dust, dust, Examples of the particles include organic solids and inorganic solids, which finally exist as particles without being dissolved in the treatment liquid.
- the amount of coarse particles present in the treatment liquid can be measured in a liquid phase using a commercially available measuring apparatus in a light scattering type in-liquid particle measurement method using a laser as a light source.
- the liquid composition of this invention is preserve
- the container of the present invention relates to a container (hereinafter also referred to as “the container of the present invention”) including a container in which the liquid composition of the present invention described above is stored.
- the storage container of the present invention at least a portion of the inner wall of the storage portion that contacts the liquid composition of the present invention (hereinafter sometimes referred to as “contact portion”) has a contact angle ⁇ with respect to water of 10 degrees or more and 150 degrees.
- the first feature is as follows. When the liquid composition of the present invention is filled and stored in such a container, it is possible to suppress deterioration in performance such as water repellency.
- the “contact angle” is an index relating to the wettability of the surface of a certain substance with respect to a certain liquid.
- the contact angle ⁇ is an index relating to the wettability of the surface of a certain substance with respect to a certain liquid.
- the contact angle in the present invention is a value measured by the ⁇ / 2 method which will be described later in Examples.
- water here means ultrapure water, and a high grade used in semiconductor manufacturing is preferable.
- ultrapure water in which the content of each of Fe, Cu, and Zn is less than 10 mass ppt is preferable.
- At least a portion of the inner wall of the housing portion that is in contact with the liquid composition of the present invention has a water contact angle ⁇ of 10 degrees to 150 degrees as described above, and 50 degrees to 125 degrees. It is more preferable that it is 70 degrees or more and 115 degrees or less.
- the contact angle ⁇ is 10 degrees or more, the inner wall of the housing portion has a small interaction with water, so that it is difficult to adsorb moisture, and it is presumed that even if moisture is adsorbed, it is easily detached. In other words, it is estimated that moisture is hardly retained. Therefore, there is almost no moisture brought into the liquid composition from the inner wall of the housing portion, and it becomes possible to suppress deterioration in performance such as water repellency due to water mixing into the liquid composition during storage. From the above viewpoint, the contact angle ⁇ is 10 degrees or more, preferably 50 degrees or more, and particularly preferably 70 degrees or more.
- the container of the present invention is required to have durability when the container is repeatedly used (when recycled).
- the contact angle ⁇ is 150 degrees or less, physical changes such as wear and delamination, chemical changes such as corrosion and chemical reaction, and changes due to adsorption of contaminants when the container is used repeatedly Etc. are suppressed, and the durability is remarkably excellent.
- the contact angle ⁇ is 150 degrees or less, preferably 125 degrees or less, and particularly preferably 115 degrees or less.
- the portion of the inner wall of the housing portion that contacts the liquid composition of the present invention has a contact angle with water after contact with the liquid composition of the present invention as ⁇ B, and before this contact
- is preferably 3 ° or more, and preferably 15 ° or less, where ⁇ A is the contact angle with water.
- means the difference in contact angle with water before and after the contact of the liquid composition of the present invention. That is, the contact angle ⁇ B refers to the contact angle with respect to water at the site after contact with the liquid composition of the present invention and then washed, and the contact angle ⁇ A is a liquid for measuring the contact angle ⁇ B.
- part before making it contact with a composition. Specifically, it is a contact angle measured by the measurement method described in the examples described later.
- is caused by the amount of the surface treatment agent adsorbed on the inner wall of the accommodating portion.
- a large difference means that the surface treatment agent adsorbed on the inner wall of the housing portion is large, and the stability over time (storage stability) is poor.
- is 15 degrees or less because the concentration of the surface treatment agent in the liquid composition decreases during storage, resulting in a surface such as water repellency of the liquid composition. This is preferable from the viewpoint of suppressing a reduction in the reforming effect.
- is more preferably 10 degrees or less, and further preferably 7 degrees or less.
- is small from the viewpoint of the temporal stability (storage stability) without the decrease in the concentration of the surface treatment agent due to storage.
- is preferably 3 ° or more, more preferably 4 ° or more, and further preferably 5 ° or more. preferable.
- At least a portion of the inner wall of the housing portion that is in contact with the liquid composition of the present invention preferably has good wettability, so that the contact angle ⁇ C with respect to the liquid composition of the present invention is 90 degrees. It is preferable that it is less than. More preferably, the contact portion has a contact angle ⁇ C with respect to the liquid composition of the present invention of 75 degrees or less, and more preferably 25 degrees or less. In addition, the contact portion is ideally a contact angle ⁇ C with respect to the liquid composition of the present invention is 0 degree or more, but may be a measurement limit value or more.
- the value of the above contact angle ⁇ C indicates that the non-aqueous organic solvent tends to get wet with respect to the inner wall of the housing part, in other words, the inner wall of the housing part is hydrophobic.
- the inner wall of the accommodating portion has a small interaction with water, it is presumed that it is difficult to adsorb moisture, and even if moisture is adsorbed, it is easy to desorb. In other words, it is estimated that moisture is hardly retained. Therefore, since there is almost no moisture brought into the liquid composition from the inner wall of the housing portion, it is possible to suppress deterioration in performance such as water repellency due to water mixing into the liquid composition during storage.
- the storage container of the present invention includes, in one form, a storage section that stores the processing liquid of the present invention and a seal section that seals the storage section.
- the inner wall of the housing portion that contacts the treatment liquid of the present invention is, in one form, at least a part selected from at least one selected from polyethylene, polypropylene, polytetrafluoroethylene, and perfluoroalkoxyalkane. It is preferable that it is formed from the material to contain.
- “at least a part” means, for example, a lining, a lining layer, a laminate layer, a sealing material used for a joint portion, a lid, a viewing window, etc. formed from other materials. The idea is that it may be.
- the inner wall of the accommodating portion that contacts the treatment liquid of the present invention in one embodiment, is made of a material containing at least one member selected from stainless steel, hastelloy, inconel and monel. Preferably it is formed.
- “at least a part” means, for example, a lining, a lining layer, a laminate layer, a sealing material used for a joint portion, a lid, a viewing window, etc. formed from other materials. The idea is that it may be.
- the ratio of the voids in the container containing the liquid composition of the present invention (hereinafter also referred to as “void ratio”) is 40 to 0.01% by volume. Is preferred.
- the upper limit value of the porosity in the accommodating portion is more preferably 35 to 1% by volume, and further preferably 30 to 5% by volume.
- the container of the present invention preferably has a moisture concentration in a gas that occupies a void portion of the container containing the liquid composition of the present invention in a range of 0.01 mass ppt to 1 mass ppm.
- the water concentration is more preferably 0.01 mass ppt to 50 mass ppb, and still more preferably 0.01 mass ppt to 1 mass ppb.
- the liquid composition of the present invention is used for forming a water-repellent protective film on a wafer having an uneven pattern on the surface.
- a wafer having an uneven pattern on the surface is often obtained by the following procedure. First, after applying a resist to the surface of a smooth wafer, the resist is exposed through a resist mask, and a resist having a desired concavo-convex pattern is obtained by etching and removing the exposed resist portion or the unexposed resist portion. Is made. Moreover, the resist which has an uneven
- the wafer having a concavo-convex pattern on the surface for example, it is preferable that at least a part of the concavo-convex pattern is a wafer containing a silicon element.
- a layer containing silicon such as silicon, polysilicon, amorphous silicon, silicon oxide, or silicon nitride, germanium (Ge), or a low dielectric constant (k value) of 2.4 or less is provided on the wafer surface.
- At least a part of the surface of the concavo-convex pattern is silicon element such as silicon, polysilicon, amorphous silicon, silicon oxide, or silicon nitride. And a material containing germanium (Ge) or a low dielectric constant material having a k value of 2.4 or less.
- the wafer having a concavo-convex pattern on the surface may be a wafer composed of a plurality of layers.
- at least one layer is a layer containing silicon such as silicon, polysilicon, amorphous silicon, silicon oxide, or silicon nitride, or germanium (Ge) or dielectric constant (k value).
- Si silicon, polysilicon, amorphous silicon, silicon oxide, or silicon nitride, or germanium (Ge) or dielectric constant (k value).
- k value dielectric constant
- the material containing Ge is not limited to a material composed only of Ge, and may be, for example, a composite compound material of Ge and Si. Specifically, Si 0.5 Ge 0.5, and the like Si 0.15 Ge 0.85.
- Examples of the low dielectric constant material having a k value of 2.4 or less include BDIII (Low-k) material manufactured by Advanced Materials Technology.
- the k value can be measured with Four Dimensions, Inc., CMmap92B (trade name) (http://www.oyama-web.com/guide4/sub25.htm) and the like.
- the wafer composed of the plurality of components is at least one selected from a material containing silicon, polysilicon, amorphous silicon, silicon oxide, silicon nitride, Ge, and a low dielectric constant material having a k value of 2.4 or less.
- a material containing silicon, polysilicon, amorphous silicon, silicon oxide, silicon nitride, Ge on at least a part of the surface of the concavo-convex pattern Also included are those in which at least one selected from low dielectric constant materials having a k value of 2.4 or less is exposed.
- a protective film is easily formed on the surface of the portion including the material in the concavo-convex pattern.
- the reactive site of the silane compound reacts with the silanol group that is the reaction site of the wafer.
- the silane compound is chemically bonded to the silicon element of the silicon wafer through a siloxane bond.
- the reactive site may be decomposed or deteriorated by water to reduce the reactivity. Therefore, the silane compound as the surface treatment agent needs to reduce contact with water.
- the preparation, filling, storage, and analytical measurement of the treatment liquid were all performed in a clean room that satisfies ISO class 2 or lower.
- the ultrapure water used below is purified by the method described in JP-A-2007-254168, and the content of each of Fe, Cu and Zn is based on the total mass of each treatment liquid. After confirming that it was less than 10 mass ppt, it was used for the adjustment of the treatment liquid.
- the organic solvent used in the following was a semiconductor grade used for semiconductor production, purified using a distillation tower whose inner wall was made of glass. The purification of the organic solvent was repeated until the content of each of Fe, Cu and Zn in each treatment liquid finally obtained was less than 10 mass ppt with respect to the total mass of each treatment liquid.
- Treatment liquids B to M Treatment liquids B to F and H to M shown in Table 1 were prepared by a method according to the preparation method of the treatment liquid A described above. Moreover, the process liquid G using the organic solvent which has not performed moisture removal was prepared.
- treatment liquids B-1 to B-11 In order to evaluate the influence of the content of the particulate metal derived from the metal impurities (Cu, Fe, and Zn) contained in the treatment liquid, treatment liquids B-1 to B-11 shown in Table 5 were prepared.
- the organic solvent propylene glycol monomethyl ether acetate (PGMEA) is changed to PGMEA having a different degree of purification with respect to the treatment liquid B shown in Table 1.
- the degree of purification of PGMEA was adjusted by mixing PGMEA after purification used in treatment liquid B and PGMEA before purification at an arbitrary ratio.
- PE A container in which the inner wall of the container is polyethylene (PE).
- PP A container in which the inner wall of the container is polypropylene (PP).
- PTFE A container in which the inner wall of the container is polytetrafluoroethylene (PTFE).
- PTFE coating A container in which the inner wall of the container is coated with PTFE.
- PFA A container in which the inner wall of the container is perfluoroalkoxyalkane (PFA).
- Electropolished stainless steel 1 A stainless steel (SUS316L) container in which the inner wall of the container is electropolished.
- Electropolished stainless steel 2 A container made by reducing the treatment current density in electropolishing with respect to electropolished stainless steel 1.
- Electropolishing stainless steel 3 Compared with electropolishing stainless steel 1, the processing current density in electropolishing is lowered to a processing current density condition between the processing current density condition of electropolishing stainless steel 1 and the processing current density condition of electropolishing stainless steel 2.
- Container Container.
- Electropolishing stainless steel 4 A container made by reducing the treatment current density in electropolishing with respect to electropolishing stainless steel 2.
- Electropolishing stainless steel 5 A container made by reducing the treatment current density in electropolishing with respect to electropolishing stainless steel 4.
- Buffed stainless steel Stainless steel (SUS316L) container in which the inner wall of the container is buffed.
- Electropolishing Hastelloy A Hastelloy container with the inner wall of the container electropolished.
- Electro-polished Inconel An inconel container in which the inner wall of the container is electropolished.
- Electropolishing monel A container for monel whose inner wall is electropolished.
- Z-1 A storage container prepared by the method described in the example (paragraph 0037) of JP-A-2014-148332. (A container body made of polyethylene terephthalate, a treated surface formed by plasma etching on the inner wall surface of the container body, and a storage container coated with a hydrophobic silicon film covering the treated surface).
- Z-2 manufactured by changing the plasma etching processing time from 10 minutes (60 times in 10 seconds) to 8 minutes (48 times in 10 seconds) in the example (paragraph 0037) of JP 2014-148332 A Storage container.
- Z-3 manufactured by changing the plasma etching processing time from 10 minutes (60 times in 10 seconds) to 6 minutes (36 times in 10 seconds) in the example (paragraph 0037) of JP2014-148332A Storage container.
- Nitrogen gas A moisture concentration is 0.01 mass ppm / L
- Nitrogen gas B moisture concentration is 0.5 mass ppm / L
- Nitrogen gas C moisture concentration is 10 mass ppm / L
- Argon gas moisture concentration of 1 mass ppm / L
- Atmosphere Water concentration exceeds 100 mass ppm / L
- the internal volume of the accommodating part was calculated from the increase in mass when 100% of ultrapure water was filled.
- the adjustment of the porosity exceeding 1% was performed by obtaining the solution mass to be filled from the volume of the solution having a desired porosity and the specific gravity of the solution, and adjusting the filling amount by the increase in mass.
- the adjustment of the minute porosity of 1% or less was performed by filling the solution with 100% and sucking an amount of the solution corresponding to the volume of the gas having a desired porosity with a clean dropper.
- a wafer formed with a clean flat film for evaluation made of each material of SiC, SiO 2 or SiN was prepared.
- a pretreatment was performed with 5% by mass of hydrofluoric acid (HF).
- a beaker test was performed using the wafer after the pretreatment. Specifically, first, treatment solutions A to M shown in Table 1 were prepared, and each treatment solution at room temperature was prepared in a beaker. The wafer was immersed in each processing solution for 5 minutes while stirring each processing solution in the beaker at 250 rpm. The wafer thus brought into contact with each processing solution was rinsed with 40 ° C. isopropyl alcohol (IPA) for 30 seconds and dried with the nitrogen gas A. The temperature during drying was 20 ° C. (room temperature).
- IPA isopropyl alcohol
- the change rate of the contact angle ⁇ before and after storage was calculated according to the following formula and evaluated according to the following criteria. The smaller the change rate, the better the water repellency of the treatment liquid and the better the storage stability of the treatment liquid stored in the container.
- Change rate of contact angle ⁇ after storage ((Contact angle ⁇ of water repellency evaluation before storage ⁇ contact angle ⁇ of water repellency evaluation after storage) ⁇ contact angle ⁇ of water repellency evaluation before storage) ⁇ 100
- the change rate of the contact angle ⁇ before and after storage was calculated according to the following formula and evaluated according to the following criteria. The smaller the change rate, the better the water repellency of the treatment liquid and the better the storage stability of the treatment liquid stored in the container.
- Change rate of contact angle ⁇ after storage ((Contact angle ⁇ of water repellency evaluation before storage ⁇ contact angle ⁇ of water repellency evaluation after storage) ⁇ contact angle ⁇ of water repellency evaluation before storage) ⁇ 100
- Change rate of contact angle ⁇ after storage ((Contact angle ⁇ of water repellency evaluation before storage ⁇ contact angle ⁇ of water repellency evaluation after storage) ⁇ contact angle ⁇ of water repellency evaluation before storage) ⁇ 100
- a test piece of the inner wall member of the container was prepared, washed with ultrapure water, washed again with IPA, and sufficiently dried. About 2 ⁇ l of ultrapure water is placed (dropped) on the surface of the test piece, and the angle between the ultrapure water and the test piece surface (contact angle) is a contact angle meter (“DM-701” manufactured by Kyowa Interface Science Co., Ltd.) Measured with The contact angle measured here was theta A.
- DM-701 manufactured by Kyowa Interface Science Co., Ltd.
- test piece that was not used for the above measurement was immersed in the prepared treatment solution at 20 ° C. for 1 minute. Then, it was immersed in isopropanol (IPA) for 1 minute, and then immersed in ultrapure water as an aqueous cleaning solution for 1 minute. Finally, the test piece was taken out from the ultrapure water and air was blown to remove the pure water on the surface.
- IPA isopropanol
- SP-ICP-MS uses a PFA coaxial nebulizer, quartz cyclone spray chamber, quartz 1 mm inner diameter torch injector, and sucks the liquid to be measured at approximately 0.2 mL / min. did.
- the oxygen addition amount was 0.1 L / min, the plasma output was 1600 W, and cell purge with ammonia gas was performed.
- the time resolution was 50 us.
- the amount of ionic metal and the amount of particulate metal, and the total amount of metal, which is the sum of the amount of ionic metal and the amount of particulate metal, were measured using the following analysis software attached to the manufacturer.
- ⁇ Total amount of metal Syngistix for ICP-MS software
- Example 9 For each of Example 1, Example 9, and Example 21, Table 2 is similarly applied except that the wafer is changed from each material of SiC, SiO 2, or SiN from the following ⁇ A> to ⁇ E>.
- Table 2 is similarly applied except that the wafer is changed from each material of SiC, SiO 2, or SiN from the following ⁇ A> to ⁇ E>.
- ⁇ A> Poly-Si SEH AMERICA.
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Abstract
Description
そして、上述したパターン倒れの問題を解決するために、予め基板表面に撥水性保護膜を形成することにより、洗浄又はリンス時にパターンに作用する液体の表面張力を小さくする技術が知られている(例えば、特開2010-114414号公報、特開2010-192878号公報、特開2010-192879号公報、特開2010-272852号公報、特開2013-108044号公報等を参照)。
[1]
水分濃度が400質量ppm以下の有機溶媒と、表面処理剤とを含有する液体組成物が収容された収容部を具備する収容容器であって、上記収容部の内壁における少なくとも上記液体組成物に接触する部位は、水に対する接触角θが10度以上150度以下である収容容器。
上記表面処理剤がシラン化合物である、[1]に記載の収容容器。
上記表面処理剤がシリル化剤である、[1]は[2]に記載の収容容器。
上記液体組成物が撥水性保護膜形成用組成物である、[1]~[3]のいずれかに記載の収容容器。
上記収容部の内壁における上記液体組成物に接触する上記部位は、上記液体組成物に接触した後における水に対する接触角をθBとし、上記接触前における水に対する接触角をθAとしたときの接触角の差|θB-θA|が、3度以上15度以下である、[1]~[4]のいずれかに記載の収容容器。
上記収容部の内壁における上記液体組成物に接触する上記部位は、上記液体組成物に対する接触角θCが90度未満である、[1]~[5]のいずれかに記載の収容容器。
上記有機溶媒の水分濃度が200質量ppm以下である、[1]~[6]のいずれかに記載の収容容器。
上記有機溶媒の水分濃度が0.01質量ppt~100質量ppmである、[1]~[7]のいずれかに記載の収容容器。
上記液体組成物が収容された上記収容部における空隙部の割合が40~0.01体積%である、[1]~[8]のいずれかに記載の収容容器。
上記液体組成物が収容された上記収容部における空隙部を占める気体中の水分濃度が0.01質量ppt~1質量ppmである、[1]~[9]のいずれかに記載の収容容器。
上記液体組成物は、Cu、Fe及びZnからなる金属種から選択される1種又は2種以上の金属原子を含有し、上記金属原子の少なくとも1種を含む粒子性メタルの合計の含有率が、上記液体組成物の全質量を基準として、0.01~100質量pptである、[1]~[10]のいずれかに記載の収容容器。
上記粒子性メタルの質量が、SP-ICP-MS法により測定されたものである、[11]に記載の収容容器。
上記収容部の内壁における上記液体組成物に接触する部位の少なくとも一部が、ポリテトラフルオロエチレン、ペルフルオロアルコキシアルカン、ポリエチレン及びポリプロピレンから選択される少なくとも1種を含有する材料から形成される、[1]~[12]のいずれかに記載の収容容器。
上記収容部の内壁における上記液体組成物に接触する部位の少なくとも一部が、ステンレス、ハステロイ、インコネル、モネルから選択される少なくとも1種を含有する材料から形成される、[1]~[13]のいずれかに記載の収容容器。
上記表面処理剤は、下記一般式[1]で表されるシリル化剤である、[1]~[14]のいずれかに記載の収容容器。
(R1)aSi(H)bX1 4-a-b [1]
式中、
R1は、一部または全ての水素原子がフッ素原子に置き換えられていてもよい炭素数1~18の炭化水素基を含む1価の有機基を表す。R1が複数存在する場合には、同一でも異なっていてもよい。
X1は、ケイ素原子と結合する原子が窒素原子である1価の置換基、ケイ素原子と結合する原子が酸素原子である1価の置換基、ハロゲン原子、ニトリル基、および、-CO-NH-Si(CH3)3からなる群から選ばれる基又は原子を表す。X1が複数存在する場合には、同一でも異なっていてもよい。
aは1~3の整数、bは0~2の整数であり、aとbの合計は1~3である。
水分濃度が400質量ppm以下の有機溶媒と、表面処理剤とを含有する液体組成物の保管方法であって、内壁の少なくとも一部が、水に対する接触角θが10度以上150度以下である部材から構成されている収容部を有する収容容器に上記液体組成物を収容することを含む、液体組成物の保管方法。
上記表面処理剤がシラン化合物である、[16]に記載の液体組成物の保管方法。
上記表面処理剤がシリル化剤である、[16]又は[17]に記載の液体組成物の保管方法。
上記液体組成物が撥水性保護膜形成用組成物である、[16]~[18]のいずれか1項に記載の液体組成物の保管方法。
上記収容部の内壁における上記液体組成物に接触する上記部位は、上記液体組成物に接触する前における水に対する接触角をθAとし、上記液体組成物に接触した後における水に対する接触角をθBとしたときの接触角の差|θB-θA|が、3度以上15度以下である、[16]~[19]のいずれかに記載の液体組成物の保管方法。
上記収容部の内壁における上記液体組成物に接触する上記部位は、上記液体組成物に対する接触角θCが90度未満である、[16]~[20]のいずれかに記載の液体組成物の保管方法。
上記有機溶媒の水分濃度が200質量ppm以下である、[16]~[21]のいずれかに記載の液体組成物の保管方法。
上記有機溶媒の水分濃度が0.01質量ppt~100質量ppmである、[16]~[22]のいずれかに記載の液体組成物の保管方法。
上記液体組成物が収容された上記収容部における空隙部の割合が40~0.01体積%である、[16]~[23]のいずれかに記載の液体組成物の保管方法。
上記液体組成物が収容された上記収容部における空隙部を占める気体中の水分濃度が0.01質量ppt~1質量ppmである、[16]~[24]のいずれかに記載の液体組成物の保管方法。
上記液体組成物は、Cu、Fe及びZnからなる金属種から選択される1種又は2種以上の金属原子を含有し、上記金属原子の少なくとも1種を含む粒子性メタルの合計の含有率が、上記液体組成物の全質量を基準として、0.01~100質量pptである、[16]~[25]のいずれかに記載の液体組成物の保管方法。
上記粒子性メタルの質量が、SP-ICP-MS法により測定されたものである、[26]に記載の液体組成物の保管方法。
上記収容部の内壁における上記液体組成物に接触する部位の少なくとも一部が、ポリテトラフルオロエチレン、ペルフルオロアルコキシアルカン、ポリエチレン及びポリプロピレンから選択される少なくとも1種を含有する材料から形成される、[16]~[27]のいずれかに記載の液体組成物の保管方法。
上記収容部の内壁における上記液体組成物に接触する部位の少なくとも一部が、ステンレス、ハステロイ、インコネル、モネルから選択される少なくとも1種を含有する材料から形成される、[16]~[28]のいずれかに記載の液体組成物の保管方法。
上記表面処理剤は、下記一般式[1]で表されるシリル化剤である、[16]~[29]のいずれかに記載の液体組成物の保管方法。
(R1)aSi(H)bX1 4-a-b [1]
式中、
R1は、一部または全ての水素原子がフッ素原子に置き換えられていてもよい炭素数1~18の炭化水素基を含む1価の有機基を表す。R1が複数存在する場合には、同一でも異なっていてもよい。
X1は、ケイ素原子と結合する原子が窒素原子である1価の置換基、ケイ素原子と結合する原子が酸素原子である1価の置換基、ハロゲン原子、ニトリル基、および、-CO-NH-Si(CH3)3からなる群から選ばれる基又は原子を表す。X1が複数存在する場合には、同一でも異なっていてもよい。
aは1~3の整数、bは0~2の整数であり、aとbの合計は1~3である。
また、本明細書における「(メタ)アクリレート」とは、「アクリレート及びメタクリレートの少なくとも1種」を意味する。また、「(メタ)アクリル酸」とは、「アクリル酸及びメタクリル酸の少なくとも1種」を意味する。
また、本明細書において「~」を用いて表される数値範囲は、「~」の前後に記載される数値を下限値および上限値として含む範囲を意味する。
以下、本発明の実施形態について詳細に説明する。
以下、液体組成物について説明し、次いで収容容器について説明する。
本発明の液体組成物は、上述の通り、半導体デバイスの製造工程において、撥水性付与等の表面改質用途に用いられるものであり、表面処理剤と非水有機溶媒とを含有する。本発明の液体組成物は、更に、酸又は塩基を含有していてもよい。
本発明の液体組成物に含有される、水分濃度が400質量ppm以下の有機溶媒(非水有機溶媒)としては、例えば、極めて水及び金属不純物の少ないグレードのものを使用することが好ましく、これを更に脱水、精製した非水有機溶媒を用いることが好ましい。
本発明の液体組成物において、非水有機溶媒は、2種以上併用してもよい。
本発明の液体組成物に含有される表面処理剤は、用途としては特に限定されないが、例えば物質表面の親疎水性を制御する用途に用いられる。
表面処理剤としては、例えば、アルキル化剤、シラン化合物、アルミニウム系カップリング剤、チタネート系カップリング剤、ジルコネートカップリング剤、スズカップリング剤、及びアルミン酸ジルコニウムカップリング剤などが挙げられる。なかでも、半導体装置の製造工程における表面処理用途では、シラン化合物を用いることがより好ましい。ここで、シラン化合物とは、分子内に、水素-ケイ素結合、又は、炭素-ケイ素結合をもつ化合物であり、シリル化剤、シランカップリング剤等が具体例として挙げられる。本発明の液体組成物において、表面処理剤は2種以上併用してもよい。
上記アルキル化剤は、例えば、R7-Xで表わされる化合物であることが好ましい。この一般式において、R7は、水素原子、炭素数1~20のアルキル基、アリル基またはベンジル基を表し、Xは、フッ素原子、塩素原子、臭素原子、沃素原子、メシルオキシ基、トシルオキシ基またはトリフロロメチルスルフォニルオキシ基を表す。
上記シリル化剤は、下記一般式[1]で表されるケイ素含有化合物からなる群から選ばれる少なくとも1つであることが好ましい。
式中、
R1は、一部または全ての水素原子がフッ素原子に置き換えられていてもよい炭素数1~18の炭化水素基を含む1価の有機基を表す。R1が複数存在する場合には、同一でも異なっていてもよい。
X1は、ケイ素原子と結合する原子が窒素原子である1価の置換基、ケイ素原子と結合する原子が酸素原子である1価の置換基、ハロゲン原子、ニトリル基、および、-CO-NH-Si(CH3)3からなる群から選ばれる基又は原子を表す。X1が複数存在する場合には、同一でも異なっていてもよい。
aは1~3の整数、bは0~2の整数であり、aとbの合計は1~3である。
1又は2、iは0~2の整数)、クロロ原子、ブロモ原子、ヨード原子、ニトリル基、または、-CO-NH-Si(CH3)3に置き換えた化合物などが挙げられる。
上記シランカップリング剤は、下記一般式[2]で表されるケイ素含有化合物からなる群から選ばれる少なくとも1つであることが好ましい。
式中、
R1は、一部または全ての水素原子がフッ素原子に置き換えられていてもよい炭素数1~18の炭化水素基を含む1価の有機基を表す。R1が複数存在する場合には、同一でも異なっていてもよい。
Y1としては、炭素数1~12(特に好ましくは、炭素数1~10)のアルキル基、シクロアルキル基、アルケニル基、アリール基、アラルキル基などの非置換一価炭化水素基や、これらの基の水素原子の一部又は全部をハロゲン原子(塩素、フッ素、臭素原子等)、シアノ基、オキシエチレン基等のオキシアルキレン基、ポリオキシエチレン基等のポリオキシアルキレン基、(メタ)アクリル基、(メタ)アクリロキシ基、アクリロイル基、メタクリロイル基、メルカプト基、アミノ基、アミド基、ウレイド基、エポキシ基などの官能基で置換した置換一価炭化水素基、これら非置換又は置換一価炭化水素基において、酸素原子、NH基、NCH3基、NC6H5基、C6H5NH-基、H2NCH2CH2NH-基などが介在した基を挙げることができる。
aは1~3の整数、bは0~2の整数であり、aとbの合計は1~3である。
チタネート系カップリング剤としては、アミン系、亜リン酸型、ピロリン酸型、カルボン酸型等のチタネートカップリング剤が挙げられる。具体的には、例えば、イソプロピルトリイソステアロイルチタネート、イソプロピルトリドデシルベンゼンスルホニルチタネート、イソプロピルトリス(ジオクチルパイロホスフェート)チタネート、テトライソプロピルビス(ジオクチルホスファイト)チタネート、テトラオクチルビス(ジトリデシルホスファイト)チタネート、テトラ(2,2-ジアリルオキシメチル)ビス(ジトリデシル)ホスファイトチタネート、ビス(ジオクチルパイロホスフェート)オキシアセテートチタネート、ビス(ジオクチルパイロホスフェート)エチレンチタネート、イソプロピルトリオクタノイルチタネート、イソプロピルジメタクリルイソステアロイルチタネート、イソプロピルイソステアロイルジアクリルチタネート、イソプロピルトリ(ジオクチルホスフェート)チタネート、イソプロピルトリクミルフェニルチタネート、イソプロピルトリ(N-アミノエチル・アミノエチル)チタネート、ジクミルフェニルオキシアセテートチタネート、ジイソステアロイルエチレンチタネート等が挙げられる。
アルミニウム系カップリング剤としては例えば、アルミニウムイソプロピレート、モノsec-ブトキシアルミニウムジイソプロピレート、アルミニウムsec-ブチレート、アルミニウムエチレート、エチルアセトアセテエートアルミニウムジイソプロピレート、アルミニウムトリス(エチルアセトアセテート)、アルキルアセトアセテートアルミニウムジイソプロピレート、アルミニウムモノアセチルアセトネートビス(エチルアセトアセテート)、アルミニウムトリス(アセチルアセトアセテート)等を挙げることができる。
式中、R2は、一部または全ての水素原子がフッ素原子に置き換えられていても良い炭素数が1乃至18の1価の炭化水素基である。
式中、R3は、一部または全ての水素原子がフッ素原子に置き換えられていても良い炭素数が1乃至18の1価の炭化水素基である。
式中、
R4は、一部または全ての水素原子がフッ素原子に置き換えられていても良い炭素数が1乃至18の1価の炭化水素基である。R4が複数存在する場合には、同一でも異なっていてもよい。
式中、
R7は、一部または全ての水素原子がフッ素原子に置き換えられていても良い炭素数が1乃至18の1価の炭化水素基である。R7が複数存在する場合には、同一でも異なっていてもよい。
X3は、ケイ素原子と結合する原子が窒素原子であり、フッ素原子やケイ素原子を含んでいても良い1価の置換基である。X3が複数存在する場合には、同一でも異なっていてもよい。
eは1~3の整数であり、fは0~2の整数であり、eとfの合計は1~3である。
本発明の液体組成物は、異物の除去又は欠陥の低減などの目的で、フィルタで濾過することが好ましい。従来からろ過用途等に用いられているものであれば特に限定されることなく用いることができる。例えば、PTFE(ポリテトラフルオロエチレン)等のフッ素樹脂、ナイロン等のポリアミド系樹脂、ポリエチレン、ポリプロピレン(PP)等のポリオレフィン樹脂(高密度、超高分子量を含む)等によるフィルタが挙げられる。これら素材の中でもポリプロピレン(高密度ポリプロピレンを含む)及びナイロンが好ましい。フィルタの孔径は、0.001~1.0μm程度が適しており、好ましくは0.02~0.5μm程度、より好ましくは0.01~0.1μm程度である。この範囲とすることにより、ろ過詰まりを抑えつつ、処理液に含まれる不純物又は凝集物など、微細な異物を確実に除去することが可能となる。
本発明の液体組成物は、Na、Ca、Al、Cr、Co、Pb、Li、Mg、Mn、Ni、K、Agなどのイオン濃度がいずれも1ppm(parts per million)以下であることが好ましく、1ppb(parts per billion)以下であることがより好ましい。特に、pptオーダー(上記濃度はいずれも質量基準)であることが更に好ましく、実質的に含まないことが特に好ましい。
また、本発明の液体組成物は、粗大粒子を実質的に含まないことが好ましい。
なお、液体組成物に含まれる粗大粒子とは、原料に不純物として含まれる塵、埃、有機固形物、無機固形物などの粒子や、処理液の調製中に汚染物として持ち込まれる塵、埃、有機固形物、無機固形物などの粒子などであり、最終的に処理液中で溶解せずに粒子として存在するものが該当する。処理液中に存在する粗大粒子の量は、レーザを光源とした光散乱式液中粒子測定方式における市販の測定装置を利用して液相で測定することができる。
<液体組成物が収容された収容容器>
本発明は、上述した本発明の液体組成物が収容された収容部を具備する収容容器(以下、「本発明の収容容器」ともいう。)に関するものである。本発明の収容容器は、収容部の内壁における少なくとも本発明の液体組成物が接触する部位(以下において、「接触部位」ということがある。)は、水に対する接触角θが10度以上150度以下であることを第一の特徴とする。本発明の液体組成物がこのような収容容器に充填され保存された場合、撥水性等の性能の劣化を抑制することが可能となる。
本発明における接触角は、後掲の実施例で説明するθ/2法で測定した値である。
[処理液Aの調製]
脱水工程として、モレキュラーシーブ3A(ユニオン昭和製)を使用して、難燃性でありOH基を含有しない有機溶媒であるハイドロフルオロエーテル(3M製HFE-7100)に対して水分除去を施した。水分除去を施したHFE-7100の水分量は、カールフィッシャー式水分計(京都電子製、MKC-610-DT型)により測定を行ったところ、30質量ppmであった。
上述した処理液Aの調製方法に準じた方法で、表1に示す処理液B~F、H~Mを調製した。また、水分除去を施していない有機溶媒を使用した処理液Gを調製した。
処理液に含まれる金属不純物(Cu、Fe及びZn)に由来する粒子性メタルの含有率による影響を評価するため、表5に記載の処理液B-1~B-11を調製した。処理液B-1~B-11は、表1に記載の処理液Bに対し、有機溶媒のプロピレングリコールモノメチルエーテルアセテート(PGMEA)を、それぞれ精製度の異なるPGMEAに変更したものである。PGMEAの精製度は、処理液Bで使用した精製後のPGMEAと、精製前のPGMEAとを任意の割合で混合することにより調整した。
PGMEA:プロピレングリコールモノメチルエーテルアセテート
IPA:イソプロピルアルコール
<保管>
得られた各処理液を、表2~表5に記載の収容容器の収容部に充填した。各処理液を収容容器に充填する際、各表に記載の充填ガスで収容部の空隙部を充填した。
表2~表5に記載の収容容器は、下記の通りである。
PE:収容部の内壁がポリエチレン(PE)の収容容器。
PP:収容部の内壁がポリプロピレン(PP)の収容容器。
PTFE:収容部の内壁がポリテトラフルオロエチレン(PTFE)の収容容器。
PTFEコーティング:収容部の内壁がPTFEでコーティングされた収容容器。
PFA:収容部の内壁がペルフルオロアルコキシアルカン(PFA)の収容容器。
電解研磨ステンレス2:電解研磨ステンレス1に対し、電解研磨における処理電流密度を下げて作製した収容容器。
電解研磨ステンレス3:電解研磨ステンレス1に対し、電解研磨における処理電流密度を下げ、電解研磨ステンレス1の処理電流密度条件と、電解研磨ステンレス2の処理電流密度条件との間の処理電流密度条件にて作製した収容容器。
電解研磨ステンレス4:電解研磨ステンレス2に対し、電解研磨における処理電流密度を下げて作製した収容容器。
電解研磨ステンレス5:電解研磨ステンレス4に対し、電解研磨における処理電流密度を下げて作製した収容容器。
電解研磨ハステロイ:収容部の内壁が電解研磨されたハステロイの収容容器。
電解研磨インコネル:収容部の内壁が電解研磨されたインコネルの収容容器。
電解研磨モネル:収容部の内壁が電解研磨されたモネルの収容容器。
Z-3:特開2014-148332号公報の実施例(段落0037)において、プラズマエッチング処理時間を、10分(10秒で60回)から6分(10秒で36回)に変更して作製した収納容器。
窒素ガスA:水分濃度が0.01質量ppm/L
窒素ガスB:水分濃度が0.5質量ppm/L
窒素ガスC:水分濃度が10質量ppm/L
アルゴンガス:水分濃度が1質量ppm/L
大気:水分濃度が100質量ppm超/L
収容部の内容積は、超純水を100%充填したときの質量の増加量より算出した。1%を超える空隙率の調整は、所望の空隙率となる溶液の体積と溶液の比重から充填する溶液質量を求め、質量の増加量により充填量を調整して行った。1%以下の微量な空隙率の調整については、溶液を100%充填した後、所望の空隙率となる気体の体積に相当する量の溶液を清浄なスポイトで吸引して行った。
容器の内壁部材のテストピースを準備し、超純水で洗浄し、更にIPAで再度洗浄した後、十分に乾燥させた。このテストピース表面上に、超純水を約2μlを置き、超純水とテストピース表面とのなす角(接触角)θを接触角計(協和界面科学社製「DM-701」)を用い、θ/2法により測定した。θ/2法では、図1に示す液体11の半径rと、高さhを求め、これらを下式に代入して求められる。
[処理液の撥水性評価]
SiC、SiO2またはSiNの各材料で構成された、評価用の清浄な平坦膜を形成したウェハを準備した。自然酸化膜を除去するため、5質量%のフッ化水素酸(HF)で下処理を行った。この下処理後のウェハを使用して、ビーカーテストを行った。具体的には、まず、表1に示す処理液A~Mを調製し、室温の各処理液をビーカー内に準備した。ビーカー内の各処理液を250rpmで攪拌しながら、ウェハを5分間各処理液中に浸漬させた。このようにして各処理液に接触させたウェハに対し、40℃のイソプロピルアルコール(IPA)にて30秒間リンス処理を施し、上記窒素ガスAで乾燥した。乾燥時の温度は、20℃(室温)とした。
B:接触角αが75°以上85°未満
C:接触角αが75°未満
調製した各処理液を、表2、表3に記載の収容容器に充填し、密閉状態且つ40℃の環境下で、2週間保管した後の処理液を用いて、上記撥水性評価と同様の評価を行った。なお、基板としては、表2に記載の実施例及び比較例の評価では、上記撥水性評価と同様の下処理を行ったSiCウェハ、SiO2ウェハ及びSiNウェハを用い、表3に記載の実施例の評価では、同様の下処理を行ったSiNウェハを用いた。
((保管前の撥水性評価の接触角α-保管後の撥水性評価の接触角α)÷保管前の撥水性評価の接触角α)×100
A:変化率が±5%以内
B:変化率が±5%超え±10%以内
C:変化率が±10%超え±15%以内
D:変化率が±15%超え
調製した処理液を、表4、表5に記載の収容容器に充填し、密閉状態且つ50℃の環境下で、30日間保管した後の処理液を用いて、上記撥水性評価と同様の評価を行った。なお、基板としては、上記撥水性評価と同様の下処理を行ったSiNウエハを用いた。
((保管前の撥水性評価の接触角α-保管後の撥水性評価の接触角α)÷保管前の撥水性評価の接触角α)×100
A:変化率が±5%以内
B:変化率が±5%超え±10%以内
C:変化率が±10%超え±15%以内
D:変化率が±15%超え
調製した処理液を、表4、表5に記載の収容容器に充填し、密閉状態且つ50℃の環境下で、3日間保管した後、処理液を取り出し、新しい処理液に入れ替えた。この操作を10回繰り返し、10回目の保管後の処理液を用いて、上記撥水性評価と同様の評価を行った。なお、基板としては、上記撥水性評価と同様の下処理を行ったSiNウエハを用いた。
保管前の接触角αに対する10回目の保管後の接触角αの変化率を算出し、以下の基準で評価を行った。変化率が小さいほど、容器を繰り返し使用しても、処理液の保管性能が劣化せず、収容容器のリサイクル性に優れる。
((保管前の撥水性評価の接触角α-保管後の撥水性評価の接触角α)÷保管前の撥水性評価の接触角α)×100
A:変化率が±7%以内
B:変化率が±7%超え±14%以内
C:変化率が±14%超え±20%以内
D:変化率が±20%超え
上記基準において、評価Cは、半導体製造工程における撥水性保護膜形成用処理液として要求されるレベルを達成している。
容器の内壁部材のテストピースを準備し、超純水で洗浄し、更にIPAで再度洗浄した後、十分に乾燥させた。このテストピース表面上に、超純水 約2μlを置き(滴下し)、超純水とテストピース表面とのなす角(接触角)を接触角計(協和界面科学社製「DM-701」)で測定した。ここで測定された接触角をθAとした。
容器の内壁部材のテストピースを準備し、超純水で洗浄し、更にIPAで再度洗浄した後、十分に乾燥させた。このテストピース表面上に、各処理液を約2μlを置き、各処理液とテストピース表面とのなす角(接触角θc)を、接触角計(協和界面科学社製「DM-701」)を用い、θ/2法により測定した。結果を表3に示す。
下記方法により、表5に記載の処理液に含有される総メタル含有率及び粒子性メタル含有率を測定した。結果を同表に示す。
清浄なガラス容器内へ超純水を計量投入し、メディアン径50nmの測定対象金属粒子を10000個/mlの濃度となるように添加した後、超音波洗浄機で30分間処理した分散液を輸送効率測定用の標準物質として用いた。
メーカー:PerkinElmer
型式:NexION350S
3)SP-ICP-MSの測定条件
SP-ICP-MSはPFA製同軸型ネブライザ、石英製サイクロン型スプレーチャンバ、石英製内径1mmトーチインジェクタを用い、測定対象液を約0.2mL/minで吸引した。酸素添加量は0.1L/min、プラズマ出力1600W、アンモニアガスによるセルパージを行った。時間分解能は50usにて解析を行った。
・イオン性メタル量と粒子性メタル量: ナノ粒子分析“SP-ICP-MS”専用Syngistix ナノアプリケーションモジュール
・総メタル量: Syngistix for ICP-MS ソフトウエア
<A> Poly-Si S.E.H AMERICA.
<B> Si0.5Ge0.5 Advanced materials technology Si/SiGe
<C> Si0.15Ge0.85 Advanced materials technology Si/SiGe
<D> Ge KST world corp. Si/Ge
<E> BDIII(Low-k) Advanced materials technology Bare Si/BDIII(k値は~2.2)
Claims (30)
- 水分濃度が400質量ppm以下の有機溶媒と、表面処理剤とを含有する液体組成物が収容された収容部を具備する収容容器であって、前記収容部の内壁における少なくとも前記液体組成物に接触する部位は、水に対する接触角θが10度以上150度以下である収容容器。
- 前記表面処理剤がシラン化合物である、請求項1に記載の収容容器。
- 前記表面処理剤がシリル化剤である、請求項1又は2に記載の収容容器。
- 前記液体組成物が撥水性保護膜形成用組成物である、請求項1~3のいずれか1項に記載の収容容器。
- 前記収容部の内壁における前記液体組成物に接触する前記部位は、前記液体組成物に接触した後における水に対する接触角をθBとし、前記接触前における水に対する接触角をθAとしたときの接触角の差|θB-θA|が、3度以上15度以下である、請求項1~4のいずれか1項に記載の収容容器。
- 前記収容部の内壁における前記液体組成物に接触する前記部位は、前記液体組成物に対する接触角θCが90度未満である、請求項1~5のいずれか1項に記載の収容容器。
- 前記有機溶媒の水分濃度が200質量ppm以下である、請求項1~6のいずれか1項に記載の収容容器。
- 前記有機溶媒の水分濃度が0.01質量ppt~100質量ppmである、請求項1~7のいずれか1項に記載の収容容器。
- 前記液体組成物が収容された前記収容部における空隙部の割合が40~0.01体積%である、請求項1~8のいずれか1項に記載の収容容器。
- 前記液体組成物が収容された前記収容部における空隙部を占める気体中の水分濃度が0.01質量ppt~1質量ppmである、請求項1~9のいずれか1項に記載の収容容器。
- 前記液体組成物は、Cu、Fe及びZnからなる金属種から選択される1種又は2種以上の金属原子を含有し、前記金属原子の少なくとも1種を含む粒子性メタルの合計の含有率が、前記液体組成物の全質量を基準として、0.01~100質量pptである、請求項1~10のいずれか1項に記載の収容容器。
- 前記粒子性メタルの質量が、SP-ICP-MS法により測定されたものである、請求項11に記載の収容容器。
- 前記収容部の内壁における前記液体組成物に接触する部位の少なくとも一部が、ポリテトラフルオロエチレン、ペルフルオロアルコキシアルカン、ポリエチレン及びポリプロピレンから選択される少なくとも1種を含有する材料から形成される、請求項1~12のいずれか1項に記載の収容容器。
- 前記収容部の内壁における前記液体組成物に接触する部位の少なくとも一部が、ステンレス、ハステロイ、インコネル、モネルから選択される少なくとも1種を含有する材料から形成される、請求項1~13のいずれか1項に記載の収容容器。
- 前記表面処理剤は、下記一般式[1]で表されるシリル化剤である、請求項1~14のいずれか1項に記載の収容容器。
(R1)aSi(H)bX1 4-a-b [1]
式中、
R1は、一部または全ての水素原子がフッ素原子に置き換えられていてもよい炭素数1~18の炭化水素基を含む1価の有機基を表す。R1が複数存在する場合には、同一でも異なっていてもよい。
X1は、ケイ素原子と結合する原子が窒素原子である1価の置換基、ケイ素原子と結合する原子が酸素原子である1価の置換基、ハロゲン原子、ニトリル基、および、-CO-NH-Si(CH3)3からなる群から選ばれる基又は原子を表す。X1が複数存在する場合には、同一でも異なっていてもよい。
aは1~3の整数、bは0~2の整数であり、aとbの合計は1~3である。 - 水分濃度が400質量ppm以下の有機溶媒と、表面処理剤とを含有する液体組成物の保管方法であって、内壁の少なくとも一部が、水に対する接触角θが10度以上150度以下である部材から構成されている収容部を有する収容容器に前記液体組成物を収容することを含む、液体組成物の保管方法。
- 前記表面処理剤がシラン化合物である、請求項16に記載の液体組成物の保管方法。
- 前記表面処理剤がシリル化剤である、請求項16又は17に記載の液体組成物の保管方法。
- 前記液体組成物が撥水性保護膜形成用組成物である、請求項16~18のいずれか1項に記載の液体組成物の保管方法。
- 前記収容部の内壁における前記液体組成物に接触する前記部位は、前記液体組成物に接触する前における水に対する接触角をθAとし、前記液体組成物に接触した後における水に対する接触角をθBとしたときの接触角の差|θB-θA|が、3度以上15度以下である、請求項16~19のいずれか1項に記載の液体組成物の保管方法。
- 前記収容部の内壁における前記液体組成物に接触する前記部位は、前記液体組成物に対する接触角θCが90度未満である、請求項16~20のいずれか1項に記載の液体組成物の保管方法。
- 前記有機溶媒の水分濃度が200質量ppm以下である、請求項16~21のいずれか1項に記載の液体組成物の保管方法。
- 前記有機溶媒の水分濃度が0.01質量ppt~100質量ppmである、請求項16~22のいずれか1項に記載の液体組成物の保管方法。
- 前記液体組成物が収容された前記収容部における空隙部の割合が40~0.01体積%である、請求項16~23のいずれか1項に記載の液体組成物の保管方法。
- 前記液体組成物が収容された前記収容部における空隙部を占める気体中の水分濃度が0.01質量ppt~1質量ppmである、請求項16~24のいずれか1項に記載の液体組成物の保管方法。
- 前記液体組成物は、Cu、Fe及びZnからなる金属種から選択される1種又は2種以上の金属原子を含有し、前記金属原子の少なくとも1種を含む粒子性メタルの合計の含有率が、前記液体組成物の全質量を基準として、0.01~100質量pptである、請求項16~25のいずれか1項に記載の液体組成物の保管方法。
- 前記粒子性メタルの質量が、SP-ICP-MS法により測定されたものである、請求項26に記載の液体組成物の保管方法。
- 前記収容部の内壁における前記液体組成物に接触する部位の少なくとも一部が、ポリテトラフルオロエチレン、ペルフルオロアルコキシアルカン、ポリエチレン及びポリプロピレンから選択される少なくとも1種を含有する材料から形成される、請求項16~27のいずれか1項に記載の液体組成物の保管方法。
- 前記収容部の内壁における前記液体組成物に接触する部位の少なくとも一部が、ステンレス、ハステロイ、インコネル、モネルから選択される少なくとも1種を含有する材料から形成される、請求項16~28のいずれか1項に記載の液体組成物の保管方法。
- 前記表面処理剤は、下記一般式[1]で表されるシリル化剤である、請求項16~29のいずれか1項に記載の液体組成物の保管方法。
(R1)aSi(H)bX1 4-a-b [1]
式中、
R1は、一部または全ての水素原子がフッ素原子に置き換えられていてもよい炭素数1~18の炭化水素基を含む1価の有機基を表す。R1が複数存在する場合には、同一でも異なっていてもよい。
X1は、ケイ素原子と結合する原子が窒素原子である1価の置換基、ケイ素原子と結合する原子が酸素原子である1価の置換基、ハロゲン原子、ニトリル基、および、-CO-NH-Si(CH3)3からなる群から選ばれる基又は原子を表す。X1が複数存在する場合には、同一でも異なっていてもよい。
aは1~3の整数、bは0~2の整数であり、aとbの合計は1~3である。
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JP2013138178A (ja) * | 2011-11-29 | 2013-07-11 | Central Glass Co Ltd | 保護膜形成用薬液の調製方法 |
Cited By (3)
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CN112888641A (zh) * | 2018-10-12 | 2021-06-01 | 中央硝子株式会社 | 液体组合物的保存方法及产品 |
WO2022054620A1 (ja) * | 2020-09-08 | 2022-03-17 | 富士フイルム株式会社 | 薬液の供給方法、パターン形成方法 |
WO2023136042A1 (ja) * | 2022-01-17 | 2023-07-20 | 富士フイルム株式会社 | 薬液、修飾基板の製造方法、積層体の製造方法、薬液収容体 |
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TWI781939B (zh) | 2022-11-01 |
KR102306472B1 (ko) | 2021-09-29 |
JPWO2017217320A1 (ja) | 2019-03-14 |
JP6866368B2 (ja) | 2021-04-28 |
US11155717B2 (en) | 2021-10-26 |
US20190112489A1 (en) | 2019-04-18 |
TW201821583A (zh) | 2018-06-16 |
TW202302808A (zh) | 2023-01-16 |
KR20190008942A (ko) | 2019-01-25 |
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