WO2023136081A1 - 薬液、修飾基板の製造方法、積層体の製造方法 - Google Patents

薬液、修飾基板の製造方法、積層体の製造方法 Download PDF

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Publication number
WO2023136081A1
WO2023136081A1 PCT/JP2022/047376 JP2022047376W WO2023136081A1 WO 2023136081 A1 WO2023136081 A1 WO 2023136081A1 JP 2022047376 W JP2022047376 W JP 2022047376W WO 2023136081 A1 WO2023136081 A1 WO 2023136081A1
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group
chemical solution
salt
specific
polar
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English (en)
French (fr)
Japanese (ja)
Inventor
旺弘 袴田
篤史 水谷
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Fujifilm Corp
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Fujifilm Corp
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Priority to KR1020247022871A priority Critical patent/KR20240122816A/ko
Priority to JP2023573947A priority patent/JPWO2023136081A1/ja
Publication of WO2023136081A1 publication Critical patent/WO2023136081A1/ja
Priority to US18/774,832 priority patent/US20240368753A1/en
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • H10P14/40—Formation of materials, e.g. in the shape of layers or pillars of conductive or resistive materials
    • H10P14/42—Formation of materials, e.g. in the shape of layers or pillars of conductive or resistive materials using a gas or vapour
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    • H10P14/40—Formation of materials, e.g. in the shape of layers or pillars of conductive or resistive materials
    • H10P14/42—Formation of materials, e.g. in the shape of layers or pillars of conductive or resistive materials using a gas or vapour
    • H10P14/43—Chemical deposition, e.g. chemical vapour deposition [CVD]
    • H10P14/432—Chemical deposition, e.g. chemical vapour deposition [CVD] using selective deposition
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    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
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    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H10P14/61—Formation of materials, e.g. in the shape of layers or pillars of insulating materials using masks
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    • H10P50/00—Etching of wafers, substrates or parts of devices
    • H10P50/20—Dry etching; Plasma etching; Reactive-ion etching
    • H10P50/28—Dry etching; Plasma etching; Reactive-ion etching of insulating materials
    • H10P50/282—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials
    • H10P50/283—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials by chemical means
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    • H10W20/45—Interconnections external to wafers or substrates, e.g. back-end-of-line [BEOL] metallisations or vias connecting to gate electrodes characterised by their insulating parts
    • H10W20/48—Insulating materials thereof
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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    • H10P76/00—Manufacture or treatment of masks on semiconductor bodies, e.g. by lithography or photolithography

Definitions

  • the present invention relates to a chemical liquid, a method for manufacturing a modified substrate, and a method for manufacturing a laminate.
  • Patent Document 1 discloses a composition containing a corrosion inhibitor. The corrosion inhibitor forms an insoluble film on the surface of copper to prevent corrosion of copper while preventing removal of other members. It states that it has been done.
  • a film formed on a region formed of a specific material is required to exhibit a high water contact angle depending on the treatment to be performed.
  • a specific material for example, a metal region
  • an object of the present invention to provide a chemical solution for manufacturing semiconductors that can form a film exhibiting a high water contact angle on a metal region when brought into contact with a substrate having a metal region.
  • Another object of the present invention is to provide a method for manufacturing a modified substrate and a method for manufacturing a laminate using the chemical solution.
  • the present inventor has completed the present invention as a result of diligent studies aimed at solving the above problems. That is, the inventors have found that the above problems can be solved by the following configuration.
  • a chemical solution for semiconductor manufacturing containing a solvent and two or more specific compounds A chemical solution for manufacturing a semiconductor, wherein the specific compound is a compound having a polar group and a vertical alignment group.
  • the polar group is selected from the group consisting of a nitrogen-containing group, a phosphoric acid group or a salt thereof, a phosphonic acid group or a salt thereof, a sulfo group or a salt thereof, a carboxyl group or a salt thereof, a thiol group, and a hydroxy group;
  • the chemical solution comprises a first specific compound having the nitrogen-containing group as the polar group and the vertical alignment group, and a second specific compound having the polar group other than the nitrogen-containing group and the vertical alignment group.
  • the chemical solution according to [1] or [2], comprising: [4] The chemical solution according to [3], wherein the polar group of the second specific compound is a phosphonic acid group or its salt, a carboxyl group or its salt, or a thiol group.
  • the third chemical liquid has the polar group selected from the group consisting of a nitrogen-containing group, a phosphonic acid group or a salt thereof, a carboxyl group or a salt thereof, and a thiol group, and the vertical alignment group.
  • a chemical solution for semiconductor manufacturing containing a solvent and two or more specific compounds A chemical liquid for manufacturing a semiconductor, wherein the above-mentioned specific compound has a specific group selected from the group consisting of a polar group, a hydrocarbon group which may have a halogen atom, and a polyoxyalkylene group.
  • the polar group is selected from the group consisting of a nitrogen-containing group, a phosphoric acid group or a salt thereof, a phosphonic acid group or a salt thereof, a sulfo group or a salt thereof, a carboxyl group or a salt thereof, a thiol group, and a hydroxy group;
  • the chemical solution according to [6], which is one or more groups that are [8] The chemical solution contains a fourth specific compound having the nitrogen-containing group that is the polar group and the specific group, and a fifth specific compound having the polar group other than the nitrogen-containing group and the specific group, [ 6] or the chemical solution according to [7].
  • a substrate having a metal region is brought into contact with the chemical solution according to any one of [1] to [15] to form a film containing the above two or more specific compounds on the metal region.
  • a method for manufacturing a modified substrate comprising a step of obtaining a modified substrate by [17] The step includes bringing the chemical solution into contact with the substrate, heating the substrate in contact with the chemical solution, and performing a rinsing treatment on the heated substrate, thereby forming the chemical solution on the metal region.
  • the method for producing a modified substrate according to [16] which is a step of obtaining a modified substrate including a film containing two or more specific compounds.
  • a method for manufacturing a laminate comprising: [19] The method for producing a laminate according to [18], further comprising the step of removing the film containing the two or more specific compounds formed on the metal region.
  • the present invention it is possible to provide a chemical solution for manufacturing a semiconductor that can form a film exhibiting a high water contact angle on a metal region when brought into contact with a substrate having a metal region.
  • a method for manufacturing a modified substrate and a method for manufacturing a laminate using the chemical solution it is also possible to provide a method for manufacturing a modified substrate and a method for manufacturing a laminate using the chemical solution.
  • a numerical range represented by “to” means a range including the numerical values before and after “to” as lower and upper limits.
  • the bonding direction of a divalent group e.g., -COO-
  • Y in a compound represented by "XYZ” is -COO-
  • the compound may be either “X—O—CO—Z” or “X—CO—O—Z”.
  • the chemical solution for semiconductor manufacturing of the present invention contains a solvent and two or more specific compounds.
  • a first embodiment of the chemical liquid contains a compound having a polar group and a vertical alignment group (hereinafter also referred to as “compound 1”) as the specific compound.
  • a second embodiment of the chemical liquid is a compound having a specific group selected from the group consisting of a polar group, a hydrocarbon group optionally having a halogen atom, and a polyoxyalkylene group as the specific compound (hereinafter , also referred to as “compound 2”).
  • the mechanism by which the chemical solution of the present invention (first and second embodiments) can form a film exhibiting a high water contact angle on a metal region when brought into contact with a substrate having a metal region is not necessarily
  • the chemical solution of the present invention contains a specific compound, and since the specific compound has a polar group, when it is brought into contact with a substrate having a metal region, the polar group of the specific compound tends to adsorb to the surface of the metal region.
  • the specific compound since the specific compound has a vertical alignment group or a specific group, the specific compound is arranged substantially perpendicular to the surface of the metal region, and a dense film containing the specific compound is likely to be formed.
  • the chemical solution of the present invention contains two or more specific compounds, thereby facilitating the formation of a denser film containing the specific compounds.
  • the specific compound tends to arrange the polar groups toward the surface side of the metal region, and a dense film is formed.
  • a film can be formed that exhibits a contact angle.
  • a film formed on a metal region and exhibiting a high water contact angle when brought into contact with a substrate having a metal region is also referred to as a "high contact angle film”. is simply referred to as "larger contact angle”.
  • a first embodiment of the chemical solution of the present invention comprises a solvent and two or more specific compounds. Also, as described above, the specific compound is Compound 1.
  • a first embodiment of the drug solution of the present invention comprises a solvent. However, even if it is a solvent, it is not included in the solvent if it corresponds to the specific compound described in detail later.
  • Solvents include water and organic solvents. Examples of organic solvents include hydrocarbon solvents, alcohol solvents, polyol solvents, glycol ether solvents, ether solvents, ketone solvents, amide solvents, sulfur-containing solvents, and ester solvents. .
  • hydrocarbon solvents examples include aliphatic hydrocarbon solvents such as n-pentane and n-hexane; alicyclic hydrocarbon solvents such as cyclohexane and methylcyclohexane; aromatic solvents such as toluene and xylene. Examples include hydrocarbon solvents.
  • alcohol solvents examples include methanol, ethanol, 1-propanol, 2-propanol (also referred to as isopropyl alcohol (IPA)), 2-butanol, isobutyl alcohol, tert-butyl alcohol, isopentyl alcohol, and 4- Aliphatic alcohol solvents having 1 to 18 carbon atoms such as methyl-2-pentanol (also referred to as methyl isobutylcarbinol (MIBC)); Alicyclic alcohol solvents having 3 to 18 carbon atoms such as cyclohexanol; benzyl aromatic alcohol solvents such as alcohol; ketone alcohol solvents such as diacetone alcohol; The number of carbon atoms in the alcohol solvent is preferably 1-8, more preferably 2-7, and even more preferably 3-6.
  • IPA isopropyl alcohol
  • MIBC methyl isobutylcarbinol
  • Alicyclic alcohol solvents having 3 to 18 carbon atoms such as cyclohexanol
  • polyol solvents examples include glycol solvents having 2 to 18 carbon atoms.
  • Glycol-based solvents include ethylene glycol, propylene glycol (1,2-propanediol), 1,3-propanediol, diethylene glycol, and dipropylene glycol.
  • Glycol ether solvents include, for example, glycol monoether solvents having 3 to 19 carbon atoms.
  • glycol monoether solvents include ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol mono-n-propyl ether, ethylene glycol mono-isopropyl ether, ethylene glycol mono-n-butyl ether, diethylene glycol monomethyl ether, and diethylene glycol monoethyl ether.
  • the number of carbon atoms in the glycol ether solvent is preferably 1-8, more preferably 2-7, and even more preferably 3-6.
  • Ketone solvents include, for example, acetone, methyl ethyl ketone, methyl isobutyl ketone, and cyclohexanone.
  • ether solvents include diethyl ether, diisopropyl ether, dibutyl ether, t-butyl methyl ether, cyclohexyl methyl ether, and tetrahydrofuran.
  • amide solvents include formamide, monomethylformamide, dimethylformamide, acetamide, monomethylacetamide, dimethylacetamide, monoethylacetamide, diethylacetamide, and N-methylpyrrolidone.
  • sulfur-containing solvents examples include dimethylsulfone, dimethylsulfoxide, and sulfolane.
  • ester-based solvents examples include n-butyl acetate, ethyl lactate, propylene glycol acetate, propylene glycol monomethyl ether acetate, ⁇ -butyrolactone, and ⁇ -valerolactone.
  • an organic solvent is preferable, and an alcohol solvent is more preferable.
  • the content of the solvent in the chemical solution is preferably 90 to 99.9% by mass, more preferably 95 to 99.9% by mass, and 97 to 99.5% by mass, relative to the total mass of the chemical solution. % is more preferred.
  • Two or more solvents may be used in combination. When two or more solvents are used in combination, the total content is preferably within the above range.
  • a first embodiment of the drug solution of the present invention comprises two or more specific compounds.
  • Compound 1 is mentioned as a specific compound. That the chemical contains two or more specific compounds means that the chemical contains two or more specific compounds having different structures. Structurally different means that the structures of the two specific compounds are not the same, for example, the types of polar groups in the two specific compounds are different, and the vertically aligned groups in the two specific compounds are of different types. The polar group and the vertical alignment group are described below.
  • the polar group of the specific compound is a polarized group, preferably a group that interacts with atoms on the surface of the metal region.
  • the polar groups are nitrogen-containing groups, phosphoric acid groups (—PO 4 H 2 ) or salts thereof, phosphonic acid groups (—PO 3 H 2 ) or salts thereof, in that they can interact with the surface atoms of the metal region.
  • Nitrogen-containing groups include primary amino groups (-NH 2 ), secondary amino groups (-NR T H), tertiary amino groups (-NR T 2 ), and quaternary ammonium groups (- N + R T 3 ).
  • R 1 T represents an alkyl group having 1 to 3 carbon atoms, and plural R 1 Ts may be different from each other. Also, a plurality of RTs may be bonded to each other to form a ring.
  • the ring to be formed is a ring containing a nitrogen atom, and examples thereof include a pyrrolidine ring, a piperidine ring, a piperazine ring and the like.
  • the nitrogen-containing group may be a nitrogen-containing heteroaryl group, and the nitrogen-containing heteroaryl group may be monocyclic or polycyclic.
  • Nitrogen-containing heteroaryl groups include pyridyl, triazine, pyrrole, pyrazole, imidazole, pyrazole, triazole, benzimidazole, and benztriazole groups.
  • a salt of a phosphate group refers to a group represented by —PO 4 2- Ct n+ 2/n .
  • Ct n+ represents an n-valent cation, and n represents 1 or 2.
  • Monovalent cations include Li + , Na + , K + , NH 4 + and the like. When Ct n+ represents a monovalent cation, its number is two.
  • Divalent cations include Mg + , Ca + and the like. When Ct n+ represents a divalent cation, its number is one.
  • a compound having a phosphoric acid group is also referred to as a "phosphate compound", and the functional group name is also referred to as "-phosphoric acid”.
  • a salt of a phosphonic acid group refers to a group represented by —PO 3 2- Ct n+ 2/n .
  • Ct n+ represents an n-valent cation, where n represents 1 or 2.
  • the same cations as the cations described above for the salt of the phosphate group can be mentioned, and the numbers thereof are also the same.
  • a compound having a phosphonic acid group is also referred to as a "phosphonic acid compound".
  • a sulfo group salt refers to a group represented by —SO 3 —Ct + .
  • Ct + represents a monovalent cation, and examples thereof include the same monovalent cations as described for the salt of the phosphate group.
  • a salt of a carboxy group refers to a group represented by —COO ⁇ Ct + .
  • Ct + represents a monovalent cation, and examples thereof include the same monovalent cations as described for the salt of the phosphate group.
  • Polar groups are, inter alia, in terms of their larger contact angles, primary amino groups, secondary amino groups, tertiary amino groups, quaternary ammonium groups, phosphate groups, phosphonic acid groups, sulfo groups,
  • One or more groups selected from the group consisting of carboxy groups, thiol groups and hydroxy groups are preferred and selected from the group consisting of primary amino groups, phosphonic acid groups, carboxy groups, thiol groups and hydroxy groups. are more preferred, and one or more groups selected from the group consisting of primary amino groups, phosphonic acid groups, carboxy groups, and thiol groups are even more preferred.
  • the number of polar groups possessed by the specific compound is preferably 1 to 4, more preferably 1 or 2, and even more preferably 1. As will be described later, when the vertical alignment group has a linear structure, the polar group possessed by the specific compound is preferably bonded to the end of the linear structure.
  • the vertical alignment group possessed by the specific compound causes the specific compound itself to adhere to the surface of the metal region when a chemical solution containing the specific compound is brought into contact with a substrate having a metal region to form a film containing the specific compound on the metal region. It refers to a group that has the function of aligning in the direction perpendicular to the surface.
  • the vertically oriented group is not particularly limited, a group selected from the group consisting of a hydrocarbon group optionally having a halogen atom and a polyoxyalkylene group (hereinafter also referred to as "specific group") is preferable.
  • a hydrocarbon group an aliphatic hydrocarbon group is preferred, and an alkyl group is preferred.
  • the number of carbon atoms in the hydrocarbon group is not particularly limited, and is preferably 3-20, more preferably 6-20, and even more preferably 10-18.
  • the hydrocarbon group may have a halogen atom. When the hydrocarbon group has halogen atoms, the number of halogen atoms is not particularly limited, but is preferably 1-10, more preferably 1-5.
  • Halogen atoms include fluorine, chlorine, bromine and iodine atoms.
  • the hydrocarbon group is preferably linear.
  • the n-butyl and 3-chloro-n-butyl groups are linear and the isobutyl group is not linear.
  • a polyoxyalkylene group is a group having a plurality of oxyalkylene groups, and examples thereof include a polyoxyethylene group and a polyoxypropylene group.
  • the number of repeating units of the oxyalkylene group in the polyoxyalkylene group is not particularly limited, it is preferably 2-20, more preferably 3-10.
  • a compound represented by formula (A) is preferable.
  • X a represents a polar group
  • Y a represents a hydrocarbon group optionally having a halogen atom or a polyoxyalkylene group-containing group.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y a are vertical alignment groups.
  • the polar group represented by Xa is as described above.
  • the hydrocarbon group optionally having a halogen atom represented by Ya is as described above.
  • the hydrocarbon group represented by Y a is preferably an alkyl group which may have a halogen atom, more preferably a linear alkyl group which may have a halogen atom.
  • the polyoxyalkylene group-containing group represented by Ya is a group containing the polyoxyalkylene group described above.
  • a group represented by formula (B) is preferable.
  • Formula (B) —L—(R 1 —O) n —R 2 L represents a single bond or a divalent linking group.
  • the divalent linking group includes a hydrocarbon group (eg, alkylene group, arylene group), -O-, -S-, -CO-, -SO 2 -, -N(R 3 )-, or these Combined groups are included.
  • R3 represents a hydrogen atom or an alkyl group.
  • R 1 represents an alkylene group. The number of carbon atoms in the alkylene group is not particularly limited, preferably 1-5, more preferably 1-3. n represents an integer of 2 or more, preferably 2-20, more preferably 3-10.
  • R2 represents a hydrogen atom or an alkyl group. The number of carbon atoms in the alkyl group is not particularly limited, and is preferably 1-20.
  • the molecular weight of the specific compound contained in the first embodiment of the chemical solution is preferably 1000 or less, more preferably 600 or less, and even more preferably 300 or less.
  • the lower limit of the molecular weight is preferably 60 or more.
  • the said molecular weight means a weight average molecular weight.
  • at least one (preferably two or more) is a specific compound having the above preferred molecular weight range (e.g., 600 or less, or 300 or less). is preferred. It is also preferable that all of the specific compounds contained in the first embodiment of the chemical solution are specific compounds having the above preferred molecular weight range.
  • a first embodiment of the drug solution contains two or more specific compounds, as described above. Above all, it is preferable to satisfy the following requirement 1 or 2 in that the contact angle is larger.
  • Requirement 1 Includes a first specific compound having a polar nitrogen-containing group and a vertical alignment group, and a second specific compound having a polar group other than the nitrogen-containing group and a vertical alignment group.
  • Requirement 2 Two or more third specific compounds having a polar group selected from the group consisting of a nitrogen-containing group, a phosphonic acid group or its salt, a carboxyl group or its salt, and a thiol group, and a vertically aligned group and the polar groups in the two or more third specific compounds are the same.
  • the first specific compound is preferably a compound represented by formula (1).
  • Formula (1) X 1 -Y 1 X 1 represents a nitrogen-containing group, and Y 1 represents a hydrocarbon group optionally having a halogen atom or a polyoxyalkylene group-containing group.
  • the nitrogen-containing group represented by X 1 is a polar group, and the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 1 are vertically aligned groups.
  • the nitrogen-containing group represented by X1 is as described above.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 1 are respectively the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y a . is synonymous with group.
  • a compound represented by formula (2) is preferable.
  • Formula (2) X 2 -Y 2 X2 represents a polar group other than a nitrogen-containing group, and Y2 represents a hydrocarbon group optionally having a halogen atom or a polyoxyalkylene group-containing group.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 2 are vertical alignment groups.
  • the polar group other than the nitrogen-containing group represented by X 2 is a group other than the nitrogen-containing group exemplified above as the polar group. groups or salts thereof, carboxy groups or salts thereof, thiol groups and hydroxy groups.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 2 are the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Ya , respectively. is synonymous with group.
  • Y 1 and Y 2 may be different or the same may be When Y 1 and Y 2 are different, both are hydrocarbon groups which may have a halogen atom, and the difference in the number of carbon atoms between the two hydrocarbon groups is preferably 6 or more.
  • the polar group possessed by the second specific compound is preferably a phosphonic acid group or a salt thereof, a carboxy group or a salt thereof, or a thiol group, and more preferably a carboxy group, a phosphonic acid group, or a thiol group.
  • the ratio of the content of the first specific compound to the total content of the specific compounds is preferably 10 to 90% by mass, more preferably 20 to 80% by mass.
  • the ratio of the content of the second specific compound to the total content of the specific compounds is preferably 10 to 90% by mass, more preferably 20 to 80% by mass.
  • X 3A -Y 3A represents a nitrogen-containing group, a phosphonic acid group or its salt, a carboxy group or its salt, and a polar group selected from the group consisting of a thiol group, and Y 3A may have a halogen atom. It represents a hydrocarbon group or a polyoxyalkylene group-containing group.
  • the nitrogen-containing group represented by X3A is as described above.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 3A are vertical alignment groups.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 3A are the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Ya , respectively. is synonymous with group.
  • Formula (3B) X 3B -Y 3B X 3B represents a nitrogen-containing group, a phosphonic acid group or its salt, a carboxy group or its salt, and a polar group selected from the group consisting of a thiol group, and Y 3B may have a halogen atom. It represents a hydrocarbon group or a polyoxyalkylene group-containing group.
  • the nitrogen-containing group represented by X3B is as described above.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y3B are vertical alignment groups.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 3B are the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Ya , respectively. is synonymous with group.
  • the polar groups possessed by the third specific compound are the same. That is, when the third specific compound A represented by formula (3A) and the third specific compound B represented by formula (3B) are included, X 3A and X 3B are the same, and Y 3A and Y 3B is different.
  • Y 3A and Y 3B are different, both are hydrocarbon groups which may have a halogen atom, and the difference in the number of carbon atoms between the two hydrocarbon groups is preferably 6 or more.
  • the ratio of the content of the third specific compound A to the total content of the specific compounds is preferably 10 to 90% by mass, more preferably 20 to 80% by mass.
  • the ratio of the content of the third specific compound B to the total content of the specific compounds is preferably 10 to 90% by mass, more preferably 20 to 80% by mass.
  • the number of carbon atoms in the vertically aligned group in the third specific compound A (preferably the number of carbon atoms in the hydrocarbon group optionally having a halogen atom represented by Y 3A in formula (3A)) is , the number of carbon atoms in the vertically aligned group in the third specific compound B (preferably the number of carbon atoms in the hydrocarbon group which may have a halogen atom represented by Y 3B in formula (3B))
  • the ratio of the content of the third specific compound A to the total content of the specific compounds is 10 to 30% by mass.
  • the content of the specific compound is preferably 0.01 to 10.0% by mass, more preferably 0.1 to 5.0% by mass, more preferably 0.1 to 5.0% by mass, relative to the total mass of the chemical solution. 5 to 3.0% by mass is more preferable.
  • the first embodiment of the chemical solution may contain other components than those mentioned above.
  • Other components include polymers.
  • Polymers include acrylic polymers, siloxane polymers, and styrenic polymers. Specific examples of the polymer include polymers described in paragraphs [0150] to [0171] of JP-A-2021-041364.
  • a second embodiment of the chemical solution of the present invention comprises a solvent and two or more specific compounds. Moreover, as described above, the specific compound is Compound 2.
  • the aspect (kind, content, etc.) of the solvent contained in the second embodiment of the chemical liquid is the same as the aspect of the solvent contained in the first embodiment of the chemical liquid, so the description is omitted.
  • a second embodiment of the drug solution of the present invention comprises two or more specific compounds.
  • Compound 2 is mentioned as a specific compound. That the chemical contains two or more specific compounds means that the chemical contains two or more specific compounds having different structures. Structurally different means that the structures of two specific compounds are not the same, for example, the types of polar groups in the two specific compounds are different, and the types of specific groups in the two specific compounds are different. Since the type of polar group in the specific compound contained in the second embodiment of the chemical solution is the same as the type of polar group in the specific compound contained in the first embodiment of the chemical solution, description thereof will be omitted.
  • the specific compound contained in the second embodiment of the chemical liquid has a specific group selected from the group consisting of a hydrocarbon group optionally having a halogen atom and a polyoxyalkylene group.
  • the definition and preferred aspects of the hydrocarbon group optionally having a halogen atom are the definition and preferred aspects of the hydrocarbon group optionally having a halogen atom, which is an example of the vertical alignment group possessed by the specific compound described above. is the same as , so the description is omitted.
  • the definition and preferred aspects of the polyoxyalkylene group are the same as the definition and preferred aspects of the polyoxyalkylene group, which is an example of the vertical alignment group of the specific compound, and thus description thereof is omitted.
  • a compound represented by formula (C) is preferable.
  • Formula (C) Xc - Yc Xc represents a polar group
  • Yc represents a hydrocarbon group optionally having a halogen atom or a polyoxyalkylene group-containing group.
  • the polar group represented by Xc is as described above.
  • the hydrocarbon group optionally having a halogen atom represented by Yc is as described above.
  • the definition and preferred aspects of the polyoxyalkylene group-containing group represented by Yc are the same as the definition and preferred aspects of the polyoxyalkylene group-containing group represented by Ya , and thus description thereof is omitted.
  • the molecular weight of the specific compound contained in the second embodiment of the chemical solution is preferably 1000 or less, more preferably 600 or less, and even more preferably 300 or less.
  • the lower limit of the molecular weight is preferably 60 or more.
  • the said molecular weight means a weight average molecular weight.
  • at least one (preferably two or more) is a specific compound having the preferred molecular weight range (e.g., 600 or less, or 300 or less). is preferred. It is also preferable that all of the specific compounds contained in the second embodiment of the chemical solution are specific compounds having the above preferred molecular weight range.
  • a second embodiment of the drug solution contains two or more specific compounds, as described above. Above all, it is preferable to satisfy the following requirement 1 or 2 in that the contact angle is larger.
  • Requirement 3 Includes a fourth specific compound having a nitrogen-containing group and a specific group that are polar groups, and a fifth specific compound having a polar group and a specific group other than a nitrogen-containing group.
  • Requirement 4 Nitrogen-containing group, phosphonic acid group or its salt, carboxyl group or its salt, and a polar group selected from the group consisting of a thiol group, and two or more sixth specific compounds having a specific group, Two or more sixth specific compounds have the same polar group.
  • the compound represented by Formula (4) is preferable as the fourth specific compound.
  • Formula (4) X 4 -Y 4 X4 represents a nitrogen-containing group
  • Y4 represents a hydrocarbon group optionally having a halogen atom or a polyoxyalkylene group-containing group.
  • the nitrogen-containing group represented by X4 is as described above.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 4 are the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Ya , respectively. is synonymous with group.
  • a compound represented by formula (5) is preferable.
  • X 5 -Y 5 X5 represents a polar group other than a nitrogen-containing group, and Y5 represents a hydrocarbon group optionally having a halogen atom or a polyoxyalkylene group-containing group.
  • the polar group other than the nitrogen-containing group represented by X 5 is a group other than the nitrogen-containing group exemplified above as the polar group, such as a phosphoric acid group or a salt thereof, a phosphonic acid group or a salt thereof, a sulfo groups or salts thereof, carboxy groups or salts thereof, thiol groups and hydroxy groups.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 5 are the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Ya , respectively. is synonymous with group.
  • Y 4 and Y 5 may be different or the same may be When Y 4 and Y 5 are different, both are hydrocarbon groups which may have a halogen atom, and the difference in the number of carbon atoms between the two hydrocarbon groups is preferably 6 or more.
  • the polar group possessed by the fifth specific compound is preferably a phosphonic acid group or a salt thereof, a carboxy group or a salt thereof, or a thiol group, and more preferably a carboxy group, a phosphonic acid group, or a thiol group.
  • the ratio of the content of the fourth specific compound to the total content of the specific compounds is preferably 10 to 90% by mass, more preferably 20 to 80% by mass.
  • the ratio of the content of the fifth specific compound to the total content of the specific compounds is preferably 10 to 90% by mass, more preferably 20 to 80% by mass.
  • the sixth specific compound includes a sixth specific compound A represented by formula (6A) and a sixth specific compound B represented by formula (6B).
  • Formula (6A) X 6A -Y 6A X 6A represents a nitrogen-containing group, a phosphonic acid group or its salt, a carboxyl group or its salt, and a polar group selected from the group consisting of a thiol group, and Y 6A may have a halogen atom. It represents a hydrocarbon group or a polyoxyalkylene group-containing group.
  • the nitrogen-containing group represented by X6A is as described above.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y6A are specific groups.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 6A are the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Ya, respectively. is synonymous with group.
  • Formula (6B) X 6B -Y 6B X 6B represents a nitrogen-containing group, a phosphonic acid group or its salt, a carboxy group or its salt, and a polar group selected from the group consisting of a thiol group, and Y 6B may have a halogen atom.
  • the nitrogen-containing group represented by X6A is as described above.
  • the above optionally halogenated hydrocarbon group and polyoxyalkylene group-containing group represented by Y6B are specific groups.
  • the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Y 6B are the hydrocarbon group optionally having a halogen atom and the polyoxyalkylene group-containing group represented by Ya, respectively. is synonymous with group.
  • the polar groups possessed by the sixth specific compound are the same. That is, when the sixth specific compound A represented by formula (6A) and the sixth specific compound B represented by formula (6B) are included, X 6A and X 6B are the same, and Y 6A and Y 6B is different.
  • Y6A and Y6B are different, both are hydrocarbon groups which may have a halogen atom, and the difference in the number of carbon atoms between the two hydrocarbon groups is preferably 6 or more.
  • the ratio of the content of the sixth specific compound A to the total content of the specific compounds is preferably 10 to 90% by mass, more preferably 20 to 80% by mass.
  • the ratio of the content of the sixth specific compound B to the total content of the specific compounds is preferably 10 to 90% by mass, more preferably 20 to 80% by mass.
  • the number of carbon atoms in the specific group in the sixth specific compound A (preferably, the number of carbon atoms in the hydrocarbon group optionally having a halogen atom represented by Y6A in formula (6A)) is 6
  • the number of carbon atoms in the specific group in the specific compound B (preferably the number of carbon atoms in the hydrocarbon group optionally having a halogen atom represented by Y 6B in formula (6B)) is larger than the specific
  • the ratio of the content of the sixth specific compound A to the total content of the compounds is 10 to 30% by mass.
  • the content of the specific compound is preferably 0.01 to 10.0% by mass, more preferably 0.1 to 5.0% by mass, more preferably 0.1 to 5.0% by mass, relative to the total mass of the chemical liquid. 5 to 3.0% by mass is more preferable.
  • the second embodiment of the drug solution may contain other components than those mentioned above.
  • Other components include polymers.
  • Polymers include acrylic polymers, siloxane polymers, and styrenic polymers. Specific examples of the polymer include polymers described in paragraphs [0150] to [0171] of JP-A-2021-041364.
  • the manufacturing method of the chemical solution of the present invention (first embodiment and second embodiment) is not particularly limited, and for example, it can be manufactured by mixing each of the above components.
  • the order or timing of mixing each component, and the order and timing are not particularly limited.
  • a chemical solution can be produced by adding two or more specific compounds to a mixer such as a mixer containing a purified solvent and then sufficiently stirring the mixture.
  • the steps described below may be performed.
  • the production method may include a metal removal step of removing metal components from the components and/or the chemical solution (hereinafter also referred to as "substance to be purified").
  • the metal removal step include step P of subjecting the material to be purified to an ion exchange method.
  • step P the material to be purified is subjected to an ion exchange method.
  • the ion exchange method is not particularly limited as long as it is a method that can adjust (reduce) the amount of metal components in the substance to be purified.
  • one or more of methods P1-P3 are included. More preferably, the ion exchange method includes two or more of methods P1 to P3, and more preferably includes all of methods P1 to P3.
  • the order of implementation is not particularly limited, but it is preferable to carry out the methods P1 to P3 in that order.
  • Method P1 A method of passing the substance to be purified through a first filling section filled with a mixed resin containing two or more resins selected from the group consisting of a cation exchange resin, an anion exchange resin, and a chelate resin.
  • Method P2 Covering at least one of the second filling section filled with the cation exchange resin, the third filling section filled with the anion exchange resin, and the fourth filling section filled with the chelate resin A method of passing a purified product through a liquid.
  • Method P3 A method of passing the substance to be purified through a membrane ion exchanger.
  • the ion exchange resins (cation exchange resins, anion exchange resins), chelate resins, and membranous ion exchangers used in each method, if in a form other than H + form or OH - form, are H + form or It is preferably used after being regenerated to the OH - form.
  • the space velocity (SV) of the material to be purified in each method is preferably 0.01 to 20.0 (1/h), more preferably 0.1 to 10.0 (1/h).
  • the treatment temperature in each method is preferably 0 to 60.degree. C., more preferably 10 to 50.degree.
  • the forms of ion exchange resins and chelate resins include, for example, granular, fibrous, and porous monolithic forms, with granular or fibrous forms being preferred.
  • the average particle diameter of the granular ion exchange resin and chelate resin is preferably 10 to 2000 ⁇ m, more preferably 100 to 1000 ⁇ m.
  • the particle size distribution of the granular ion-exchange resin and chelate resin it is preferable that the proportion of resin particles in the range of ⁇ 200 ⁇ m of the average particle size is 90% or more.
  • the average particle size and particle size distribution can be measured, for example, by using a particle size distribution analyzer (Microtrac HRA3920, manufactured by Nikkiso Co., Ltd.) using water as a dispersion medium.
  • the ion exchange method is preferably carried out until the content of the metal components contained in the material to be purified falls within the preferred range of the content of the metal components described above.
  • the manufacturing method preferably includes a filtration step of filtering the liquid in order to remove foreign matter, coarse particles, and the like from the liquid.
  • the filtration method is not particularly limited, and known filtration methods can be used. Among them, filtering using a filter is preferable.
  • Filters used for filtering can be used without any particular limitation as long as they are conventionally used for filtering purposes.
  • Materials constituting the filter include, for example, fluorine-based resins such as PTFE (polytetrafluoroethylene), polyamide-based resins such as nylon, and polyolefin resins such as polyethylene and polypropylene (PP) (including high-density and ultra-high molecular weight). , and polyarylsulfones.
  • fluorine-based resins such as PTFE (polytetrafluoroethylene), polyamide-based resins such as nylon, and polyolefin resins such as polyethylene and polypropylene (PP) (including high-density and ultra-high molecular weight).
  • PP polypropylene
  • polyarylsulfones are preferred.
  • the lower limit is preferably 70 mN/m or more, and the upper limit is preferably 95 mN/m or less.
  • the critical surface tension of the filter is preferably 75-85 mN/m.
  • the critical surface tension value is the manufacturer's nominal value.
  • the pore size of the filter is preferably about 0.001-1.0 ⁇ m, more preferably about 0.02-0.5 ⁇ m, and even more preferably about 0.01-0.1 ⁇ m.
  • the filtering by the first filter may be performed only once, or may be performed twice or more.
  • the filters may be of the same type or of different types, but are preferably of different types.
  • the first filter and the second filter preferably differ in at least one of pore size and material of construction. It is preferable that the pore size in the second and subsequent filtering is the same as or smaller than the pore size in the first filtering. Also, the first filters having different pore diameters within the above range may be combined.
  • the pore size here can refer to the nominal value of the filter manufacturer.
  • the chemical solution manufacturing method may further include a static elimination step of neutralizing the chemical solution.
  • a known container can be used as the container for storing the chemical solution. It is preferable that the container has a high degree of cleanliness in the container for use in semiconductors and less elution of impurities.
  • Examples of containers include "Clean Bottle” series (manufactured by Aicello Chemical Co., Ltd.) and “Pure Bottle” (manufactured by Kodama Resin Industry).
  • the inner wall of the container is a multilayer container having a six-layer structure composed of six resins, or a multilayer container having a seven-layer structure composed of seven resins. It is also preferred to use a container.
  • multilayer containers examples include containers described in JP-A-2015-123351, the contents of which are incorporated herein.
  • Materials for the inner wall of the container include, for example, at least one first resin selected from the group consisting of polyethylene resin, polypropylene resin, and polyethylene-polypropylene resin, a second resin different from the first resin, stainless steel, and hastelloy. , Inconel, and Monel.
  • the inner wall of the container is preferably formed or coated using the above materials.
  • a fluorine resin (perfluoro resin) is preferable as the second resin.
  • a fluororesin is used, elution of oligomers of ethylene or propylene can be suppressed.
  • the container include FluoroPure PFA composite drum (manufactured by Entegris), page 4 of Japanese Patent Publication No. 3-502677, page 3 of International Publication No. 2004/016526, and International Publication No. 99/046309. No. 9 pamphlet and the container described on page 16 can be mentioned.
  • quartz and an electropolished metal material are also preferable other than the fluororesin.
  • the metal material used for the electrolytically polished metal material contains at least one selected from the group consisting of chromium (Cr) and nickel (Ni), and the total content of Cr and Ni is Preference is given to metallic materials that are more than 25% by weight relative to the total weight. Examples include stainless steel and Ni--Cr alloys.
  • the total content of Cr and Ni in the metal material is preferably 25% by mass or more, more preferably 30% by mass or more, relative to the total mass of the metal material.
  • the upper limit is preferably 90% by mass or less with respect to the total mass of the metal material.
  • stainless steel examples include known stainless steels. Among them, stainless steel containing 8% by mass or more of Ni is preferable, and austenitic stainless steel containing 8% by mass or more of Ni is more preferable.
  • Ni--Cr alloys include, for example, known Ni--Cr alloys. Among them, a Ni—Cr alloy having a Ni content of 40 to 75% by mass and a Cr content of 1 to 30% by mass is preferable.
  • the Ni—Cr alloy may further contain boron, silicon, tungsten, molybdenum, copper, or cobalt in addition to the above alloys, if necessary.
  • Examples of methods for electropolishing a metal material include known methods. Specifically, the methods described in paragraphs [0011] to [0014] of JP-A-2015-227501 and paragraphs [0036] to [0042] of JP-A-2008-264929 are mentioned. the contents of which are incorporated herein.
  • the metal material is preferably buffed.
  • Examples of the buffing method include known methods.
  • the size of the abrasive grains used for the buffing finish is preferably #400 or less because the unevenness of the surface of the metal material is likely to be smaller. Buffing is preferably performed before electropolishing.
  • the metal material may be processed by combining one or more of multiple stages of buffing, acid cleaning, magnetic fluid polishing, and the like, which are performed by changing the count such as the size of abrasive grains.
  • the inside of the container is preferably cleaned before being filled with the chemical solution.
  • the liquid used for washing can be appropriately selected according to the application, and liquid containing at least one of the chemical solution or the component added to the chemical solution is preferable.
  • the inside of the container may be replaced with an inert gas (for example, nitrogen and argon) with a purity of 99.99995% by volume or more in order to prevent changes in the components of the chemical solution during storage.
  • an inert gas for example, nitrogen and argon
  • a gas with a particularly low water content is preferred.
  • room temperature or temperature control may be used. Among them, it is preferable to control the temperature in the range of -20 to 20°C from the viewpoint of preventing deterioration.
  • the chemical solutions of the present invention are preferably used for processing substrates having metal regions.
  • the chemical solution of the present invention may be brought into contact with a substrate having a metal region.
  • a modified substrate is obtained in which a film (high contact angle film) containing two or more specific compounds contained in the chemical solution of the present invention is formed on a substrate having a metal region. A method for manufacturing the modified substrate will be described later.
  • a substrate with metal regions is a substrate with metal regions and other regions.
  • the metal region refers to a region whose surface is made of metal, and the other region refers to a region whose surface is made of something other than metal.
  • the metal constituting the metal region is not particularly limited, but is preferably a transition metal, more preferably a group 6 to 11 element, more preferably a group 6 element, a group 8 element, a group 9 element, or a group 11 element, ruthenium or Tungsten is particularly preferred.
  • the metal forming the metal region may be an alloy containing the above metals. Materials forming other regions include insulators, and insulators include oxides (eg, metal oxides, metal nitrides, SiO 2 , etc.). It is also preferred that the substrate with metal regions is a semiconductor substrate with metal regions.
  • the treatment preferably forms a high contact angle film on the substrate having the metal regions, and more preferably forms a high contact angle film only on the metal regions.
  • the high contact angle film preferably functions as a mask when forming a film on a substrate having a metal region by chemical vapor deposition (CVD). That is, in the region where the high contact angle film formed by the chemical solution of the present invention is formed, it is difficult to deposit a film by CVD (hereinafter also referred to as “CVD film”), and in the region where the high contact angle film is not formed, CVD is difficult.
  • a film is preferably deposited.
  • the high contact angle film functions as a mask for CVD, a laminate is obtained in which the CVD film is selectively formed on other regions on the substrate.
  • the contact angle of the high contact angle film is preferably 60° or more, more preferably 90° or more, and even more preferably 105° or more, because the high contact angle film can easily function as a mask for CVD.
  • the upper limit is not particularly limited, and is often 120° or less.
  • a modified substrate including a high contact cornea is preferably produced by bringing the chemical solution of the present invention into contact with a substrate having a metal region.
  • the high contact angle film is preferably formed only on the metal region. Further, the high contact angle film more preferably functions as a mask for CVD.
  • a modified substrate of a more preferred embodiment can be suitably applied to the production of a laminate.
  • the contact method is not particularly limited, and includes a method of applying or spraying a chemical solution onto a substrate having a metal region, and a method of immersing a substrate having a metal region in a chemical solution.
  • a method for applying the chemical solution to the substrate is not particularly limited, and a known method can be used, for example, spin coating. Further, when the substrate is immersed in the chemical, convection may be caused in the chemical.
  • the contact temperature is not particularly limited, but is preferably 10 to 50°C.
  • the substrate having the metal region it is also preferable to heat the substrate having the metal region after bringing the chemical solution into contact with the substrate.
  • the solvent contained in the chemical solution can be removed and the film containing the specific compound can be made denser.
  • the heating temperature is not particularly limited, 50 to 300°C is preferable, and 60 to 180°C is more preferable.
  • the heating method is not particularly limited, and includes a method of contacting with a heating element (for example, heating with a hot plate) and a method of irradiating with infrared rays.
  • the rinsing treatment can remove from the substrate the specific compound adhering to areas other than the desired area.
  • the rinsing method is not particularly limited, but includes a method of contacting the rinsing liquid with a heated substrate.
  • the contact method the same method as the method of contacting the chemical solution with the substrate having the metal region can be used.
  • the contact temperature is not particularly limited, but is preferably 10 to 50°C.
  • the rinsing liquid is not particularly limited, but includes the solvent contained in the chemical solution of the present invention. A solvent contained in the chemical liquid used for forming the high contact cornea may be used as the rinse liquid.
  • a laminate is obtained in which a CVD film is formed on regions where the high contact angle film is not formed (regions other than the metal regions).
  • the CVD process may be performed by a known technique, but thermal CVD, plasma CVD, or atomic layer deposition (ALD) is preferred, and ALD is more preferred.
  • ALD atomic layer deposition
  • a precursor which is the raw material for the CVD film, is supplied to the surface of the modified substrate. Materials constituting the CVD film to be formed can be controlled by the type of precursor to be supplied, the supply atmosphere, the oxidizing agent, and the like.
  • Materials for the formed CVD film are not particularly limited, and include metals, metal oxides and metal nitrides.
  • Metals include aluminum, titanium, chromium, iron, cobalt, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, ruthenium, palladium, lanthanum, cerium, hafnium, tantalum, tungsten, platinum, and bismuth. be done.
  • Metal oxides include aluminum oxide, titanium oxide, zinc oxide, zirconium oxide, hafnium oxide, and tantalum oxide.
  • Metal nitrides include titanium nitride and tantalum nitride. In the CVD process, a process for modifying the surface of the region where the high contact angle film is not formed may be performed.
  • the thickness of the CVD film on the region where the high contact angle film is not formed is compared with the thickness of the CVD film on the region where the high contact angle film is formed.
  • the film thickness ratio is preferably 0.75 or less, more preferably 0.5 or less, and even more preferably 0.25 or less.
  • the lower limit of the above ratio is 0, and may be 0. That is, the CVD film may not be formed on the region where the high contact angle film is formed.
  • the high contact angle film may be further removed.
  • a laminate is obtained in which the CVD film is formed only on the regions other than the metal regions.
  • a method for removing the high contact cornea is not particularly limited, but dry etching, wet etching, and combinations thereof may be used. Dry etching includes a method of supplying reactive ions or reactive radicals to the surface of a laminate having a high contact angle film. Reactive ions or reactive radicals may be generated by plasma or the like, and are preferably generated using a mixed gas containing one or more gases selected from the group consisting of oxygen, nitrogen and hydrogen. The mixed gas may contain a rare gas.
  • dry etching may be physical etching using a sputtering phenomenon.
  • Wet etching may be performed by supplying an etchant to the surface of the laminate having a high contact angle film.
  • the etchant include an etchant containing an oxidizing agent such as ozone, and an etchant containing an organic solvent.
  • the organic solvent of the etching solution containing an organic solvent include the organic solvents contained in the above chemical solutions, and hydrocarbon-based solvents are preferred.
  • ⁇ Evaluation method> According to the following procedure, a film containing two or more specific compounds (high contact angle film) was formed on a substrate using the chemical solutions of Examples and Comparative Examples, and the water contact angle of the film was evaluated. Further, the substrate on which the high contact angle film was formed was processed to form an oxide film by the ALD method, and the deposition selectivity was evaluated from the thickness of the formed oxide film.
  • a W layer wafer having a tungsten layer formed on one surface of a commercially available silicon wafer (12 inches in diameter) by CVD, and a Ru layer wafer having a ruthenium layer formed by CVD were prepared as substrates.
  • the CVD processing time was adjusted so that the thickness of the tungsten layer and the ruthenium layer was 20 nm.
  • the obtained W layer wafer and Ru layer wafer were cut into 2 cm squares and immersed in each chemical solution. Each wafer was immersed in the chemical while stirring the chemical in a container with a magnetic stirrer at 250 rpm, the temperature of the chemical was 25° C., and the immersion time was 10 minutes. As for the W layer wafer, the above immersion was performed after the following pretreatment was performed. The W layer wafer was immersed in a 1 mass % citric acid aqueous solution. The immersion in the citric acid aqueous solution was carried out while stirring the chemical in the container with a magnetic stirrer under the condition of 250 rpm, the temperature of the chemical was 25° C., and the immersion time was 1 minute. After the immersion, the W layer wafer was dried by blowing nitrogen gas.
  • heat treatment was performed on each wafer that had been immersed in the chemical solution.
  • the heat treatment was performed using a hot plate at a heating temperature of 120° C. and a heating time of 5 minutes.
  • the temperature of each wafer was set to 25° C. and then rinsed with isopropyl alcohol (IPA).
  • IPA isopropyl alcohol
  • the rinsing treatment is carried out by immersing the substrate after the heat treatment in IPA, and the immersion is performed while stirring the IPA in the container with a magnetic stirrer under the conditions of 250 rpm, the temperature of the IPA is 25 ° C., and the immersion time. was 30 seconds.
  • each wafer was dried by blowing nitrogen gas. By the above treatment, a high contact angle film was formed on each wafer to obtain a sample.
  • the water contact angle of the sample obtained by the above method was measured by the following method. The measurement was carried out at 23° C. using DMs-501 manufactured by Kyowa Interface Science Co., Ltd. The value was measured three times 500 milliseconds after the water droplet contacted the surface, and the average value was taken as the contact angle. In addition, the surface tension of water was analyzed as 72.9 mN/m. Based on the contact angle obtained by the above measurement, the contact angle was evaluated according to the following criteria. Evaluation of B or more is preferable practically.
  • ⁇ AA The contact angle of water is 105° or more ⁇ A: The contact angle of water is 90° or more and less than 105° ⁇ B: The contact angle of water is 60° or more and less than 90° ⁇ C: The contact angle of water is less than 60°
  • a sample was obtained in the same manner as for the above contact angle, ALD treatment was performed in the following procedure, and deposition selectivity was evaluated.
  • an aluminum oxide layer was formed on the obtained sample using an atomic layer deposition apparatus (AD-230LP manufactured by Samco). Trimethylaluminum was used as an organometallic raw material, and water was used as an oxidizing agent.
  • the ALD processing temperature was set to 150° C., and the ALD processing was performed on each sample under the condition that the film thickness was 5 nm for each wafer when the high contact angle film was not formed.
  • the film thickness of the aluminum oxide layer of each sample after the ALD treatment was measured using a spectroscopic ellipsometer (M-2000XI, manufactured by JA Woollam Japan Co., Ltd.). The film thickness was measured at 5 points on the sample, and the average value was taken as the film thickness. The measurement was performed with a measurement range of 1.2-2.5 eV and measurement angles of 70° and 75°. It should be noted that the smaller the film thickness, the more difficult it is to deposit a film by ALD processing.
  • Table 1 shows the chemical components and their proportions, the contact angle evaluation results, and the deposition selectivity evaluation results.
  • A-1 octadecylamine A-2: dodecylamine A-3: decylamine A-4: butylamine A-5: propylamine
  • B-1 octadecanoic acid
  • B-2 dodecanoic acid
  • C- 1 octadecylphosphonic acid
  • C-2 dodecylphosphonic acid
  • D-1 octadodecanol
  • E-1 octadecanethiol
  • ⁇ F-2 the following compound (molecular weight 677.06)
  • ⁇ F-3 the following compound (molecular weight 793.22)
  • ⁇ H-2 A polymer having the following structure described in paragraphs [0170] to [0171] of JP-A-2021-041364 The polymer having the following structure is described in paragraph [0170] of JP-A-2021-041364. Synthesized according to the method of The synthesized polymer having the following structure had a weight average molecular weight of 6,000 and a number average molecular weight of 5,600.
  • ⁇ H-3 A polymer having the following structure described in paragraphs [0164] to [0165] of JP-A-2021-041364
  • the polymer having the following structure is described in paragraph [0164] of JP-A-2021-041364 Synthesized according to the method of The synthesized polymer having the following structure had a weight average molecular weight of 5,100 and a number average molecular weight of 4,800.
  • Example 1 From the results in Table 1, it was found that the chemicals of the present invention (Examples 1 to 16) can form a film exhibiting a high water contact angle on a metal region when brought into contact with a substrate having a metal region. confirmed.
  • Comparative Examples 1 and 2 which do not contain the specific compound, did not exhibit the above effects.
  • Comparative Examples 3 and 4 which contain only one specific compound, did not exhibit the above effects.
  • the polar group possessed by the specific compound is one selected from the group consisting of a nitrogen-containing group, a phosphonic acid group, a carboxy group, and a thiol group. It was confirmed that the contact angle was larger in the case of the above groups.
  • Example 8 From a comparison between Examples 1 to 4, 7 and 12 and Example 8, it has a polar group selected from the group consisting of a nitrogen-containing group, a phosphonic acid group or its salt, a carboxyl group or its salt, and a thiol group. It was confirmed that when two or more third specific compounds were included and the polar groups of the two or more third specific compounds were the same, the contact angle was larger. From the comparison between Example 17 and Example 18, it was confirmed that when the molecular weight of one or more specific compounds among the specific compounds was 600 or less, the contact angle was larger.

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