WO2021153122A1 - 処理液、被処理物の処理方法 - Google Patents
処理液、被処理物の処理方法 Download PDFInfo
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- WO2021153122A1 WO2021153122A1 PCT/JP2020/048515 JP2020048515W WO2021153122A1 WO 2021153122 A1 WO2021153122 A1 WO 2021153122A1 JP 2020048515 W JP2020048515 W JP 2020048515W WO 2021153122 A1 WO2021153122 A1 WO 2021153122A1
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- 238000000034 method Methods 0.000 title claims abstract description 95
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- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims abstract description 58
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 37
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Images
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11D7/5022—Organic solvents containing oxygen
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
- G03F7/425—Stripping or agents therefor using liquids only containing mineral alkaline compounds; containing organic basic compounds, e.g. quaternary ammonium compounds; containing heterocyclic basic compounds containing nitrogen
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
- H01L21/02071—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a delineation, e.g. RIE, of conductive layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
- H01L21/32133—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only
- H01L21/32134—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only by liquid etching only
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0073—Anticorrosion compositions
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5013—Organic solvents containing nitrogen
Definitions
- the present invention relates to a treatment liquid and a method for treating an object to be treated.
- Patent Document 1 discloses a detergent composition containing N-hydroxyformamide and the like.
- a technique for treating an object to be processed composed of a substrate or the like using a treatment liquid is being studied.
- the treatment liquid used for such treatment of the object to be treated is excellent in, for example, the removability of organic residues generated by the treatment (dry etching treatment or the like) performed on the object to be processed in advance (hereinafter,). , Simply “excellent in organic residue removal”) is required. Further, the treatment liquid is also required to be able to achieve a certain performance even after a lapse of time, and is also required to be excellent in stability.
- Another object of the present invention is to provide a treatment liquid having excellent organic residue removing property and excellent stability. Another object of the present invention is to provide a method for treating an object to be treated with respect to the above-mentioned treatment liquid.
- [1] water and, With hydroxylamine Contains hydrazine, a hydrazine salt, and one or more hydrazines selected from the group consisting of hydrazine derivatives.
- [3] The treatment solution according to [1] or [2], wherein the total content of the hydrazines is 0.005 to 0.5 parts by mass with respect to 100 parts by mass of the hydroxylamine.
- the hydrazine derivative is one or more selected from the group consisting of a compound represented by the general formula (A), a compound represented by the general formula (B), a compound having a pyrazole ring, and salts thereof. ,
- the treatment liquid according to any one of [1] to [3].
- H 2 NN X (B)
- 2 two R N are each independently a hydrogen atom or a substituent. Two RNs may be combined with each other to form a ring. Provided that at least one of two R N, is other than a hydrogen atom.
- X represents a divalent group.
- [9] Furthermore, it contains one or more second anion selected from the group consisting of SO 4 2-and PO 4 3-,
- the treatment solution according to any one of [1] to [10] further containing a chelating agent.
- the chelating agents are diethylenetriaminetetraacetic acid, ethylenediaminetetraacetic acid, trans-1,2-diaminocyclohexanetetraacetic acid, oxalic acid, malonic acid, succinic acid, citric acid, methanesulfonic acid, 1-hydroxyethylidene-1,1-diphosphon.
- the benzotriazoles are an alkyl group which may further contain a substituent, an aryl group which may further contain a substituent, a halogen atom, an amino group which may further contain a substituent, a nitro group, and further substitutions.
- the anticorrosive agents are benzotriazole, 5-aminotetrazole, 1-hydroxybenzotriazole, 5-phenylthiol-benzotriazole, 5-chlorobenzotriazole, 4-chlorobenzotriazole, 5-bromobenzotriazole, 4-bromobenzotriazole.
- 5-Fluorobenzotriazole 4-Fluorobenzotriazole, Nafttriazole, Triltriazole, 5-Phenyl-benzotriazole, 5-Nitrobenzotriazole, 4-Nitrobenzotriazole, 3-Amino-5-mercapto-1,2, 4-Triazole, 2- (5-amino-pentyl) -benzotriazole, 1-amino-benzotriazole, 5-methyl-1H-benzotriazole, benzotriazole-5-carboxylic acid, 4-methylbenzotriazole, 4-ethyl Benzotriazole, 5-ethylbenzotriazole, 4-propylbenzotriazole, 5-propylbenzotriazole, 4-isopropylbenzotriazole, 5-isopropylbenzotriazole, 4-n-butylbenzotriazole, 5-n-butylbenzotriazole, 4 -Isobutylbenzotriazole, 5-is
- the present invention it is possible to provide a treatment liquid having excellent organic residue removing property and excellent stability. Further, according to the present invention, it is also possible to provide a method for treating an object to be treated related to the above-mentioned treatment liquid.
- the numerical range represented by using “-” means a range including the numerical values before and after "-" as the lower limit value and the upper limit value.
- ppm means “parts-per-parts ( 10-6 )
- ppb means “parts-per-parts ( 10-9 )
- ppt means “ppt”. It means “parts-per-trillion ( 10-12 )”.
- room temperature is "25 ° C”.
- the treatment solution of the present invention contains water, hydroxylamine, and one or more hydrazines selected from the group consisting of hydrazine, hydrazine salts, and hydrazine derivatives, and hydrazine with respect to 100 parts by mass of hydroxylamine.
- the content of the class is 1 part by mass or less.
- the moderately abundant unshared electron pair on nitrogen allows hydrazines and / or hydroxylamine to interact favorably with organic matter in coexistence with hydroxylamine. It is presumed that the treatment solution has excellent organic residue removability. Furthermore, since the content of hydrazines is less than a predetermined amount, it is presumed that the decomposition of hydroxylamine that may occur during storage of the treatment liquid is suppressed, which contributes to the excellent stability of the treatment liquid. Further, when the treatment liquid of the present invention contains a predetermined type and amount of anions, the removability of the residue containing a metal as a main component, which the object to be treated may further have (hereinafter, simply "the treatment liquid".
- the organic residue removability is more excellent, the stability is more excellent, the metal residue removability is more excellent, and / or the smoothness of the object to be treated is more excellent. Is also simply referred to as "the effect of the treatment liquid is superior".
- the treatment liquid contains water.
- the water is not particularly limited, and examples thereof include distilled water, ion-exchanged water, and pure water.
- the content of water in the treatment liquid is not particularly limited, but is preferably 50% by mass or more, more preferably 70% by mass or more, still more preferably 80% by mass or more, based on the total mass of the treatment liquid.
- the upper limit is less than 100% by mass.
- the treatment liquid contains hydroxylamine (NH 2 OH). Hydroxylamine may be ionized in the treatment solution.
- the content of the hydroxylamine compound is not particularly limited, but 0.001 to 25% by mass is preferable with respect to the total mass of the treatment liquid in that the effect of the treatment liquid is more excellent.
- the content of hydroxylamine is 0.001% by mass or more with respect to the total mass of the treatment liquid, the detergency of the treatment liquid is more excellent, and when it is 25% by mass or less, the smoothness of the object to be treated is more excellent. ..
- the content of hydroxylamine is preferably, for example, 0.05 to 15% by mass, more preferably 0.1 to 10% by mass, based on the total mass of the treatment liquid, in that the performance balance of the treatment liquid is excellent. 0.5 to 8% by mass is more preferable.
- the content of hydroxylamine in the treatment liquid can be measured by an ion chromatograph method (Dionex ICS-2100 manufactured by Thermo Fisher Scientific Co., Ltd., etc.). Further, when the components and blending of the raw material used for preparing the treatment liquid are known, it may be calculated from the blending amount.
- the treatment solution contains one or more hydrazines selected from the group consisting of hydrazine, hydrazine salt (hydrazine salt), and hydrazine derivative (hydrazine derivative).
- the hydrazine derivative may be a salt or a non-salt.
- Examples of the hydrazine salt include hydrazine sulfate, hydrazine hydrochloride, and hydrazine acetate.
- H 2 NN X
- the hydrazine derivative is not an azole other than pyrazoles (benzotriazoles and the like).
- R N represent each independently a hydrogen atom or a substituent.
- Two RNs may be combined with each other to form a ring.
- at least one of two R N is other than a hydrogen atom (in other words, at least one of two R N is a substituent, or two R N are bonded to each other to form a ring There is).
- R N which may have a substituent an alkyl group (may. Carbon atoms in branched be linear is preferably 1 to 5), or, -L N -NH 2 (L N represents a single bond or a divalent linking group.
- a group consisting of (preferably) is preferred.
- the two R C independently represents a hydrogen atom or a substituent.
- the total number of atoms other than hydrogen atoms in the hydrazine derivative is preferably 3 to 30, more preferably 3 to 15, and even more preferably 3 to 8.
- hydrazine derivative examples include pyrazole, carbhydrazide, semicarbazide, thiosemicarbazide, monomethylhydrazide, t-butylhydrazine, dimethylhydrazine (1,1-dimethylhydrazine), and aminoguanidine.
- hydrazines preferably contain at least hydrazine.
- the content of hydrazine is preferably 20 to 100% by mass, more preferably 50 to 100% by mass, based on the total mass of hydrazines.
- the total content of hydrazines (preferably hydrazine) with respect to 100 parts by mass of hydroxylamine is 1 part by mass or less.
- the total content is preferably 0.5 parts by mass or less from the viewpoint of more excellent stability of the treatment liquid.
- the total content is preferably 0.00001 parts by mass or more, more preferably 0.0001 parts by mass or more, further preferably 0.0005 parts by mass or more, and 0. More than .005 parts by mass is particularly preferable.
- the total content of hydrazines (preferably hydrazine) in the treatment liquid is preferably 0.0001 to 3000 mass ppm with respect to the total mass of the treatment liquid. If the total content is 0.0001 mass ppm or more (preferably 0.0005 mass ppm or more, more preferably 0.005 mass ppm or more, still more preferably 0.05 mass ppm or more), the organic residue of the treatment liquid Excellent property removal. When the total content is 3000 mass ppm or less (preferably 300 mass ppm or less), the stability of the treatment liquid is more excellent.
- the type and content of hydrazines in the treatment liquid can be measured by an ion chromatograph method (Dionex ICS-2100 manufactured by Thermo Fisher Scientific Co., Ltd., etc.). Further, when the components and blending of the raw material used for preparing the treatment liquid are known, it may be calculated from the blending amount.
- the method for introducing hydrazines into the treatment liquid is not particularly limited, and for example, a substance containing hydrazines (hydrazines themselves or an aqueous solution thereof, etc.) may be added at the time of preparation of the treatment liquid. good. Further, hydrazines may be introduced into the treatment liquid by using a substance containing hydrazines as a trace component (impurity or the like) as a raw material in the preparation of the treatment liquid.
- Treatment liquid, Cl -, NO 2 -, and, NO 3 - is preferable to contain one or more of the first anion selected from the group consisting of, more to contain two or more of the first anion It is preferable to contain three kinds of first anions, and it is more preferable to contain them.
- the treatment liquid, Cl -, NO 2 -, and, NO 3 - preferably contains a total seed.
- the total content of the first anion (Cl -, NO 2 -, and, NO 3 - total content of) is preferably 0.00001 to 100 mass parts.
- the total content is 0.00001 parts by mass or more, the metal residue removing property of the treatment liquid is more excellent, and when the total content is 100 parts by mass or less, the smoothness of the object to be treated is more excellent.
- the total content is preferably, for example, 0.0001 to 30 parts by mass, more preferably 0.1 to 25 parts by mass, and even more preferably 0.1 to 10 parts by mass in that the performance balance of the treatment liquid is excellent. ..
- the present inventor considers the reason why the effect of the treatment liquid is more excellent when the treatment liquid contains anions as described above. That is, in the treatment liquid of the present invention, when the first anion is present in water, the anion reacts suitably with the residue containing metal after dry etching, and the solubility in water is improved to improve the detergency. Can be improved. Such an effect becomes more remarkable when the total content of the first anion is equal to or more than a predetermined amount with respect to hydroxylamine. Further, it is presumed that if the total content of the first anion is less than a predetermined amount with respect to hydroxylamine, so-called pitting corrosion of the metal by the anion can be suppressed and the smoothness of the surface after treatment can be improved. ..
- the total content of the first anion in the treatment liquid is preferably 0.001 to 50,000 mass ppm with respect to the total mass of the treatment liquid.
- the total content is 0.001 mass ppm or more with respect to the total mass of the treatment liquid, the detergency of the treatment liquid is more excellent, and when the total content is 50,000 mass ppm or less, the smoothness of the object to be treated is more excellent.
- the total content is more preferably 1 to 25,000 mass ppm, more preferably 2 to 15,000 mass ppm, based on the total mass of the treatment liquid.
- the content of Cl ⁇ in the treatment liquid is preferably 0.001 to 5000 mass ppm with respect to the total mass of the treatment liquid.
- the Cl ⁇ content is 0.05 mass ppm or more with respect to the total mass of the treatment liquid, the detergency of the treatment liquid is more excellent, and when it is 5000 mass ppm or less, the smoothness of the object to be treated is more excellent.
- the Cl ⁇ content is more preferably 0.05 to 2000 mass ppm, still more preferably 0.1 to 500 mass ppm, based on the total mass of the treatment liquid, in terms of excellent balance of performance of the treatment liquid. ..
- NO 2 - content, relative to the total mass of the treatment liquid is preferably 0.001 to 30,000 mass ppm.
- NO 2 - content of the total weight of the processing liquid more excellent cleaning of the treatment liquid as long as more than 0.001 ppm by mass, more smoothness of the object to be processed as long as 30000 ppm by mass or less Excellent.
- NO 2 - content, relative to the total mass of the treatment liquid for example, more preferably from 0.5 to 20,000 mass ppm, more preferably 1-5000 mass ppm.
- NO 3 - content, relative to the total mass of the treatment liquid is preferably from 0.001 to 30,000 mass ppm.
- NO 3 - content of the total weight of the processing liquid more excellent cleaning of the treatment liquid as long as more than 0.001 ppm by mass, more smoothness of the object to be treated not more than 30000 ppm by mass Excellent.
- NO 3 - content, relative to the total mass of the treatment liquid for example, more preferably from 0.5 to 20,000 mass ppm, more preferably 1-5000 mass ppm.
- NO 2 -, and, NO 3 - and, in particular, also referred to as a specific anion.
- NO 2 -, and, NO 3 - total content by weight of the two specific anionic consisting, based on the total weight of the processing solution is preferably from 0.001 to 50,000 mass ppm.
- the total mass of the specific anions is more preferably 1 to 50,000 mass ppm and further preferably 2 to 10000 mass ppm with respect to the total mass of the treatment liquid in that the performance balance of the treatment liquid is excellent.
- the treatment liquid preferably contains Cl ⁇ in an amount of more than 0% by mass ppm, more preferably 0.001% by mass or more, based on the total mass of the treatment liquid.
- the ratio of the total mass of the specific anion to the mass of Cl ⁇ is preferably 1.1 to 100, more preferably 1.5 to 30.
- the content of the first anion in the treatment liquid, "Cl - containing mass ⁇ NO 3 - - containing mass ⁇ NO 2 of the content mass” preferably satisfy the relationship, "0.001 ppm ⁇ It is more preferable to satisfy the relationship of " content mass of Cl ⁇ ⁇ mass of NO 2 ⁇ content mass of NO 3 ⁇ ".
- Treatment liquid may further contain one or more second anion selected from the group consisting of SO 4 2-and PO 4 3-.
- the treatment liquid is, SO 4 2-and PO 4 3-, and may contain only one of both which may contain both may not be contained. If the treatment solution contains one or more second anion, for hydroxylamine 100 parts by weight, the total content of the first anion and the second anion (Cl -, NO 2 -, NO 3 -, SO 4 2- , and the total content of PO 4 3-) is preferably 0.0001 to 30 parts by weight.
- the total content is 0.0001 parts by mass or more, the detergency of the treatment liquid is more excellent, and when it is 30 parts by mass or less, the smoothness of the object to be treated is more excellent.
- the total content is more preferably 0.1 to 25 parts by mass, still more preferably 0.1 to 10 parts by mass, for example, in terms of excellent balance of performance of the treatment liquid.
- the total content of the second anion (SO 4 2-and PO 4 total content of 3-), based on the total weight of the developer, 0 mass It is preferably more than ppm and 1000 mass ppm or less, and more preferably more than 0 mass ppm and 50 mass ppm or less.
- the treatment solution contains SO 4 2-
- the content of SO 4 2-is with respect to the total mass of the treatment liquid is preferably not more than 0 mass ppm super 500 ppm by weight, 0 mass ppm Ultra 30 More preferably, the mass is ppm or less.
- the content of PO 4 3- is preferably from 0 mass ppm super 500 ppm by weight, 0 mass ppm Ultra 30 More preferably, the mass is ppm or less.
- the contents of the first anion and the second anion in the treatment liquid can be measured by an ion chromatograph method (Dionex ICS-2100 of Thermo Fisher Scientific Co., Ltd., etc.). Further, when the components and blending of the raw material used for preparing the treatment liquid are known, it may be calculated from the blending amount.
- the method for introducing the first anion and / or the second anion into the treatment liquid is not particularly limited, and for example, a substance containing the first anion and / or the second anion (nitrite, nitrite, hydrochloric acid, sulfuric acid, etc.) (Hydronic acid and aqueous solutions thereof, etc.) may be added at the time of preparation of the treatment liquid using the first anion and / or the second anion as a source. Further, a compound that produces a substance containing a first anion and / or a second anion by dissolution in water, a chemical reaction, or the like may be used as a source of the first anion and / or the second anion.
- a substance containing the first anion and / or the second anion nitrite, nitrite, hydrochloric acid, sulfuric acid, etc.
- the treatment liquid may contain a chelating agent.
- the treatment liquid contains a chelating agent, the cleaning property of the treatment liquid is more excellent.
- the chelating agent referred to here does not include the above-mentioned hydrazines.
- the chelating agent means a substance (preferably an acid) capable of functioning as a chelating ligand, and a compound containing 1 or more (preferably 1 to 8) acid groups is preferable.
- the acid group is not particularly limited, but at least one functional group selected from the group consisting of a carboxylic acid group, a sulfonic acid group, and a phosphonic acid group is preferable.
- Examples of the chelating agent containing a carboxylic acid group include polyaminopolycarboxylic acids, aliphatic dicarboxylic acids, aliphatic polycarboxylic acids containing a hydroxyl group, and ascorbic acids.
- a polyaminopolycarboxylic acid is a compound containing a plurality of amino groups and a plurality of carboxylic acid groups, for example, mono- or polyalkylene polyamine polycarboxylic acid, polyaminoalcan polycarboxylic acid, polyaminoalkanol polycarboxylic acid, and hydroxy.
- Alkyl ether polyamines include polycarboxylic acids.
- polyaminopolycarboxylic acid examples include butylenediaminetetraacetic acid, diethylenetriaminetetraacetic acid (DTPA), ethylenediaminetetrapropionic acid, triethylenetetraminehexacetic acid, 1,3-diamino-2-hydroxypropane-N, N, N', N'-tetraacetic acid, propylenediaminetetraacetic acid, ethylenediaminetetraacetic acid (EDTA), trans-1,2-diaminocyclohexanetetraacetic acid, ethylenediaminediaminetetraacetic acid, ethylenediaminediaminedipropionic acid, 1,6-hexamethylene-diamine-N, N , N', N'-tetraacetic acid, N, N-bis (2-hydroxybenzyl) ethylenediamine-N, N-diacetacate, diaminopropanetetraacetic acid, 1,4,7,10
- diethylenetriaminepentacetic acid DTPA
- EDTA ethylenediaminetetraacetic acid
- trans-1,2-diaminocyclohexanetetraacetic acid is preferable.
- the aliphatic dicarboxylic acids include oxalic acid, malonic acid, succinic acid, and maleic acid, and oxalic acid, malonic acid, or succinic acid is preferable.
- the aliphatic polycarboxylic acids containing a hydroxyl group include malic acid, tartaric acid, and citric acid, and citric acid is preferable.
- ascorbic acids include ascorbic acid, isoascorbic acid, ascorbic acid sulfate ester, ascorbic acid phosphate ester, ascorbic acid 2-glucoside, ascorbic acid palmitate, tetraisopalmitate ascorbyl, and ascorbic acid isopalminate.
- ascorbic acids such as these salts, and ascorbic acid is preferable.
- Examples of the chelating agent containing a sulfonic acid group include methanesulfonic acid.
- chelating agents containing a phosphonic acid group include methyldiphosphonic acid, aminotri (methylenephosphonic acid), 1-hydroxyethylidene-1,1-diphosphonic acid, nitrilotrismethylenephosphonic acid (NTMP), and ethylenediaminetetrakis (methylene).
- EDTPO Hexamethylenediaminetetra (Methylenephosphonic acid), Propropylenediaminetetra (Methylenephosphonic acid), Diethylenetriaminepenta (Methylenephosphonic acid), Triethylenetetraminehexa (Methylenephosphonic acid), Triaminotriethylaminehexa (Methylene) Phosphonate), trans-1,2-cyclohexanediaminetetra (methylenephosphonic acid), glycol etherdiaminetetra (methylenephosphonic acid) and tetraethylenepentaminehepta (methylenephosphonic acid), and glycine-N, N-bis (phosphonic acid).
- Methylene phosphonic acid) (glyphosine) can be mentioned.
- the chelating agent is diethylenetriaminetetraacetic acid, ethylenediaminetetraacetic acid, trans-1,2-diaminocyclohexanetetraacetic acid, oxalic acid, malonic acid, succinic acid, citric acid, methanesulfonic acid, 1 in that the effect of the treatment liquid is more excellent.
- One or more selected from the group consisting of -hydroxyethylidene-1,1-diphosphonic acid and nitrilotrismethylenephosphonic acid is preferable.
- the chelating agent is more preferably diethylenetriamine pentaacetic acid or citric acid.
- the content of the chelating agent is preferably 0.01 to 20% by mass, preferably 0.1 to 20% by mass, based on the total mass of the treatment liquid, in that the effect of the treatment liquid is more excellent. 15% by mass is more preferable, and 0.2 to 5% by mass is further preferable. Only one type of chelating agent may be used, or two or more types may be used. When two or more types of chelating agents are used, the total amount thereof is preferably within the above range.
- the treatment liquid may contain an anticorrosive agent.
- the anticorrosive agent has a function of eliminating overetching of the object to be treated, and the smoothness of the object to be treated is further improved.
- the anticorrosive agent referred to here does not include the above-mentioned hydrazines and chelating agents.
- anticorrosive agent for example, a compound represented by the following formula (1X) is preferable.
- R 6a , R 6b and R 6c each independently represent a hydrogen atom or a substituent.
- the substituents include a hydrocarbon group, a halogen atom (fluorine atom, chlorine atom, bromine atom, iodine atom, etc.), an amino group, a nitro group, and an alkoxy group (the number of carbon atoms is 1 to 12).
- 1 to 6 is more preferable, 1 to 3 is more preferable), or a hydroxyl group is preferable.
- These substituents may further contain substituents, if possible.
- Examples of the substituent that the above hydrocarbon group and the above alkoxy group may further contain include, for example, a hydroxyl group, a carboxyl group, or a substituted or unsubstituted amino group (as a substituent, the number of carbon atoms).
- An alkyl group having 1 to 6 is preferable, and an alkyl group having 1 to 3 carbon atoms is more preferable).
- Examples of the substituent that the amino group may further contain include an alkyl group having 1 to 6 carbon atoms.
- the hydrocarbon groups represented by R 6a and R 6b are independently alkyl groups (the number of carbon atoms is preferably 1 to 12, more preferably 1 to 6 and 1 to 3). More preferably), an alkenyl group (preferably 2-12 carbon atoms, more preferably 2-6 carbon atoms), an alkynyl group (preferably 2-12 carbon atoms, more preferably 2-6 carbon atoms), an aryl group (carbons). The number is preferably 6 to 22, more preferably 6 to 14, and even more preferably 6 to 10) and an alkyne group (the number of carbon atoms is preferably 7 to 23, more preferably 7 to 15, and 7 to 11). More preferably). These hydrocarbon groups may further contain substituents, if possible, and examples of substituents that may be further contained are as described above.
- R 6a and R 6b may be combined to form a ring.
- the ring formed by combining R 6a and R 6b include a benzene ring and a naphthalene ring.
- the ring may further have a substituent (for example, a hydrocarbon group having 1 to 5 carbon atoms, a carboxyl group, or the like).
- the anticorrosive agent is preferably azoles (compounds containing a complex 5-membered ring structure containing one or more nitrogens).
- azoles as anticorrosive agents are other than pyrazoles.
- benzotriazoles compounds containing a benzotriazole structure
- the anticorrosive agent is benzotriazoles.
- Bentriazoles include, for example, an alkyl group which may further contain a substituent, an aryl group which may further contain a substituent, a halogen atom (fluorine atom, chlorine atom, bromine atom, iodine atom, etc.), and the like.
- the alkyl group preferably has 1 to 12 carbon atoms, more preferably 1 to 6 carbon atoms, and even more preferably 1 to 3 carbon atoms.
- the preferred carbon number is intended to include the number of carbon atoms in the substituents that the alkyl group can contain.
- the aryl group preferably has 6 to 22 carbon atoms, more preferably 6 to 14 carbon atoms, and even more preferably 6 to 10 carbon atoms.
- the preferred carbon number is intended to include the number of carbon atoms in the substituents that the aryl group can contain.
- the alkoxy group preferably has 1 to 12 carbon atoms, more preferably 1 to 6 carbon atoms, and even more preferably 1 to 3 carbon atoms.
- the preferred carbon number is intended to include the number of carbon atoms in the substituents that the alkoxy group can contain.
- substituents that may be further contained in the alkyl group, the aryl group, and the alkoxy group include, for example, a hydroxyl group, a carboxyl group, or a substituted or unsubstituted amino group (substituent group) independently of each other.
- An alkyl group having 1 to 6 carbon atoms is preferable, and an alkyl group having 1 to 3 carbon atoms is more preferable).
- Examples of the substituent which may be further contained in the amino group include an alkyl group having 1 to 6 carbon atoms.
- benzotriazoles When the benzotriazoles are benzotriazoles containing a substituent, it is preferable that independent substituents are substituted at any one or more of the 1, 4, and 5 positions. It is preferable that the substituent is substituted at any one of the 4-position, 4-position, and 5-position. Substituents other than the 1-position, 4-position, and 5-position of benzotriazole may or may not be substituted. Preferred examples of substituents contained in benzotriazole are as described above. Of these, benzotriazole in which the amino group is substituted at the 1-position or benzotriazole in which the alkyl group is substituted at the 5-position is preferable. The benzotriazoles are also preferably unsubstituted benzotriazoles.
- benzotriazoles include benzotriazole (BTA), 1-hydroxybenzotriazole, 5-phenylthiol-benzotriazole, 5-chlorobenzotriazole, 4-chlorobenzotriazole, 5-bromobenzotriazole, 4-bromobenzotriazole, 5-Fluorobenzotriazole, 4-fluorobenzotriazole, naphthotriazole, tolyltriazole, 5-phenyl-benzotriazole, 5-nitrobenzotriazole, 4-nitrobenzotriazole, 3-amino-5-mercapto-1,2,4 -Triazole, 2- (5-amino-pentyl) -benzotriazole, 1-amino-benzotriazole, 5-methyl-1H-benzotriazole, benzotriazole-5-carboxylic acid, 4-methylbenzotriazole, 4-ethylbenzo Triazole, 5-ethylbenzotriazole, 4-propylbenzotriazole,
- anticorrosive agents other than benzotriazoles include 1,2,4-triazole (TAZ), 5-aminotetrazole (ATA), 5-amino-1,3,4-thiadiazol-2-thiol and 3-amino.
- TZ 1,2,4-triazole
- ATA 5-aminotetrazole
- ATA 5-amino-1,3,4-thiadiazol-2-thiol
- 3-amino 1-amino-1,2,4- Triazole, 1-amino-1,2,3-triazole, 1-amino-5-methyl-1,2,3-triazole, 3-mercapto-1,2,4-triazole, 3-isopropyl-1,2, 4-Triazole, 1H-tetrazole-5-acetic acid, 2-mercaptobenzothiazole (2-MBT), 1-phenyl-2-tetrazoline-5-thione, 2-mercaptobenzoimidazole (2-MBI), 4-methyl- 2-Phenylimidazole, 2-mercaptothiazolin,
- Anticorrosive agents include benzotriazole, 5-aminotetrazole, 1-hydroxybenzotriazole, 5-phenylthiol-benzotriazole, 5-chlorobenzotriazole, 4-chlorobenzotriazole, 5-bromobenzotriazole, 4-bromobenzotriazole, 5-Fluorobenzotriazole, 4-fluorobenzotriazole, naphthotriazole, tolyltriazole, 5-phenyl-benzotriazole, 5-nitrobenzotriazole, 4-nitrobenzotriazole, 3-amino-5-mercapto-1,2,4 -Triazole, 2- (5-amino-pentyl) -benzotriazole, 1-amino-benzotriazole, 5-methyl-1H-benzotriazole, benzotriazole-5-carboxylic acid, 4-methylbenzotriazole, 4-ethylbenzo Triazole, 5-ethylbenzotriazole, 4-propylbenzotri
- the anticorrosive agent is more preferably benzotriazole, 1-amino-benzotriazole, or 5-methyl-1H-benzotriazole, and even more preferably 5-methyl-1H-benzotriazole.
- the content of the anticorrosive agent is preferably 0.01 to 10% by mass, preferably 0.05 to 5% by mass, based on the total mass of the treatment liquid. More preferred. Only one type of anticorrosive agent may be used, or two or more types may be used. When two or more kinds of anticorrosive agents are used, the total amount thereof is preferably within the above range.
- the treatment liquid of the present invention may contain an organic solvent.
- the organic solvent may be a water-soluble organic solvent.
- the fact that the organic solvent is water-soluble means that water at 25 ° C. and the organic solvent can be mixed (dissolved) at an arbitrary ratio.
- the organic solvent include alcohol-based solvents, ketone-based solvents, ester-based solvents, ether-based solvents (for example, glycol diether), sulfone-based solvents, sulfoxide-based solvents, nitrile-based solvents, and amide-based solvents. These solvents may be water soluble.
- the treatment liquid preferably contains one or more kinds of organic solvents selected from the group consisting of alcohol-based solvents, ketone-based solvents, ester-based solvents, and ether-based solvents.
- the alcohol-based solvent examples include alkanediol (including, for example, alkylene glycol), alkoxyalcohol (including, for example, glycol monoether), saturated aliphatic monohydric alcohol, unsaturated non-aromatic monohydric alcohol, and ring. Examples thereof include low molecular weight alcohols containing a structure. Among them, the alcohol solvent is preferably glycol monoether or saturated aliphatic monohydric alcohol.
- alkanediol examples include glycol, 2-methyl-1,3-propanediol, 1,3-propanediol, 2,2-dimethyl-1,3-propanediol, 1,4-butanediol, and 1,3.
- -Butanediol, 1,2-butanediol, 2,3-butanediol, pinacol, alkylene glycol and the like can be mentioned.
- alkylene glycol examples include ethylene glycol, propylene glycol, hexylene glycol, diethylene glycol, dipropylene glycol, triethylene glycol, and tetraethylene glycol.
- alkoxy alcohol examples include 3-methoxy-3-methyl-1-butanol, 3-methoxy-1-butanol, 1-methoxy-2-butanol, glycol monoether and the like.
- glycol monoether examples include ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol mono-n-propyl ether, ethylene glycol monoisopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, and diethylene glycol mono.
- Saturated aliphatic monohydric alcohols include, for example, methanol, ethanol, n-propyl alcohol, isopropyl alcohol, 1-butanol, 2-butanol, isobutyl alcohol, tert-butyl alcohol, 2-pentanol, t-pentyl alcohol, and , Hexanol and the like.
- unsaturated non-aromatic monohydric alcohols examples include allyl alcohol, propargyl alcohol, 2-butenyl alcohol, 3-butenyl alcohol, 4-pentene-2-ol and the like.
- low molecular weight alcohols containing a ring structure examples include tetrahydrofurfuryl alcohol, furfuryl alcohol, and 1,3-cyclopentanediol.
- ketone solvent examples include acetone, propanone, cyclobutanone, cyclopentanone, cyclohexanone, diacetone alcohol, 2-butanone, 5-hexanedione, 1,4-cyclohexanedione, 3-hydroxyacetphenone, and 1,3-cyclohexane.
- dione and cyclohexanone examples include dione and cyclohexanone.
- ester solvent examples include glycol monoesters such as ethyl acetate (ethyl acetate), butyl acetate (butyl acetate), ethylene glycol monoacetate and diethylene glycol monoacetate, and propylene glycol monomethyl ether acetate and ethylene glycol monomethyl.
- glycol monoether monoesters such as ether acetate, propylene glycol monoethyl ether acetate, and ethylene glycol monoethyl ether acetate.
- sulfone solvent examples include sulfolane, 3-methylsulfolane, 2,4-dimethylsulfolane and the like.
- sulfoxide solvent examples include dimethyl sulfoxide and the like.
- nitrile solvent examples include acetonitrile and the like.
- amide solvent examples include N, N-dimethylformamide, 1-methyl-2-pyrrolidone, 2-pyrrolidinone, 1,3-dimethyl-2-imidazolidinone, ⁇ -caprolactam, formamide, N-methylformamide, and the like.
- amide solvent examples include acetamide, N-methylacetamide, N, N-dimethylacetamide, N-methylpropanamide, and hexamethylphosphoric triamide.
- the content of the organic solvent is preferably 0.1 to 20% by mass, more preferably 0.5 to 10% by mass, based on the total mass of the treatment liquid. Only one kind of organic solvent may be used, or two or more kinds may be used. When two or more kinds of organic solvents are used, the total amount thereof is preferably within the above range.
- the treatment liquid may contain a reducing agent different from hydroxylamine. Hydrazines, chelating agents, and anticorrosive agents are not included in reducing agents different from hydroxylamine.
- the reducing agent different from hydroxylamine is not particularly limited, but a reducing substance such as a compound containing an OH group or a CHO group or a compound containing a sulfur atom is preferable.
- the reducing agent has an oxidizing action and has a function of oxidizing OH- ions, dissolved oxygen, etc. that cause decomposition of hydroxylamine.
- One kind is preferable.
- R 4a to R 4e each independently represent a hydrocarbon group which may have a hydrogen atom, a hydroxyl group, or a hetero atom.
- R 4a to R 4e contain a hydrocarbon group which may have a hetero atom, the hydrocarbon group may have a substituent.
- examples of the hydrocarbon group which may have a heteroatom represented by R 4a to R 4e include a hydrocarbon group and a hydrocarbon group containing a heteroatom.
- an alkyl group preferably 1 to 12 carbon atoms, more preferably 1 to 6 carbon atoms
- an alkenyl group preferably 2 to 12 carbon atoms.
- 2 to 6 are more preferable
- alkynyl group carbon number is preferably 2 to 12, 2 to 6 is more preferable
- aryl group carbon number is preferably 6 to 22, 6 to 14 is more preferable, 6 ⁇ 10 is more preferable
- an alkyne group the number of carbon atoms is preferably 7 to 23, more preferably 7 to 15, further preferably 7 to 11).
- hydrocarbon group containing a heteroatom represented by R 4a to R 4e -CH 2- in the above-mentioned hydrocarbon group is, for example, -O-, -S-, -CO-,-. SO 2 - and -NR a - any one selected from the group consisting of or a divalent substituted group with a group formed by combining a plurality of these can be cited.
- the Ra represents a hydrogen atom or a hydrocarbon group having 1 to 20 carbon atoms (preferably an alkyl group having 1 to 5 carbon atoms).
- substituent for example, a hydroxyl group, a carboxyl group, or a substituted or unsubstituted amino group (as the substituent, an alkyl group having 1 to 6 carbon atoms is preferable, and an alkyl group having 1 to 3 carbon atoms is more preferable. ).
- Examples of the compound represented by the above formula (4) include gallic acid, resorcinol, ascorbic acid, tert-butylcatechol, catechol, isoeugenol, o-methoxyphenol, 4,4'-dihydroxyphenyl-2,2-.
- Examples include propane, isoamyl salicylate, benzyl salicylate, methyl salicylate, and 2,6-di-t-butyl-p-cresol.
- the compound represented by the formula (4) preferably has two or more hydroxyl groups, and more preferably three or more, from the viewpoint of reducing addition.
- the position where the hydroxyl group is substituted is not particularly limited, but R 4a and / or R 4b are particularly preferable from the viewpoint of reducing addition.
- Examples of the compound represented by the formula (4) having two or more hydroxyl groups include catechol, resorcinol, tert-butylcatechol, and 4,4'-dihydroxyphenyl-2,2-propane.
- Examples of the compound represented by the formula (4) having three or more hydroxyl groups include gallic acid.
- Examples of the compound containing a sulfur atom include mercaptosuccinic acid, dithiodiglycerol [S (CH 2 CH (OH) CH 2 (OH)) 2 ], and bis (2,3-dihydroxypropylthio) ethylene [CH 2].
- a compound containing an SH group (mercapto compound) is preferable, and 1-thioglycerol, 3-mercapto-1-propanesulfonate sodium, 2-mercaptoethanol, 3-mercapto-1-propanol, or thioglycol Acids are more preferred, and 1-thioglycerol or thioglycolic acid is even more preferred.
- one type of reducing agent different from hydroxylamine may be used alone, or two or more types may be used in combination.
- the treatment liquid may contain fluoride.
- Fluoride promotes the decomposition and solubilization of residues.
- the fluoride is not particularly limited, but is hydrofluoric acid (HF), fluorosilicic acid (H 2 SiF 6 ), fluoroboric acid, ammonium fluoride fluoride salt ((NH 4 ) 2 SiF 6 ), tetramethyl hexafluorophosphate.
- Ammonium, ammonium fluoride, ammonium fluoride salt, ammonium fluoride salt, quaternary ammonium tetrafluoroborate and quaternary phosphonium tetrafluoroborate represented by the formulas NR 4 BF 4 and PR 4 BF 4, respectively.
- tetrabutylammonium tetrafluoroborate (TBA-BF 4 ) can be mentioned.
- quaternary ammonium tetrafluoroborate represented by the above formulas NR 4 BF 4 and PR 4 BF 4 , respectively for example, tetramethylammonium tetrafluoroborate, tetraethylammonium tetrafluoroborate, tetrafluoroborate
- R may be homologous or heterologous to each other and are hydrogen, linear, branched or cyclic C1-C6 alkyl groups ( For example, a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, a hexyl group), and a linear
- the treatment liquid may contain a metal component.
- the metal component include metal particles and metal ions.
- the content of the metal component indicates the total content of the metal particles and the metal ions.
- the treatment liquid may contain either one of the metal particles and the metal ions, or may contain both.
- the treatment liquid preferably contains both metal particles and metal ions.
- the metal atom contained in the metal component examples include Ag, Al, As, Au, Ba, Ca, Cd, Co, Cr, Cu, Fe, Ga, Ge, K, Li, Mg, Mn, Mo, Na. , Ni, Pb, Sn, Sr, Ti, and a metal atom selected from the group consisting of Zn.
- the metal component may contain one kind of metal atom or two or more kinds.
- the metal particles may be simple substances or alloys, and may exist in a form in which the metal is associated with an organic substance.
- the metal component may be a metal component unavoidably contained in each component (raw material) contained in the treatment liquid, or may be a metal component unavoidably contained during the production, storage, and / or transfer of the treatment liquid. However, it may be added intentionally.
- the content of the metal component is often more than 0 mass ppt and 10 mass ppm or less with respect to the total mass of the treatment liquid, and the effect of the treatment liquid is more excellent. It is preferably more than mass ppm and 1 mass ppm or less, and more preferably more than 0 mass ppb and 100 mass ppb or less.
- the type and content of the metal component in the treatment liquid can be measured by the SP-ICP-MS method (Single Nano Particle Inductive Coupled Plasma Mass Spectrometry).
- the treatment liquid may contain a pH adjuster other than the above-mentioned components.
- the pH adjuster include acid compounds and base compounds.
- acid compound examples include acetic acid, perchloric acid, hypochlorous acid, and periodic acid.
- Base compound examples of the basic compound include aqueous ammonia, an amine compound different from hydroxylamine and hydrazines, and a quaternary ammonium hydroxide salt.
- examples of the amine compound different from hydroxylamine and hydrazines include cyclic compounds (compounds containing a cyclic structure).
- Examples of the cyclic compound include amine compounds containing a cyclic structure, which will be described later.
- the quaternary ammonium hydroxide salt is not included in the amine compound which is different from hydroxylamine and hydrazines.
- an amine compound having a cyclic structure is preferable.
- the amino group may be present in only one of the cyclic structure and the outside of the cyclic structure, or may be present in both.
- Examples of the amine compound containing a cyclic structure include tetrahydrofurfurylamine, N- (2-aminoethyl) piperazine, 1,8-diazabicyclo [5.4.0] -7-undecene, and 1,4-diazabicyclo [2.
- Examples of the quaternary ammonium hydroxide salt include compounds represented by the following formula (5).
- R 5a to R 5d independently have an alkyl group having 1 to 16 carbon atoms, an aryl group having 6 to 16 carbon atoms, an aralkyl group having 7 to 16 carbon atoms, or 1 carbon atom. Represents ⁇ 16 hydroxyalkyl groups. At least two of R 5a to R 5d may be coupled to each other to form an annular structure, and in particular, at least one of the combination of R 5a and R 5b and the combination of R 5c and R 5d may be mutually connected. They may be combined to form a cyclic structure.
- Examples of the compound represented by the above formula (5) include tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, methyltripropylammonium hydroxide, and methyltributyl.
- Ammonium hydroxide, ethyltrimethylammonium, dimethyldiethylammonium hydroxide, benzyltrimethylammonium hydroxide, hexadecyltrimethylammonium hydroxide, or (2-hydroxyethyl) trimethylammonium hydroxide are preferred.
- the content of the quaternary ammonium hydroxide salt is preferably 0.05 to 10% by mass, preferably 0.1 to 5% by mass, based on the total mass of the treatment liquid. % Is more preferable.
- water-soluble amines other than those described above can also be used.
- the pka of the water-soluble amine is preferably 7.5 to 13.0 at room temperature.
- the water-soluble amine is intended to be an amine capable of dissolving 50 g or more in 1 L of water at room temperature. Ammonia water is not included as the water-soluble amine.
- water-soluble amine an unsubstituted hydroxylamine and a hydroxylamine derivative may be used.
- the pka of the water-soluble amine in the present specification is the acid dissociation constant in water.
- the acid dissociation constant in water can be measured by a combination of a spectrometer and potentiometric titration.
- the pH adjuster is composed of acetic acid, perchloric acid, hypochlorous acid, periodic acid, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide, aqueous ammonia, and water-soluble amine.
- acetic acid perchloric acid, hypochlorous acid, periodic acid, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide, aqueous ammonia, and water-soluble amine.
- perchloric acid hypochlorous acid
- periodic acid tetramethylammonium hydroxide
- tetraethylammonium hydroxide tetrabutylammonium hydroxide
- aqueous ammonia aqueous ammonia
- water-soluble amine water-soluble amine
- the pH of the treatment liquid is preferably 1 to 13 and more preferably 6 to 11 in that the effect of the treatment liquid is more excellent.
- the pH of the treatment liquid is a value measured by F-51 (trade name) manufactured by HORIBA, Ltd. at room temperature (25 ° C.).
- the content of the pH adjuster may be appropriately set so that the treatment liquid can have a desired pH.
- the method for producing the above-mentioned treatment liquid is not particularly limited, and a known production method can be used. For example, a method of mixing water, hydroxylamine, and hydrazines (or an aqueous solution thereof, etc.) can be mentioned. When mixing the above components, other optional components (substances containing a first anion and / or a second anion, etc.) may be further mixed, if necessary. Further, when producing the treatment liquid, the treatment liquid may be filtered and purified using a filter, if necessary.
- the treatment liquid of the present invention is preferably used for an object to be treated containing a metal-based material which is a material containing a metal, and is also referred to as a cobalt-containing substance containing a cobalt atom (simply referred to as a "cobalt-containing substance"). ) Is more preferably used for the object to be treated. Further, the treatment liquid is preferably used for a cobalt-containing material containing a cobalt atom and a material to be treated containing a metal-containing material containing a metal atom other than the cobalt atom.
- the treatment liquid may be contained in a container and stored until use. Such a container and the treatment liquid contained in the container are collectively referred to as a treatment liquid container.
- the treatment liquid is taken out from the stored treatment liquid container and used. Further, the treatment liquid may be transported as a treatment liquid container.
- the container it is preferable that the container has a high degree of cleanliness and less impurities are eluted for semiconductor applications.
- Examples of usable containers include the "clean bottle” series manufactured by Aicello Chemical Corporation and the "pure bottle” manufactured by Kodama Resin Industry.
- the inner wall of the container is preferably formed of one or more resins selected from the group consisting of polyethylene resin, polypropylene resin and polyethylene-polypropylene resin, or a resin different from this. It is also preferable that the inner wall of the container is made of a metal that has been subjected to rust prevention and metal elution prevention treatment, such as stainless steel, Hastelloy, Inconel and Monel.
- a fluororesin (perfluororesin) is preferable.
- a container whose inner wall is a fluororesin By using a container whose inner wall is a fluororesin, it is possible to suppress the occurrence of a problem of elution of ethylene or propylene oligomer as compared with a container whose inner wall is a polyethylene resin, a polypropylene resin, or a polyethylene-polypropylene resin.
- Examples of the container whose inner wall is a fluororesin include a FluoroPure PFA composite drum manufactured by Entegris. In addition, it is described on pages 4 of the special table No. 3-502677, page 3 of the pamphlet of International Publication No. 2004/016526, and pages 9 and 16 of the pamphlet of International Publication No. 99/46309. Containers can also be used.
- quartz and an electropolished metal material are also preferably used for the inner wall of the container.
- the metal material used for producing the electropolished metal material contains at least one selected from the group consisting of chromium and nickel, and the total content of chromium and nickel is 25 with respect to the total mass of the metal material. It is preferably a metal material having a mass% of more than%, and examples thereof include stainless steel and nickel-chromium alloys.
- the total content of chromium and nickel in the metal material is preferably 30% by mass or more with respect to the total mass of the metal material.
- the upper limit of the total content of chromium and nickel in the metal material is not particularly limited, but is preferably 90% by mass or less with respect to the total mass of the metal material.
- the stainless steel is not particularly limited, and known stainless steel can be used. Among them, an alloy containing 8% by mass or more of nickel is preferable, and an austenitic stainless steel containing 8% by mass or more of nickel is more preferable.
- austenitic stainless steels include SUS (Steel Use Stainless) 304 (Ni content 8% by mass, Cr content 18% by mass), SUS304L (Ni content 9% by mass, Cr content 18% by mass), and SUS316. (Ni content 10% by mass, Cr content 16% by mass) and SUS316L (Ni content 12% by mass, Cr content 16% by mass) can be mentioned.
- the nickel-chromium alloy is not particularly limited, and a known nickel-chromium alloy can be used. Of these, nickel-chromium alloys having a nickel content of 40 to 75% by mass and a chromium content of 1 to 30% by mass are preferable. Examples of the nickel-chromium alloy include Hastelloy (trade name, the same shall apply hereinafter), Monel (trade name, the same shall apply hereinafter), and Inconel (trade name, the same shall apply hereinafter).
- Hastelloy C-276 Ni content 63% by mass, Cr content 16% by mass
- Hastelloy-C Ni content 60% by mass, Cr content 17% by mass
- Hastelloy C- 22 Ni content 61% by mass, Cr content 22% by mass
- the nickel-chromium alloy may further contain boron, silicon, tungsten, molybdenum, copper, or cobalt in addition to the above alloy, if necessary.
- the method for electrolytically polishing a metal material is not particularly limited, and a known method can be used.
- a known method can be used.
- the methods described in paragraphs [0011]-[0014] of JP2015-227501 and paragraphs [0036]-[0042] of JP2008-264929 can be used.
- the metal material is preferably buffed.
- the method of buffing is not particularly limited, and a known method can be used.
- the size of the abrasive grains used for finishing the buffing is not particularly limited, but # 400 or less is preferable because the unevenness on the surface of the metal material tends to be smaller.
- the buffing is preferably performed before the electrolytic polishing.
- the metal material may be processed by combining one or two or more of a plurality of stages of buffing, acid cleaning, magnetic fluid polishing, etc., which are performed by changing the count such as the size of the abrasive grains. ..
- the inside of these containers is washed before filling with the treatment liquid.
- the liquid used for cleaning preferably has a reduced amount of metal impurities in the liquid.
- the treatment liquid may be bottling, transported or stored in a container such as a gallon bottle or a coated bottle after production.
- the inside of the container may be replaced with an inert gas (chisso, argon, etc.) having a purity of 99.99995% by volume or more for the purpose of preventing changes in the components in the treatment liquid during storage.
- an inert gas chisso, argon, etc.
- a gas having a low water content is preferable.
- the temperature may be normal temperature, but the temperature may be controlled in the range of ⁇ 20 ° C. to 20 ° C. in order to prevent deterioration.
- the treatment liquid may be a kit in which the raw material is divided into a plurality of parts. Further, the treatment liquid may be prepared as a concentrated liquid. When the treatment liquid is a concentrated liquid, the concentration ratio thereof is appropriately determined depending on the composition of the composition, but is preferably 5 to 2000 times. That is, the concentrated solution is diluted 5 to 2000 times before use.
- the treatment liquid is typically a metal-based material which is a material containing a metal. It can be used in contact with the contained object to be treated. At this time, the object to be treated may contain a plurality of types of metal-based materials. It is also preferable that the treatment liquid dissolves at least one of the metal-based materials which may contain a plurality of types.
- Metallic materials include metal atoms (cobalt (Co), ruthenium (Ru), tungsten (W), molybdenum (Mo), aluminum (Al), copper (Cu), titanium (Ti), and / or tantalum (Ta). ) Etc.), and examples thereof include single metals, alloys, metal oxides (may be composite oxides), and metal nitrides (may be composite nitrides).
- the content of the metal atom in the metal-based material is preferably 30 to 100% by mass, more preferably 40 to 100% by mass, still more preferably 52 to 100% by mass, based on the total mass of the metal-based material.
- the metal-based material include cobalt-containing substances and metal-containing substances. Details of the cobalt-containing substance and the metal-containing substance will be described later.
- At least one of the metal-based materials that may contain a plurality of types of the object to be treated is a cobalt-containing material
- the treatment liquid is brought into contact with the object to be treated containing the cobalt-containing material. It is also preferable to dissolve (etch) the cobalt-containing material. That is, the treatment liquid may be, for example, an etching treatment liquid.
- the object to be treated is a metal-containing material containing a metal atom other than the cobalt atom (hereinafter, also simply referred to as “other metal atom”) together with the cobalt-containing material (hereinafter, also simply referred to as “metal-containing material”). It is also preferable to contain it.
- the treatment liquid may be used for etching only the cobalt-containing material, or may be used for etching both the cobalt-containing material and the metal-containing material.
- the form of the object to be processed is not particularly limited, and for example, as shown in FIG. 1, the substrate 12, the insulating film 14 containing the holes arranged on the substrate 12, and the inner wall of the holes of the insulating film 14
- the object to be treated may be the object 10 containing the metal-containing portion 16 arranged in layers along the hole and the cobalt-containing portion 18 filled in the hole.
- the metal-containing part can function as a barrier metal layer.
- FIG. 1 describes an embodiment in which the object to be treated contains one cobalt-containing portion, the present invention is not limited to this embodiment, and for example, as shown in FIG. 2, the substrate 12 and the substrate 12 are arranged.
- the object to be treated 20 may be contained. That is, the object to be treated may have a cobalt-containing material in a plurality of places and may contain a metal-containing material in a plurality of places.
- the type of substrate that may be contained in the object to be processed is not particularly limited, and is a semiconductor wafer, a glass substrate for a photomask, a glass substrate for liquid crystal display, a glass substrate for plasma display, a substrate for FED (Field Exposure Display), and the like.
- Examples thereof include various substrates such as a substrate for an optical disk, a substrate for a magnetic disk, and a substrate for a photomagnetic disk.
- Examples of the material constituting the semiconductor substrate include group III-V compounds such as silicon, silicon germanium, and GaAs, or any combination thereof.
- the size, thickness, shape, layer structure, and the like of the substrate are not particularly limited and can be appropriately selected as desired.
- the insulating film As the insulating film, a known insulating film is used. In FIGS. 1 and 2, the insulating film contains a hole portion, but the present invention is not limited to this embodiment, and the insulating film may be an insulating film containing a groove portion.
- the cobalt-containing material may have a cobalt atom, for example, cobalt alone (metal cobalt), cobalt alloy (preferably an alloy in which cobalt is the metal component having the highest content mass), cobalt oxide, and cobalt. Cobalt can be mentioned.
- the content of cobalt atoms in the cobalt-containing material is preferably 50 to 100% by mass, more preferably 80 to 100% by mass, and even more preferably 99 to 100% by mass, based on the total mass of the cobalt-containing material.
- the type of other metal atoms in the metal-containing material is not particularly limited, and examples thereof include titanium and tantalum. Among them, as the other metal atom, a noble metal atom is preferable to cobalt.
- the metal-containing material may contain the above-mentioned other metal atoms, and examples thereof include simple metals, alloys, oxides, and nitrides.
- titanium alone, titanium alloy, titanium oxide, titanium nitride, tantalum alone, tantalum alloy, tantalum oxide, or tantalum nitride is preferable because the effect of the treatment liquid is more excellent.
- the cobalt-containing substance and the metal-containing substance may be in contact with each other in the object to be treated or may be arranged via other members.
- the form of the cobalt-containing substance and the metal-containing substance is not particularly limited, and may be, for example, any of a film-like form, a wiring-like form, and a particle-like form.
- the thickness thereof is not particularly limited and may be appropriately selected depending on the intended use. For example, 50 nm or less is preferable, 20 nm or less is more preferable, and 10 nm or less is further preferable. ..
- the cobalt-containing material and the metal-containing material may be arranged only on one main surface of the substrate, or may be arranged on both main surfaces. Further, the cobalt-containing substance and the metal-containing substance may be arranged on the entire main surface of the substrate, or may be arranged on a part of the main surface of the substrate.
- the object to be treated may contain two or more kinds of cobalt-containing substances, or may contain two or more kinds of metal-containing substances.
- the object to be treated containing the cobalt-containing material contains a different metal-based material instead of the cobalt-containing material.
- these objects to be treated may contain a ruthenium-containing substance, a tungsten-containing substance, a molybdenum-containing substance, an aluminum-containing substance, or a copper-containing substance instead of the cobalt-containing substance.
- ruthenium-containing material, tungsten-containing material, molybdenum-containing material, aluminum-containing material, and copper-containing material include, for example, ruthenium, tungsten, molybdenum, aluminum, and cobalt in the cobalt-containing material described above, respectively. It is the same as replacing it with copper.
- the object to be treated contains a ruthenium-containing substance, a tungsten-containing substance, a molybdenum-containing substance, an aluminum-containing substance, or a copper-containing substance instead of the cobalt-containing substance, "another metal" in the above-mentioned metal-containing substance is used.
- Atoms are also metal atoms other than ruthenium atoms, metal atoms other than tungsten atoms, metal atoms other than molybdenum atoms, metal atoms other than aluminum atoms, and other metal atoms other than copper atoms, respectively. It becomes a metal atom. Even in this case, as the metal-containing material, titanium alone, titanium alloy, titanium oxide, titanium nitride, tantalum alone, tantalum alloy, tantalum oxide, or tantalum nitride is preferable.
- the object to be treated may contain various layers and / or structures as desired.
- the substrate may contain metal wiring, a gate electrode, a source electrode, a drain electrode, an insulating layer, a ferromagnetic layer, and / or a non-magnetic layer and the like.
- the substrate may contain exposed integrated circuit structures such as interconnect mechanisms such as metal wiring and dielectric materials. Examples of the metal and alloy used in the interconnection mechanism include aluminum, copper-aluminum alloy, copper, titanium, tantalum, cobalt, silicon, titanium nitride, tantalum nitride, and tungsten.
- the substrate may contain layers of silicon oxide, silicon nitride, silicon carbide, and / or carbon-doped silicon oxide.
- the manufacturing method of the object to be processed is not particularly limited.
- an insulating film is formed on the substrate, holes or grooves are formed in the insulating film, and a sputtering method, a chemical vapor deposition (CVD) method, and a molecular beam epitaxy (MBE) are used.
- a flattening treatment such as CMP may be carried out to produce the object to be treated shown in FIG.
- Examples of the method for treating the object to be treated according to the present invention include a method in which the object to be treated containing at least one kind of metal-based material is brought into contact with the treatment liquid.
- a method in which the object to be treated containing at least one kind of metal-based material is brought into contact with the treatment liquid By adopting such a method, one or more of the metal-based materials contained in the object to be processed can be dissolved, or the object to be processed can be washed (cleaning of the dry etching residue contained in the object to be processed, etc.). ..
- the method for treating the object to be treated of the present invention there is a method in which the object to be treated containing at least a cobalt-containing substance is brought into contact with the treatment liquid to dissolve the cobalt-containing substance.
- a method for treating an object to be treated is also referred to as a first aspect of the method for treating an object to be treated according to the present invention.
- the method of contacting the object to be treated with the treatment liquid is not particularly limited, and for example, a method of immersing the object to be treated in the treatment liquid placed in a tank, a method of spraying the treatment liquid on the object to be treated, a method of spraying the treatment liquid onto the object to be treated, and a method to be treated. Examples include a method of flowing the treatment liquid on top and any combination thereof. Above all, a method of immersing the object to be treated in the treatment liquid is preferable.
- a mechanical stirring method may be used.
- the mechanical stirring method include a method of circulating the treatment liquid on the object to be treated, a method of flowing or spraying the treatment liquid on the object to be treated, and stirring the treatment liquid by ultrasonic waves or megasonic. The method can be mentioned.
- the contact time between the object to be treated and the treatment liquid can be adjusted as appropriate.
- the treatment time (contact time between the treatment liquid and the object to be treated) is not particularly limited, but is preferably 0.25 to 10 minutes, more preferably 0.5 to 2 minutes.
- the temperature of the treatment liquid during the treatment is not particularly limited, but is preferably 20 to 75 ° C, more preferably 20 to 65 ° C.
- the cobalt-containing material in the object to be treated is mainly dissolved.
- the metal-containing material may or may not be dissolved together with the cobalt-containing material by this treatment.
- the metal-containing material may be dissolved intentionally or unavoidably.
- the amount of the metal-containing material inevitably dissolved is small.
- the amount of the metal-containing material inevitably dissolved is small, which is also referred to as the treatment liquid having excellent member resistance to the metal-containing material.
- the object to be treated may contain a ruthenium-containing substance, a tungsten-containing substance, a molybdenum-containing substance, an aluminum-containing substance, or a copper-containing substance in place of or in addition to the cobalt-containing substance. ..
- the following second aspect can be mentioned. That is, the step A in which the object to be treated containing the metal layer is subjected to an oxidation treatment to oxidize the surface layer of the metal layer to form a metal oxide layer, and the object to be treated obtained in the step A.
- This is a method for treating an object to be treated which comprises a step B of bringing the metal oxide layer into contact with a treatment liquid to dissolve the metal oxide layer.
- the second aspect may be one form of the first aspect.
- the metal layer is a form of a metal-based material and is a layer made of a metal-based material that can be oxidized.
- the metal layer is preferably, for example, a simple substance or an alloy of a metal.
- the metal layer includes a cobalt-containing substance (cobalt simple substance or cobalt alloy, etc.), a ruthenium-containing substance (lutenium simple substance or ruthenium alloy, etc.), a tungsten-containing substance (tungsten simple substance or tungsten alloy, etc.), and a molybdenum-containing substance (molybdenum simple substance or molybdenum alloy, etc.).
- an alloy such as an alloy
- an aluminum-containing material a single aluminum or an aluminum alloy, etc.
- a copper-containing material a single copper or a copper alloy, etc.
- a cobalt-containing material a single cobalt or a cobalt alloy, etc.
- the metal oxide layer is a layer formed by oxidizing the surface layer of the metal layer, and can be said to be a form of a metal-based material.
- a part of the surface layer of the metal layer may be a metal oxide layer, or the entire surface layer of the metal layer may be a metal oxide layer.
- the metal oxide layer is an oxide of a metal alone or an alloy, and is a cobalt oxide, an oxide of a cobalt alloy, a ruthenium oxide, an oxide of a ruthenium alloy, a tungsten oxide, an oxide of a tungsten alloy, a molybdenum oxide, or a molybdenum.
- the oxidation treatment is a treatment of oxidizing the surface layer of the metal layer, for example, 1 to 10 atomic layers to form a metal oxide layer.
- the metal oxide layer is often more soluble (easily etched) in the treatment solution than the metal layer. That is, in the second aspect, the surface of the metal layer is made into a thin metal oxide layer in step A, and the metal oxide layer (and the metal layer existing under the metal oxide layer) is inevitably formed by using the treatment liquid in step B. By removing only the part that can be dissolved), only the very thin surface of the metal layer contained in the object to be treated can be removed (dissolved). Further, by repeating the steps A and B alternately and repeatedly, the etching amount can be controlled with high accuracy. When the process A and the process B are alternately performed, it is preferable that the process A and the process B are performed 1 to 20 times each.
- the object to be treated to which the second aspect can be applied may contain one type of metal layer alone, or may contain two or more types of metal layers. Further, the object to be treated to which the second aspect can be applied may contain a metal-based material other than the metal layer or the metal oxide layer, and a part or all of such the metal-based material is the step A and the step. It may be intentionally or unavoidably removed via B.
- Step A is a step of subjecting the object to be treated containing the metal layer to an oxidation treatment to oxidize the surface layer of the metal layer to form a metal oxide layer.
- oxidation treatment for oxidizing the surface layer of the metal layer to form a metal oxide layer. It can be carried out by performing ozone treatment in which ozone gas is brought into contact, heat treatment in oxygen that heats in an oxygen atmosphere, etc.), or plasma treatment using oxygen gas, which will be described later.
- ozone treatment in which ozone gas is brought into contact
- heat treatment in oxygen that heats in an oxygen atmosphere, etc. heat treatment in oxygen that heats in an oxygen atmosphere, etc.
- plasma treatment using oxygen gas which will be described later.
- One type of oxidation treatment may be carried out, or two or more types may be carried out.
- the oxidation treatment it is preferable to carry out at least a liquid treatment in which a predetermined solution is brought into contact with the object to be treated.
- the oxidation solution may be any solution that can oxidize the surface layer of the metal layer.
- the oxidation solution is preferably a solution other than the treatment solution of the present invention.
- oxidation solution examples include water, a mixed aqueous solution of hydrogen peroxide, ammonia and hydrogen peroxide (APM), a mixed aqueous solution of hydrofluoric acid and hydrogen peroxide (FPM), and a mixed aqueous solution of sulfuric acid and hydrogen peroxide (SPM). ),
- a mixed aqueous solution of hydrochloric acid and hydrogen peroxide (HPM), oxygen-dissolved water, ozone-dissolved water, perchloric acid, and a solution selected from the group consisting of nitrate (hereinafter, also referred to as "specific solution”) is preferable. ..
- the specific solution is preferably a solution selected from the group consisting of water, hydrogen peroxide solution, APM, FPM, SPM, HPM, oxygen-dissolved water, and ozone-dissolved water.
- the composition of the hydrogen peroxide solution is, for example, the content of H 2 O 2 is 0.5 to 31% by mass, more preferably 3 to 15% by mass, based on the total mass of the hydrogen peroxide solution.
- the description of these preferable composition ratios is that ammonia water is 28% by mass ammonia water, hydrofluoric acid is 49% by mass hydrofluoric acid, sulfuric acid is 98% by mass sulfuric acid, hydrochloric acid is 37% by mass hydrochloric acid, and hydrogen peroxide solution is 30% by mass.
- the composition ratio in the case of% hydrofluoric acid solution is intended.
- the volume ratio is based on the volume at room temperature.
- composition of the ozone dissolved water for example, with respect to the total weight content of the ozone-dissolved water of O 3, an aqueous solution of 1 to 200 mass ppm.
- Perchlorate for example, an aqueous solution of from 0.001 to 60 mass% content of HClO 4 are based on the total weight of the solution.
- Nitric acid is, for example, an aqueous solution containing 0.001 to 60% by mass of HNO 3 based on the total mass of the solution.
- the method of contacting the object to be treated with the oxidizing solution is not particularly limited. Examples include a method of spraying the oxidizing solution, a method of flowing the oxidizing solution on the object to be treated, and any combination thereof.
- the contact time between the object to be treated and the oxidizing solution is, for example, preferably 0.25 to 10 minutes, more preferably 0.5 to 5 minutes.
- the temperature of the oxidizing solution is preferably 20 to 75 ° C, more preferably 20 to 60 ° C.
- examples of the oxidizing gas that comes into contact with the object to be treated include dry air, oxygen (O 2 ) gas, ozone (O 3 ) gas, and a mixed gas thereof.
- the oxidation gas may contain a gas other than the above-mentioned gas.
- the oxidizing gas that comes into contact with the object to be treated is preferably oxygen gas or ozone gas.
- oxygen gas or ozone gas is brought into contact with the object to be treated, it is also preferable to bring it into contact with an oxygen atmosphere, an ozone atmosphere, or a mixed gas atmosphere of oxygen and ozone.
- the gas treatment it is also preferable to heat the object to be treated (for example, heating at 40 to 200 ° C.) while contacting the oxide gas.
- the gas treatment is preferably ozone treatment in which ozone gas is brought into contact with the object to be treated, or heat treatment in oxygen in which the object to be treated is heated in an oxygen atmosphere.
- ozone gas may be brought into contact with the object to be treated in an ozone atmosphere, or ozone gas may be brought into contact with the object to be treated in a mixed gas atmosphere of ozone gas and other gases (for example, oxygen gas). ..
- the ozone treatment may be a treatment of heating the object to be treated while bringing it into contact with ozone gas.
- the object to be treated may contain a metal-based material other than the metal layer which is oxidized by the oxidation treatment and the surface layer becomes a metal oxide layer, and such a metal-based material may be contained. Part or all of the material may be intentionally or unavoidably removed by step A (particularly liquid treatment). Further, in step A (particularly in the case of liquid treatment), a part of the metal layer of the object to be treated may be intentionally or unavoidably removed.
- the step B is a method for treating the object to be treated, which comprises the step B in which the object to be treated obtained in the step A and the treatment liquid are brought into contact with each other to dissolve the metal oxide layer.
- the method of contacting the object to be treated with the treatment liquid is not limited, and examples similar to the method of contacting the object to be treated with the oxidizing solution can be mentioned.
- the contact time between the object to be treated and the treatment liquid is preferably, for example, 0.25 to 10 minutes, more preferably 0.5 to 5 minutes.
- the temperature of the treatment liquid is preferably 20 to 75 ° C, more preferably 20 to 60 ° C.
- step B the removal of the metal oxide layer may be performed partially or entirely.
- a part or all of the metal layer (for example, the metal layer that has been exposed to the surface layer by removing the metal oxide layer covering the surface) may be intentionally or unavoidably removed.
- the object to be treated may contain a metal oxide layer and other metal-based materials other than the metal layer forming the metal oxide layer on the surface, or a part of such a metal-based material or All may be removed intentionally or inevitably.
- the metal layer and / or the other metal-based material is not intentionally dissolved, it is preferable that the amount of the metal layer and / or the other metal-based material inevitably dissolved is small.
- the treatment liquid used in step B may be degassed in advance to reduce the amount of dissolved oxygen.
- the exposed metal layer obtained by removing the metal oxide layer by the treatment liquid is oxidized by the dissolved oxygen in the treatment liquid to become a new metal oxide layer, and such a metal oxide layer is further removed by the treatment liquid, resulting in the result.
- the removal of an excessive amount of the metal layer can be suppressed by reducing the amount of dissolved oxygen in the treatment liquid.
- the object to be processed containing a metal-based material is subjected to a dry etching treatment, and then the object to be processed is brought into contact with the treatment liquid.
- An embodiment of removing the dry etching residue can be mentioned.
- the metal-based material contained in the object to be treated in this embodiment may be one kind alone or two or more kinds.
- at least one type is preferably a cobalt-containing material, a ruthenium-containing material, a molybdenum-containing material, an aluminum-containing material, or a copper-containing material, and is preferably a cobalt-containing material.
- the object to be processed is subjected to a dry etching process on the object to be processed containing a cobalt-containing substance containing a cobalt atom, and then the object to be processed and the treatment liquid are subjected to a dry etching treatment.
- a dry etching process on the object to be processed containing a cobalt-containing substance containing a cobalt atom, and then the object to be processed and the treatment liquid are subjected to a dry etching treatment.
- An embodiment in which the dry etching residue is removed by contact is preferable.
- the object to be treated that comes into contact with the treatment liquid contains a metal-based material.
- the object to be treated is brought into contact with the treatment liquid after being subjected to the dry etching treatment.
- the object to be processed at the time of contact with the treatment liquid contains a dry etching residue on the surface.
- the dry etching residue existing on the surface of such an object to be treated is removed.
- Such a method for treating an object to be treated is also referred to as a third aspect of the method for treating an object to be treated according to the present invention.
- the third aspect may be one form in which the configuration of the object to be processed and the purpose of the treatment in the above-mentioned first aspect are particularly limited.
- the treatment liquid of the present invention can also be suitably used for such applications for cleaning the object to be treated (application for removing residues).
- FIG. 3 shows a schematic diagram showing an example of the object to be processed (the object to be processed after the dry etching process) in the third aspect.
- the object to be processed 30 shown in FIG. 3 is provided with a metal-containing film 34, an etching stop layer 36, an interlayer insulating film 38, and a metal hard mask 40 in this order on a substrate 32, and is placed in a predetermined position after undergoing a dry etching step or the like.
- a hole 42 is formed in which the metal-containing film 34 is exposed. That is, the object to be treated shown in FIG.
- the 3 includes a substrate 32, a metal-containing film 34, an etching stop layer 36, an interlayer insulating film 38, and a metal hard mask 40 in this order, and an opening of the metal hard mask 40. It is a laminate having holes 42 penetrating from the surface of the portion to the surface of the metal-containing film 34.
- the inner wall 44 of the hole 42 is composed of a cross-sectional wall 44a made of an etching stop layer 36, an interlayer insulating film 38 and a metal hard mask 40, and a bottom wall 44b made of an exposed metal-containing film 34, and is a dry etching residue 46. Is attached.
- the metal hard mask in the object to be processed may become a barrier metal after the object to be processed is further processed.
- the layer that becomes the barrier metal in the subsequent process may be used as a metal hard mask in the dry etching process. That is, the barrier metal may be used as a metal hard mask.
- the metal-containing film 34 and the metal hard mask 40 contains cobalt.
- the metal-containing film 34 is a cobalt-containing substance and the metal hard mask 40 is a metal-containing substance, or the metal-containing film 34 is a metal-containing substance and the metal hard mask 40 is a cobalt-containing substance. Is preferable.
- the metal-containing film 34 is a cobalt-containing material and the metal hard mask 40 is a metal-containing material.
- the dry etching residue may be an organic residue containing an organic substance as a main component.
- the organic residue is a residue having an organic substance content of 50% by mass or more.
- the organic residue may be a residue that does not substantially contain a metal-containing substance and / or a cobalt-containing substance.
- the dry etching residue may contain a metal component as a main component, or may be a metal residue containing a metal-containing substance and / or a cobalt-containing substance.
- the metal residue is a residue having a metal component content of more than 50% by mass.
- the metal residue may be a residue that is substantially free of organic substances.
- a method of bringing the treatment liquid into contact with the object to be treated there is a method of bringing the treatment liquid into contact with the object to be treated.
- the method of contacting the treatment liquid with the object to be treated is the same as described above in the first aspect.
- the dry etching residue on the object to be processed is removed.
- a metal-based material for example, a cobalt-containing substance, preferably a cobalt-containing substance which is a metal-containing film 34
- a metal-based material for example, a cobalt-containing substance, preferably a cobalt-containing substance which is a metal-containing film 34
- the dissolution of the metal-based material may be intentional dissolution for removing a part or all of the metal-containing film 34 (cobalt-containing material or the like) in the bottom wall 44b of the hole 42. , It may be an unavoidable dissolution caused by contact of the treatment liquid with a metal-based material (cobalt-containing substance or the like).
- this treatment method may include a rinsing step of rinsing the object to be treated with a rinsing solution.
- the method for treating the object to be treated in the first aspect, the second aspect, or the third aspect described above may further include a rinsing step after the procedure described in the description of each of the above aspects. Further, the rinsing step may be included between the step A and the step B in the second aspect.
- rinsing solution examples include water, hydrofluoric acid (preferably 0.001 to 1% by mass hydrofluoric acid), sulfuric acid (preferably 0.001 to 1% by mass hydrochloric acid), and aqueous hydrogen peroxide solution (preferably 0.5 to 1% by mass).
- Is 10 to 60 mass ppm ozone water hydrogen water (preferably 10 to 20 mass ppm hydrogen water), citric acid aqueous solution (preferably 0.01 to 10 mass% citric acid aqueous solution), sulfuric acid (preferably 1 to 10 mass by mass).
- the volume ratio of "37 mass% hydrochloric acid: 60 mass% sulfuric acid” is (Osui) corresponding to the combination of "2.6: 1.4" to "3.4: 0.6"), ultrapure water, and sulfuric acid.
- perchloric acid preferably 0.001 to 1% by mass perchloric acid
- aqueous oxalic acid solution preferably 0.01 to 10% by mass oxalic acid aqueous solution
- acetic acid Preferably 0.01 to 10 mass% acetic acid aqueous solution or acetic acid stock solution
- perioic acid aqueous solution preferably 0.5 to 10 mass% perioic acid aqueous solution.
- Perioic acid is, for example, orthoperiodine. Acids and metaperioic acids are preferred).
- the preferred conditions for FPM, SPM, APM, and HPM are, for example, the same as the preferred conditions for FPM, SPM, APM, and HPM used as the specific solution described above.
- Hydrofluoric acid, nitric acid, perchloric acid, and hydrochloric acid are intended as aqueous solutions in which HF, HNO 3 , HClO 4 , and HCl are dissolved in water, respectively.
- Ozone water, carbon dioxide water, and hydrogen water are intended as aqueous solutions in which O 3 , CO 2 , and H 2 are dissolved in water, respectively.
- These rinsing solutions may be mixed and used as long as the purpose of the rinsing step is not impaired.
- the rinse liquid may contain an organic solvent.
- Specific methods of the rinsing step include a method of bringing the rinsing liquid into contact with the object to be treated.
- the contacting method is carried out by immersing the substrate in the rinse liquid contained in the tank, spraying the rinse liquid on the substrate, flowing the rinse liquid on the substrate, or any combination thereof.
- the treatment time is not particularly limited, but is, for example, 5 seconds to 5 minutes.
- the temperature of the rinsing liquid during the treatment is not particularly limited, but for example, in general, 16 to 60 ° C. is preferable, and 18 to 40 ° C. is more preferable.
- the temperature is preferably 90 to 250 ° C.
- the present treatment method may include a drying step of carrying out a drying treatment, if necessary, after the rinsing step.
- the method of drying treatment is not particularly limited, but spin drying, flow of dry gas on the substrate, heating means of the substrate such as heating with a hot plate or an infrared lamp, IPA (isopropyl alcohol) steam drying, marangoni drying, rotagoni drying, or , A combination thereof.
- the drying time varies depending on the specific method used, but is usually about 30 seconds to several minutes.
- This processing method may be carried out in combination before or after other steps performed in the method for manufacturing a semiconductor device.
- the present treatment method may be incorporated into other steps during the implementation of the present treatment method, or the present treatment method may be incorporated into the other steps.
- Other steps include, for example, a step of forming each structure such as a metal wiring, a gate structure, a source structure, a drain structure, an insulating layer, a ferromagnetic layer and / or a non-magnetic layer (layer formation, etching, chemical mechanical polishing, modification). Etc.), resist forming step, exposure step and removal step, heat treatment step, cleaning step, inspection step and the like.
- the target of application of the treatment liquid is, for example, NAND, DRAM (Dynamic Random Access Memory), SRAM (Static Random Access Memory), ReRAM (Resistive Random Access Memory), FRAM (Registered Random Access Memory), FRAM (Registered Random Access Memory), FRAM It may be (Magnetoresistive Random Access Memory), PRAM (Phase change Random Access Memory), or the like, or it may be a logic circuit, a processor, or the like.
- Treatment solution The components shown below were mixed in a predetermined formulation to prepare treatment solutions to be applied to each test.
- Each raw material used in each of the treatment liquids shown below was purified using a high-purity grade, and further distilled, ion-exchanged, filtered, or a combination thereof in advance.
- ⁇ Organic solvent> -Methanol isopropyl alcohol, 1-butanol, 1,3-propanediol, ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, 3-methoxy-3-methyl-1-butanol, 3-methoxy-1-butanol, 1 -Methoxy-2-butanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monobutyl ether, triethylene glycol monomethyl ether, 1-methoxy-2-propanol, acetone, cyclohexanone, 2 -Butanol, ethyl acetate, butyl acetate, propylene glycol monomethyl ether acetate
- ⁇ Corrosion inhibitor> -Benzotriazole-5-aminotetrazole-5-phenylbenzotriazole-1-aminobenzotriazole-5-methyl-1H-benzotriazole-benzotriazole-5-carboxylic acid-4-methylbenzotriazole
- ⁇ Chelating agent> Diethylenetriamine-5 acetic acid ⁇ ethylenediamine-4acetic acid ⁇ Trans-1,2-diaminocyclohexane 4 acetic acid ⁇ Oxalic acid ⁇ Malonic acid ⁇ Citrate ⁇ Methanesulfonic acid ⁇ 1-hydroxyethylidene-1,1-diphosphonic acid ⁇ Nitrilotrismethylenephosphonic acid
- nitrite / nitrate aqueous solution in pure water was prepared by reacting between H 2 O and NO 2, it is an aqueous solution containing nitric acid and nitrous acid.
- ⁇ Water> -Water Water purified by repeating distillation, filter filtration, and ion exchange of ultrapure water until the first anion and the second anion became less than the detection limit was used.
- the detection limit was less than 0.001 mass ppm. In the detection, if necessary, a treatment such as removing a part of water from the sample to be detected to concentrate the target substance was performed, and then the measurement was performed.
- 1,8-diazabicyclo [5.4.0] -7-undecene pH adjuster used to adjust to the basic side
- one of acetic acid and 1,8-diazabicyclo [5.4.0] -7-undecene was added as a pH adjuster in a required amount.
- the amount of the pH adjuster added was 3.0% by mass or less with respect to the total mass of the treatment liquids in all the treatment liquids.
- the resist film, metal hard mask (TiN layer), an etch stop layer (Al 2 O 3 layer), Co layer and an interlayer insulating (ILD) layer was prepared a multi-layer substrate are laminated in this order .
- This multi-layer substrate is subjected to patterning treatment by lithography, etching treatment using a plasma etching apparatus for metal, and removal treatment of a resist film by oxygen plasma ashing, and a multi-layer substrate for evaluation test (hereinafter referred to as "test").
- test a multi-layer substrate for evaluation test
- a treatment liquid 200 mL was filled in a glass beaker having a volume of 500 mL.
- the temperature of the treatment liquid was raised to 40 ° C. while stirring with a stirrer.
- the test piece was washed by immersing the test piece prepared above in a treatment liquid having a liquid temperature of 40 ° C. for 5 minutes while stirring. While the test piece was immersed in the treatment solution, the test piece was held using 4-inch long plastic locking tweezers so that the side surface of the test piece from which the photoresist was removed faced the stir bar.
- test piece was immediately removed from the treatment solution and placed in 400 mL of ion-exchanged water (water temperature 17 ° C.) filled in a plastic beaker having a capacity of 500 mL and gently agitated. After immersing the test piece in ion-exchanged water for 30 seconds, the test piece was immediately taken out and rinsed under an ion-exchanged water stream at 17 ° C. for 30 seconds.
- ion-exchanged water water temperature 17 ° C.
- test piece was exposed to a stream of nitrogen gas to blow off the droplets adhering to the surface of the test piece, and the surface of the test piece was dried.
- nitrogen drying step the test piece was removed from the holding portion of the plastic tweezers, and the test piece was placed in a plastic storage box with a lid with the element side facing up and stored.
- the surface of the obtained test piece was subjected to composition analysis by X-ray Photoelectron Spectroscopy (XPS).
- XPS X-ray Photoelectron Spectroscopy
- the surface of the obtained test piece was measured using an XPS device (manufactured by ULVAC-PHI, trade name QuanteraSXM).
- the carbon atomic weights contained in the organic residue of the test piece measured before and after the treatment were compared, and the reduction rate due to the treatment was calculated and used as the organic residue removal rate.
- the organic residue removability of each treatment liquid was evaluated according to the following evaluation criteria.
- Organic residue removal rate is 95% or more 2: Organic residue removal rate is 80% or more and less than 95% 3: Organic residue removal rate is 75% or more and less than 80% 4: Organic residue removal rate is 50% or more Less than 75% 5: Organic residue removal rate is less than 50%
- the calculation was performed, and the obtained maintenance rate was classified according to the following evaluation criteria, and the stability of each treatment liquid was evaluated. The maintenance rate did not exceed 100% regardless of which treatment liquid was used. 1: Maintenance rate is 99% or more 2: Maintenance rate is 95% or more and less than 99% 3: Maintenance rate is 85% or more and less than 95% 4: Maintenance rate is 75% or more and less than 85% 5: Maintenance rate is less than 75%
- a substrate having a metal cobalt layer formed on one surface of a commercially available silicon wafer (diameter: 12 inches) by a CVD (Chemical Vapor Deposition) method was prepared.
- the thickness of the metallic cobalt layer was 20 nm.
- the obtained substrate is immersed in water at 40 ° C. for 1 minute, and then immersed in each of the treatment solutions listed in the table at 40 ° C. for 30 seconds as one cycle, and the cycle is repeated until the metallic cobalt is dissolved by 10 nm. went.
- An object to be treated (pre-treatment laminate) having a metal cobalt layer, a SiN film, a SiO 2 film, and a barrier metal (TaN) containing a predetermined opening was formed on the substrate (Si) in this order.
- plasma etching (dry etching) is performed using the barrier metal as a mask, and the SiN film and SiO 2 film are etched until the metal cobalt layer is exposed to form via holes, and the sample is sampled. 1 was manufactured (see FIG. 3).
- the evaluation of metal residue removability is 1 to 6 and the evaluation of smoothness is 1 to 8.
- the "Hydrazines (to HA 100 parts)” column shows the total content (parts by mass) of hydrazines with respect to 100 parts by mass of hydroxylamine in each treatment liquid. When two kinds of hydrazines are used, the mass content of each of the two kinds of hydrazines is adjusted to be equal.
- the "anion (ppm)” column indicates the content (mass ppm) of each anion in each treatment liquid with respect to the total mass of the treatment liquid.
- the “First anion content (to HA 100 parts)” column shows the total content (mass part) of the first anion with respect to 100 parts by mass of hydroxylamine in each treatment liquid.
- the "First anion content (to HA 100 parts)" column shows the total content (mass part) of the first anion and the second anion with respect to 100 parts by mass of hydroxylamine in each treatment liquid.
- the "pH” column indicates the pH of each treatment solution.
- the components (remaining) not specified in the table in each treatment liquid consist of a pH adjuster added to achieve a predetermined pH and water.
- Tables 1a-1 and 1a-2 show the formulation of the treatment liquid and the test results in Examples 001 to 049 separately.
- the treatment liquid of Example 001 contains 0.1% by mass of hydroxylamine with respect to the total mass of the treatment liquid, and contains hydrazine as hydrazines in an amount of 0.001% by mass (hydroxylamine) with respect to the total mass of the treatment liquid. 0.0001 parts by mass), no first anion, no second anion, no chelating agent, no anticorrosive agent No organic solvent is contained, and the rest is a pH adjuster and water added so as to have a pH of 9.
- the test results of the treatment liquid of Example 001 showed that the evaluation of organic residue removability was 3, the evaluation of stability was 3, the evaluation of metal residue removability was 9, and the evaluation of smoothness was 3. be.
- Tables 1b-1 and subsequent tables and Table 1b-2 and subsequent tables have the same relationship.
- the treatment liquid contained a chelating agent (more preferably diethylenetriamine pentaacetic acid or citric acid), it was confirmed that the effect of the treatment liquid was more excellent (Examples 093 to 155, and Examples 055, 056, 063, (See Comparison of Results with 064, 070, 071, 072, etc.).
- a chelating agent more preferably diethylenetriamine pentaacetic acid or citric acid
- the treatment liquid contains an anticorrosive agent (more preferably benzotriazole, 1-amino-benzotriazole, or 5-methyl-1H-benzotriazole, more preferably 5-methyl-1H-benzotriazole), the treatment liquid (Refer to the comparison of the results with Examples 156 to 204, and Examples 055, 056, 063, 064, 070, 071, 072, etc.).
- an anticorrosive agent more preferably benzotriazole, 1-amino-benzotriazole, or 5-methyl-1H-benzotriazole, more preferably 5-methyl-1H-benzotriazole
- the treatment liquid contains one or more organic solvents (more preferably ethylene glycol monobutyl ether) selected from the group consisting of alcohol solvents, ketone solvents, ester solvents, and ether solvents
- the treatment liquid (Refer to the comparison of the results with Examples 205 to 372 and Examples 055, 056, 063, 064, 070, 071, 072, etc.).
- Processed object 12 Substrate 14 Insulating film 16 Metal-containing part 18 Cobalt-containing part 30
- Processed object 32
- Substrate 34 Metal-containing film 36
- Etching stop layer 38
- Interlayer insulating film 40
- Hole 46
- Dry etching residue 44
- Inner wall 44a cross-section wall 44b bottom wall
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Abstract
Description
例えば、特許文献1においては、N-ヒドロキシホルムアミドを含むことを特徴とする洗浄剤組成物等が開示されている。
このような被処理物の処理に供される処理液は、例えば、被処理物に対して事前にされた処理(ドライエッチング処理等)によって生じた有機系の残渣物の除去性に優れる(以下、単に「有機残渣物除去性が優れる」とも言う)ことが求められている。また、処理液は、例えば、経時後でも一定の性能を実現できることも求められており、安定性に優れることも求められている。
また、本発明は、上記処理液に関する、被処理物の処理方法の提供も課題とする。
水と、
ヒドロキシルアミンと、
ヒドラジン、ヒドラジン塩、及び、ヒドラジン誘導体からなる群から選択される1種以上のヒドラジン類と、を含有し、
上記ヒドロキシルアミン100質量部に対する、上記ヒドラジン類の合計含有量が1質量部以下である、処理液。
〔2〕
上記ヒドロキシルアミン100質量部に対する、上記ヒドラジン類の合計含有量が0.0001質量部以上である、〔1〕に記載の処理液。
〔3〕
上記ヒドロキシルアミン100質量部に対する、上記ヒドラジン類の合計含有量が0.005~0.5質量部である、〔1〕又は〔2〕に記載の処理液。
〔4〕
上記ヒドラジン誘導体が、一般式(A)で表される化合物、一般式(B)で表される化合物、ピラゾール環を有する化合物、及び、これらの塩からなる群から選択される1種以上である、〔1〕~〔3〕のいずれかに記載の処理液。
H2N-N-RN 2 (A)
H2N-N=X (B)
一般式(A)中、2つのRNは、それぞれ独立に、水素原子又は置換基を表す。2つのRNが互いに結合して環を形成していてもよい。ただし、2つのRNの少なくとも一方は、水素原子以外である。
一般式(B)中、Xは二価の基を表す。
〔5〕
上記ヒドラジン類が、ヒドラジンを含有する、〔1〕~〔4〕のいずれかに記載の処理液。
〔6〕
更に、Cl-、NO2 -、及び、NO3 -からなる群から選択される1種以上の第1アニオンを含有する、〔1〕~〔5〕のいずれかに記載の処理液。
〔7〕
Cl-、NO2 -、及び、NO3 -からなる3種の上記第1アニオンを含有する、〔6〕に記載の処理液。
〔8〕
上記ヒドロキシルアミン100質量部に対する、上記第1アニオンの合計含有量が0.0001~30質量部である、〔6〕又は〔7〕に記載の処理液。
〔9〕
更に、SO4 2-及びPO4 3-からなる群から選択される1種以上の第2アニオンを含有し、
上記ヒドロキシルアミン100質量部に対する、上記第1アニオンと上記第2アニオンとの合計含有量が0.0001~30質量部である、〔6〕~〔8〕のいずれかに記載の処理液。
〔10〕
NO2 -、及び、NO3 -の合計含有質量が、Cl-の含有質量よりも多い、〔6〕~〔9〕のいずれかに記載の処理液。
〔11〕
更に、キレート剤を含有する、〔1〕~〔10〕のいずれかに記載の処理液。
〔12〕
上記キレート剤が、カルボン酸基、ホスホン酸基、及び、スルホン酸基からなる群から選択される官能基を含有する、〔11〕に記載の処理液。
〔13〕
上記キレート剤が、ジエチレントリアミン五酢酸、エチレンジアミン四酢酸、トランス-1,2-ジアミノシクロヘキサン四酢酸、シュウ酸、マロン酸、コハク酸、クエン酸、メタンスルホン酸、1-ヒドロキシエチリデン-1,1-ジホスホン酸、及び、ニトリロトリスメチレンホスホン酸からなる群から選択される1種以上である、〔11〕又は〔12〕に記載の処理液。
〔14〕
更に、防食剤を含有する、〔1〕~〔13〕のいずれかに記載の処理液。
〔15〕
上記防食剤が、ベンゾトリアゾール類である、〔14〕に記載の処理液。
〔16〕
上記ベンゾトリアゾール類が、更に置換基を含有してもよいアルキル基、更に置換基を含有してもよいアリール基、ハロゲン原子、更に置換基を含有してもよいアミノ基、ニトロ基、更に置換基を含有してもよいアルコキシ基、及び、ヒドロキシル基からなる群から選択される1種以上の置換基によって置換されていてもよいベンゾトリアゾールである、〔15〕に記載の処理液。
〔17〕
上記防食剤が、ベンゾトリアゾール、5-アミノテトラゾール、1-ヒドロキシベンゾトリアゾール、5-フェニルチオール-ベンゾトリアゾール、5-クロロベンゾトリアゾール、4-クロロベンゾトリアゾール、5-ブロモベンゾトリアゾール、4-ブロモベンゾトリアゾール、5-フルオロベンゾトリアゾール、4-フルオロベンゾトリアゾール、ナフトトリアゾール、トリルトリアゾール、5-フェニル-ベンゾトリアゾール、5-ニトロベンゾトリアゾール、4-ニトロベンゾトリアゾール、3-アミノ-5-メルカプト-1,2,4-トリアゾール、2-(5-アミノ-ペンチル)-ベンゾトリアゾール、1-アミノ-ベンゾトリアゾール、5-メチル-1H-ベンゾトリアゾール、ベンゾトリアゾール-5-カルボン酸、4-メチルベンゾトリアゾール、4-エチルベンゾトリアゾール、5-エチルベンゾトリアゾール、4-プロピルベンゾトリアゾール、5-プロピルベンゾトリアゾール、4-イソプロピルベンゾトリアゾール、5-イソプロピルベンゾトリアゾール、4-n-ブチルベンゾトリアゾール、5-n-ブチルベンゾトリアゾール、4-イソブチルベンゾトリアゾール、5-イソブチルベンゾトリアゾール、4-ペンチルベンゾトリアゾール、5-ペンチルベンゾトリアゾール、4-ヘキシルベンゾトリアゾール、5-ヘキシルベンゾトリアゾール、5-メトキシベンゾトリアゾール、5-ヒドロキシベンゾトリアゾール、ジヒドロキシプロピルベンゾトリアゾール、1-[N,N-ビス(2-エチルヘキシル)アミノメチル]-ベンゾトリアゾール、5-t-ブチルベンゾトリアゾール、5-(1’,1’-ジメチルプロピル)-ベンゾトリアゾール、5-(1’,1’,3’-トリメチルブチル)ベンゾトリアゾール、5-n-オクチルベンゾトリアゾール、及び、5-(1’,1’,3’,3’-テトラメチルブチル)ベンゾトリアゾールからなる群から選択される1種以上である、〔14〕に記載の処理液。
〔18〕
更に、アルコール系溶剤、ケトン系溶剤、エステル系溶剤、及び、エーテル系溶剤からなる群から選択される1種以上の有機溶剤を含有する、〔1〕~〔17〕のいずれかに記載の処理液。
〔19〕
pHが6~11である、〔1〕~〔18〕のいずれかに記載の処理液。
〔20〕
コバルト原子を含有するコバルト含有物、及び、コバルト原子以外の他の金属原子を含有する金属含有物を含有する被処理物に対して使用される、〔1〕~〔19〕のいずれかに記載の処理液。
〔21〕
上記コバルト含有物が、コバルト単体、コバルト合金、コバルト酸化物、又は、コバルト窒化物である、〔20〕に記載の処理液。
〔22〕
コバルト原子を含有するコバルト含有物を含有する被処理物と、〔1〕~〔21〕のいずれかに記載の処理液とを接触させて、上記コバルト含有物を溶解させる、被処理物の処理方法。
〔23〕
金属層を含有する被処理物に対して、
水、過酸化水素水、アンモニア及び過酸化水素の混合水溶液、フッ酸及び過酸化水素水の混合水溶液、硫酸及び過酸化水素水の混合水溶液、塩酸及び過酸化水素水の混合水溶液、酸素溶存水、並びに、オゾン溶存水からなる群から選択される溶液を接触させる液処理、
オゾンガスを接触させるオゾン処理、
酸素雰囲気下で加熱する酸素中加熱処理、又は、
酸素ガスを用いたプラズマ処理、を施して、上記金属層の表層を酸化させて金属酸化層とする工程Aと、
上記工程Aで得られた被処理物と、〔1〕~〔19〕のいずれかに記載の処理液とを接触させて、上記金属酸化層を溶解させる工程Bと、を含有する被処理物の処理方法。
〔24〕
上記工程Aと上記工程Bとを交互に繰り返し実施する、〔23〕に記載の被処理物の処理方法。
〔25〕
上記金属層が、コバルト単体又はコバルト合金であるコバルト含有物からなる、〔23〕又は〔24〕に記載の被処理物の処理方法。
〔26〕
金属系材料を含有する被処理物にドライエッチング処理を施した後、
上記被処理物と〔1〕~〔19〕のいずれかに記載の処理液とを接触させて、ドライエッチング残渣物を除去する、被処理物の処理方法。
〔27〕
上記金属系材料がコバルト原子を含有するコバルト含有物である、〔26〕に記載の被処理物の処理方法。
また、本発明によれば、上記処理液に関する被処理物の処理方法も提供できる。
以下に記載する構成要件の説明は、本発明の代表的な実施形態に基づいてなされる場合があるが、本発明はそのような実施形態に制限されない。
本発明の処理液は、水と、ヒドロキシルアミンと、ヒドラジン、ヒドラジン塩、及び、ヒドラジン誘導体からなる群から選択される1種以上のヒドラジン類と、を含有し、ヒドロキシルアミン100質量部に対する、ヒドラジン類の含有量が1質量部以下である。
処理液がこのような構成をとることで上記課題が解決される機序は必ずしも明確ではないが、本発明者は以下のように考えている。
すなわち、本発明の処理液中は、水中に、ヒドロキシルアミンとヒドラジン類とを同時に含有する。ヒドラジン類は、窒素原子をヒドロキシルアミンよりも多く有しており、窒素原子が有する非共有電子対の数がヒドロキシルアミンよりも多い。このように、ヒドラジン類が適度に豊富に窒素上の非共有電子対を有することで、ヒドロキシルアミンとの共存化において、ヒドラジン類及び/又はヒドロキシルアミンが有機物に対して好適に相互作用することができ、処理液の優れた有機残渣物除去性が実現できている、と推測している。更に、ヒドラジン類の含有量が所定量以下であるため、処理液の保管中に生じ得るヒドロキシルアミンの分解が抑制され、処理液の優れた安定性に寄与している、と推測している。
また、本発明の処理液が、所定の種類及び量のアニオンを含有する場合、被処理物が更に有し得る、金属を主成分として含有する残渣物の除去性(以下、単に「処理液の金属残渣物除去性」ともいう)、及び/又は、処理を実施した後の被処理物が含有し得る金属含有物(コバルト含有物等)の表面平滑性(以下、単に「被処理物の平滑性」ともいう)も優れる。
以下、本発明の処理液に関して、有機残渣物除去性がより優れること、安定性がより優れること、金属残渣物除去性がより優れること、及び/又は、被処理物の平滑性がより優れることを、単に「処理液の効果がより優れる」とも言う。
処理液は、水を含有する。
水は特に制限されず、例えば、蒸留水、イオン交換水、及び、純水が挙げられる。
処理液は、ヒドロキシルアミン(NH2OH)を含有する。
ヒドロキシルアミンは処理液中で電離していてもよい。
ヒドロキシルアミンの含有量が、処理液の全質量に対して、0.001質量%以上であれば処理液の洗浄性がより優れ、25質量%以下であれば被処理物の平滑性がより優れる。
処理液の性能のバランスが優れる点で、ヒドロキシルアミンの含有量は、処理液の全質量に対して、例えば、0.05~15質量%が好ましく、0.1~10質量%がより好ましく、0.5~8質量%が更に好ましい。
処理液中のヒドロキシルアミンの含有量は、イオンクロマトグラフ法(サーモフィッシャー社のDionex ICS-2100等)で測定できる。
また、処理液の調製に使用した原料の成分及び配合が既知である場合、配合量から計算で求めてもよい。
処理液は、ヒドラジン、ヒドラジン塩(ヒドラジンの塩)、及び、ヒドラジン誘導体(ヒドラジンの誘導体)からなる群から選択される1種以上のヒドラジン類を含有する。
ヒドラジン誘導体は、塩であってもよいし塩以外であってもよい。
ヒドラジン塩としては、ヒドラジン硫酸塩、ヒドラジン塩酸塩、及び、ヒドラジン酢酸塩が挙げられる。
ヒドラジン誘導体としては、例えば、一般式(A)で表される化合物(H2N-N-RN 2で表される化合物)、一般式(B)で表される化合物(H2N-N=Xで表される化合物)、ピラゾール環を有する化合物(ピラゾール類)、及び、これらの塩(硫酸塩、塩酸塩、又は、酢酸塩等)が挙げられる。
H2N-N-RN 2 (A)
H2N-N=X (B)
なお、ヒドラジン誘導体は、ピラゾール類以外のアゾール類(ベンゾトリアゾール類等)ではないことも好ましい。
RNで表される置換基としては、置換基を有してもよいアルキル基(直鎖状でも分岐鎖状でもよい。炭素数は1~5が好ましい)、又は、-LN-NH2(LNは単結合又は二価の連結基を表す。二価の連結基は、-CO-、-CS-、-NH-、-C(=NH)-、又は、これらの2以上の組み合わせからなる基が好ましい)が好ましい。
ヒドラジンの含有量は、ヒドラジン類の全質量に対して、20~100質量%が好ましく、50~100質量%がより好ましい。
また、処理液の調製に使用した原料の成分及び配合が既知である場合、配合量から計算で求めてもよい。
処理液は、Cl-、NO2 -、及び、NO3 -からなる群から選択される1種以上の第1アニオンを含有することが好ましく、2種以上の第1アニオンを含有することがより好ましく、3種の第1アニオンを含有することが更に好ましい。
つまり、処理液は、Cl-、NO2 -、及び、NO3 -の全種を含有することが好ましい。
処理液中において、ヒドロキシルアミン100質量部に対する、第1アニオンの合計含有量(Cl-、NO2 -、及び、NO3 -の合計含有量)は、0.00001~100質量部が好ましい。
上記合計含有量が、0.00001質量部以上であれば処理液の金属残渣物除去性がより優れ、100質量部以下であれば被処理物の平滑性がより優れる。処理液の性能のバランスが優れる点で、上記合計含有量は、例えば、0.0001~30質量部が好ましく、0.1~25質量部がより好ましく、0.1~10質量部が更に好ましい。
すなわち、本発明の処理液中は、水中に、第1アニオンが存在すると、ドライエッチングの後の金属を含む残渣物等に対してアニオンが好適に反応し、水に対する溶解性が上がり洗浄性を向上できる。このような作用は、第1アニオンの合計含有量が、ヒドロキシルアミンに対して所定量以上であれば、より顕著になる。また第1アニオンの合計含有量が、ヒドロキシルアミンに対して所定量以下であれば、アニオンによる金属への、いわゆる孔食腐食が抑制され処理後表面の平滑性を向上できる、と推測している。
上記合計含有量が、処理液の全質量に対して、0.001質量ppm以上であれば処理液の洗浄性がより優れ、50000質量ppm以下であれば被処理物の平滑性がより優れる。処理液の性能のバランスが優れる点で、上記合計含有量は、処理液の全質量に対して、例えば、1~25000質量ppmがより好ましく、2~15000質量ppmが更に好ましい。
Cl-の含有量が、処理液の全質量に対して、0.05質量ppm以上であれば処理液の洗浄性がより優れ、5000質量ppm以下であれば被処理物の平滑性がより優れる。
処理液の性能のバランスが優れる点で、Cl-の含有量は、処理液の全質量に対して、例えば、0.05~2000質量ppmがより好ましく、0.1~500質量ppmが更に好ましい。
NO2 -の含有量が、処理液の全質量に対して、0.001質量ppm以上であれば処理液の洗浄性がより優れ、30000質量ppm以下であれば被処理物の平滑性がより優れる。処理液の性能のバランスが優れる点で、NO2 -の含有量は、処理液の全質量に対して、例えば、0.5~20000質量ppmがより好ましく、1~5000質量ppmが更に好ましい。
NO3 -の含有量が、処理液の全質量に対して、0.001質量ppm以上であれば処理液の洗浄性がより優れ、30000質量ppm以下であれば被処理物の平滑性がより優れる。処理液の性能のバランスが優れる点で、NO3 -の含有量は、処理液の全質量に対して、例えば、0.5~20000質量ppmがより好ましく、1~5000質量ppmが更に好ましい。
NO2 -、及び、NO3 -からなる2種の特定アニオンの合計含有質量は、処理液の全質量に対して、0.001~50000質量ppmが好ましい。
処理液の性能のバランスが優れる点で、特定アニオンの合計含有質量は、処理液の全質量に対して、1~50000質量ppmがより好ましく、2~10000質量ppmが更に好ましい。
例えば、Cl-の含有質量に対する、特定アニオンの合計含有質量の比(特定アニオンの合計含有質量/Cl-の含有質量)は、1.1~100が好ましく、1.5~30がより好ましい。
処理液は、更に、SO4 2-及びPO4 3-からなる群から選択される1種以上の第2アニオンを含有してもよい。
つまり、処理液は、SO4 2-及びPO4 3-の、一方のみを含有してもよいし、両方とも含有してもよいし、両方とも含有しなくてもよい。
処理液が1種以上の第2アニオンを含有する場合、ヒドロキシルアミン100質量部に対する、第1アニオンと第2アニオンとの合計含有量(Cl-、NO2 -、NO3 -、SO4 2-、及び、PO4 3-の合計含有量)は、0.0001~30質量部が好ましい。
上記合計含有量が、0.0001質量部以上であれば処理液の洗浄性がより優れ、30質量部以下であれば被処理物の平滑性がより優れる。処理液の性能のバランスが優れる点で、上記合計含有量は、例えば、0.1~25質量部がより好ましく、0.1~10質量部が更に好ましい。
処理液がSO4 2-を含有する場合、処理液中、SO4 2-の含有量は、処理液の全質量に対して、0質量ppm超500質量ppm以下が好ましく、0質量ppm超30質量ppm以下がより好ましい。
処理液がPO4 3-を含有する場合、処理液中、PO4 3-の含有量は、処理液の全質量に対して、0質量ppm超500質量ppm以下が好ましく、0質量ppm超30質量ppm以下がより好ましい。
また、処理液の調製に使用した原料の成分及び配合が既知である場合、配合量から計算で求めてもよい。
また、水への溶解又は化学反応等によって、第1アニオン及び/又は第2アニオンを含有する物質を生じさせる化合物を、第1アニオン及び/又は第2アニオンの供給源としてもよい。このような例としては、水と反応して亜硝酸を生じさせる、三酸化二窒素が挙げられる。
更に、不純物(微量成分)として第1アニオン及び/又は第2アニオンを含有する物質を処理液の調製に原料として使用することで、処理液に第1アニオン及び/又は第2アニオンを導入してもよい。
処理液は、キレート剤を含有していてもよい。処理液がキレート剤を含有する場合、処理液の洗浄性がより優れる。ただし、ここでいうキレート剤には上述のヒドラジン類は含まれない。
上記酸基は特に制限されないが、カルボン酸基、スルホン酸基、及び、ホスホン酸基からなる群より選ばれる少なくとも1種の官能基が好ましい。
ポリアミノポリカルボン酸は、複数のアミノ基及び複数のカルボン酸基を含有する化合物であり、例えば、モノ-又はポリアルキレンポリアミンポリカルボン酸、ポリアミノアルカンポリカルボン酸、ポリアミノアルカノールポリカルボン酸、及び、ヒドロキシアルキルエーテルポリアミンポリカルボン酸が挙げられる。
脂肪族ジカルボン酸類としては、例えば、シュウ酸、マロン酸、コハク酸、及び、マレイン酸が挙げられ、シュウ酸、マロン酸、又は、コハク酸が好ましい。
ヒドロキシル基を含有する脂肪族ポリカルボン酸類としては、例えば、リンゴ酸、酒石酸、及び、クエン酸が挙げられ、クエン酸が好ましい。
アスコルビン酸類としては、例えば、アスコルビン酸、イソアスコルビン酸、アスコルビン酸硫酸エステル、アスコルビン酸リン酸エステル、アスコルビン酸2-グルコシド、アスコルビン酸パルミチン酸エステル、テトライソパルミチン酸アスコルビル、及び、アスコルビン酸イソパルミネート、並びに、これらの塩等のアスコルビン酸類が挙げられ、アスコルビン酸が好ましい。
中でも、キレート剤は、ジエチレントリアミン五酢酸又はクエン酸がより好ましい。
キレート剤は1種のみを用いても、2種以上を用いてもよい。キレート剤を2種以上用いる場合は、その合計量が上記範囲内であることが好ましい。
処理液は、防食剤を含有していてもよい。防食剤は、被処理物のオーバーエッチングを解消する機能を有し、被処理物の平滑性がより向上する。ここでいう防食剤には、上述のヒドラジン類及びキレート剤は含まれない。
上記置換基としては、それぞれ独立に、炭化水素基、ハロゲン原子(フッ素原子、塩素原子、臭素原子、又は、ヨウ素原子等)、アミノ基、ニトロ基、アルコキシ基(炭素数は、1~12が好ましく、1~6がより好ましく、1~3が更に好ましい)、又は、ヒドロキシル基が好ましい。これらの置換基は、可能な場合、更に置換基を含有してもよい。
上記炭化水素基及び上記アルコキシ基が、更に含有してもよい置換基としては、例えば、それぞれ独立に、ヒドロキシル基、カルボキシル基、又は、置換若しくは無置換のアミノ基(置換基としては、炭素数1~6のアルキル基が好ましく、炭素数1~3のアルキル基がより好ましい)が挙げられる。
上記アミノ基が、更に含有してもよい置換基としては、例えば、炭素数1~6のアルキル基が挙げられる。
これらの炭化水素基は、可能な場合、更に置換基を含有してもよく、更に含有してもよい置換基の例は上述の通りである。
R6aとR6bとが結合して形成する環としては、例えば、ベンゼン環及びナフタレン環が挙げられる。R6aとR6bとが結合して環を形成した場合、上記環は、更に置換基(例えば、炭素数1~5の炭化水素基、又はカルボキシル基等)を有していてもよい。
アゾール類としては、ベンゾトリアゾール類(ベンゾトリアゾール構造を含有する化合物)であるのも好ましい。つまり、防食剤がベンゾトリアゾール類であるのも好ましい。
ベンゾトリアゾール類は、例えば、更に置換基を含有してもよいアルキル基、更に置換基を含有してもよいアリール基、ハロゲン原子(フッ素原子、塩素原子、臭素原子、又は、ヨウ素原子等)、更に置換基を含有してもよいアミノ基、ニトロ基、更に置換基を含有してもよいアルコキシ基、及び、ヒドロキシル基からなる群から選択される1種以上の置換基によって置換されていてもよいベンゾトリアゾールが挙げられる。
上記アリール基の炭素数は、6~22が好ましく、6~14がより好ましく、6~10が更に好ましい。上記好ましい炭素数は、上記アリール基が含有し得る置換基中の炭素原子の数も計上した数を意図する。
上記アルコキシ基の炭素数は、1~12が好ましく、1~6がより好ましく、1~3が更に好ましい。上記好ましい炭素数は、上記アルコキシ基が含有し得る置換基中の炭素原子の数も計上した数を意図する。
上記アミノ基、における、更に含有してもよい置換基としては、例えば、炭素数1~6のアルキル基が挙げられる。
ベンゾトリアゾールの1位、4位、及び、5位以外にも置換基が置換していてもよいし置換していなくてもよい。
ベンゾトリアゾールが含有する置換基の好ましい例は上述の通りである。
中でも、1位にアミノ基が置換しているベンゾトリアゾール、又は、5位にアルキル基が置換しているベンゾトリアゾールが好ましい。
ベンゾトリアゾール類は、無置換のベンゾトリアゾールであるのも好ましい。
中でも、防食剤は、ベンゾトリアゾール、1-アミノ-ベンゾトリアゾール、又は、5-メチル-1H-ベンゾトリアゾールがより好ましく、5-メチル-1H-ベンゾトリアゾールが更に好ましい。
防食剤は1種のみを用いても、2種以上を用いてもよい。防食剤を2種以上用いる場合は、その合計量が上記範囲内であることが好ましい。
本発明の処理液は有機溶剤を含有してもよい。
有機溶剤は、水溶性の有機溶剤でもよい。
有機溶剤が水溶性であるとは、25℃の水と有機溶剤とが、任意の割合で混和(溶解)できることを意図する。
有機溶剤としては、アルコール系溶剤、ケトン系溶剤、エステル系溶剤、エーテル系溶剤(例えば、グリコールジエーテル)、スルホン系溶剤、スルホキシド系溶剤、ニトリル系溶剤、及び、アミド系溶剤等が挙げられる。
これらの溶剤は水溶性であってもよい。
中でも、処理液は、アルコール系溶剤、ケトン系溶剤、エステル系溶剤、及び、エーテル系溶剤からなる群から選択される1種以上の有機溶剤を含有するのが好ましい。
中でも、アルコール系溶剤は、グリコールモノエーテル又は飽和脂肪族一価アルコールが好ましい。
これらの中でも、エチレングリコールモノブチルエーテルが好ましい。
有機溶剤は1種のみを用いても、2種以上を用いてもよい。有機溶剤を2種以上用いる場合は、その合計量が上記範囲内であることが好ましい。
処理液は、ヒドロキシルアミンとは異なる還元剤を含有していてもよい。なお、ヒドラジン類、キレート剤、及び、防食剤は、ヒドロキシルアミンとは異なる還元剤には含まれない。
ヒドロキシルアミンとは異なる還元剤は特に制限されないが、OH基若しくはCHO基を含有する化合物、又は、硫黄原子を含有する化合物等の還元性物質が好ましい。上記還元剤は、酸化作用を有し、ヒドロキシルアミンを分解する原因となるOH-イオン又は溶存酸素等を酸化する機能を有する。
OH基若しくはCHO基を含有する化合物、又は、硫黄原子を含有する化合物等の還元性物質のなかでも、式(4)で表される化合物、及び、硫黄原子を含有する化合物からなる群より選ばれる1種が好ましい。
また、上記R4a~R4eで表されるヘテロ原子を含有する炭化水素基としては、上述した炭化水素基中の-CH2-が、例えば-O-、-S-、-CO-、-SO2-及び-NRa-からなる群より選択されるいずれか1種又はこれらの複数を組み合わせた2価の基で置換された基が挙げられる。上記Raは、水素原子又は炭素数1~20の炭化水素基(炭素数1~5のアルキル基が好ましい。)を表す。
ヒドロキシル基を2個以上有する式(4)で表される化合物としては、例えば、カテコール、レゾルシノール、tert-ブチルカテコール、及び、4,4’-ジヒドロキシフェニル-2,2-プロパンが挙げられる。また、ヒドロキシル基を3個以上有する式(4)で表される化合物としては、例えば、没食子酸が挙げられる。
処理液は、フッ化物を含有していてもよい。フッ化物は、残渣物の分解及び可溶化を促進する。
フッ化物は特に制限されないが、フッ化水素酸(HF)、フルオロケイ酸(H2SiF6)、フルオロホウ酸、フルオロケイ酸アンモニウム塩((NH4)2SiF6)、ヘキサフルオロリン酸テトラメチルアンモニウム、フッ化アンモニウム、フッ化アンモニウム塩、重フッ化アンモニウム塩、式NR4BF4及びPR4BF4でそれぞれ表されるテトラフルオロホウ酸第4級アンモニウム及びテトラフルオロホウ酸第4級ホスホニウム、並びに、テトラフルオロホウ酸テトラブチルアンモニウム(TBA-BF4)が挙げられる。
なお、上述の式NR4BF4及びPR4BF4でそれぞれ表されるテトラフルオロホウ酸第4級アンモニウム(例えば、テトラフルオロホウ酸テトラメチルアンモニウム、テトラフルオロホウ酸テトラエチルアンモニウム、テトラフルオロホウ酸テトラプロピルアンモニウム、テトラフルオロホウ酸テトラブチルアンモニウム)及びテトラフルオロホウ酸第4級ホスホニウムにおいて、Rは、互いに同種又は異種であってよく、水素、直鎖、分岐、又は環状のC1~C6アルキル基(例えば、メチル基、エチル基、プロピル基、ブチル基、ペンチル基、ヘキシル基)、並びに、直鎖又は分岐のC6~C10アリール基(例えば、ベンジル基)である。フッ化物は単独でも2種類以上適宜組み合わせて用いてもよい。
処理液がフッ化物を含有する場合、フッ化物の含有量は、処理液全質量に対して、0.01~30質量%が好ましく、0.1~15質量%がより好ましい。
処理液は、金属成分を含有していてもよい。
金属成分としては、金属粒子及び金属イオンが挙げられ、例えば、金属成分の含有量という場合、金属粒子及び金属イオンの合計含有量を示す。
処理液は、金属粒子及び金属イオンのいずれか一方が含有してもよく、両方を含有してもよい。処理液は、金属粒子及び金属イオンの両方を含有するのが好ましい。
金属成分は、金属原子を1種含有してもよいし、2種以上含有してもよい。
金属粒子は、単体でも合金でもよく、金属が有機物と会合した形態で存在していてもよい。
金属成分は、処理液に含まれる各成分(原料)に不可避的に含まれている金属成分でもよいし、処理液の製造、貯蔵、及び/又は、移送時に不可避的に含まれる金属成分でもよいし、意図的に添加してもよい。
処理液は、上述した成分以外のpH調整剤を含有していてもよい。pH調整剤としては、酸化合物及び塩基化合物が挙げられる。
酸化合物としては、例えば、酢酸、過塩素酸、次亜塩素酸、及び、過ヨウ素酸が挙げられる。
塩基化合物としては、例えば、アンモニア水、ヒドロキシルアミンともヒドラジン類とも異なるアミン化合物、及び、四級水酸化アンモニウム塩が挙げられる。
なお、ヒドロキシルアミンともヒドラジン類とも異なるアミン化合物としては、環状化合物(環状構造を含有する化合物)が挙げられる。環状化合物としては、例えば、後述する環状構造を含有するアミン化合物が挙げられる。
なお、ヒドロキシルアミンともヒドラジン類とも異なるアミン化合物中に、四級水酸化アンモニウム塩は包含されない。
環状構造を含有するアミン化合物において、アミノ基は、上記環状構造中及び上記環状構造外のいずれか一方のみに存在していても、両方に存在していてもよい。
環状構造を含有するアミン化合物としては、例えば、テトラヒドロフルフリルアミン、N-(2-アミノエチル)ピペラジン、1,8-ジアザビシクロ[5.4.0]-7-ウンデセン、1,4-ジアザビシクロ[2.2.2]オクタン、ヒドロキシエチルピペラジン、ピペラジン、2-メチルピペラジン、トランス-2,5-ジメチルピペラジン、シス-2,6-ジメチルピペラジン、2-ピペリジンメタノール、シクロヘキシルアミン、及び、1,5-ジアザビシクロ[4,3,0]-5-ノネンが挙げられる。
なかでも、上記アミン化合物として、テトラヒドロフルフリルアミン、N-(2-アミノエチル)ピペラジン、1,8-ジアザビシクロ[5.4.0]-7-ウンデセン、又は、1,4-ジアザビシクロ[2.2.2]オクタンが好ましい。
処理液がヒドロキシルアミンともヒドラジン類とも異なるアミン化合物を含有する場合、その含有量は、処理液の全質量に対して、0.1~50質量%が好ましく、0.5~30質量%がより好ましい。
水溶性アミンのpkaは、室温で、7.5~13.0であることが好ましい。なお、本明細書において、水溶性アミンとは、室温で1Lの水中に50g以上溶解し得るアミンを意図する。また、水溶性アミンとして、アンモニア水は含めない。
pKaが7.5~13である水溶性アミンとしては、例えば、ジグリコールアミン(DGA)(pKa=9.80)、メチルアミン(pKa=10.6)、エチルアミン(pKa=10.6)、プロピルアミン(pKa=10.6)、ブチルアミン(pKa=10.6)、ペンチルアミン(pKa=10.0)、エタノールアミン(pKa=9.3)、プロパノールアミン(pKa=9.3)、ブタノールアミン(pKa=9.3)、メトキシエチルアミン(pKa=10.0)、メトキシプロピルアミン(pKa=10.0)、ジメチルアミン(pKa=10.8)、ジエチルアミン(pKa=10.9)、ジプロピルアミン(pKa=10.8)、トリメチルアミン(pKa=9.80)、及び、トリエチルアミン(pKa=10.72)が挙げられる。
また、水溶性アミンとして、無置換ヒドロキシルアミン及びヒドロキシルアミン誘導体を使用してもよい。
なお、本明細書における水溶性アミンのpkaは、水中における酸解離定数である。水中における酸解離定数は、スペクトロメーターと電位差測定の組み合わせにより測定できる。
本明細書において、処理液のpHは、室温(25℃)において、(株)堀場製作所製、F-51(商品名)で測定した値である。
pH調整剤の含有量は、処理液を目的のpHにできるように適宜設定すればよい。
上記処理液の製造方法は特に制限されず、公知の製造方法が使用できる。例えば、水、ヒドロキシルアミン、及び、ヒドラジン類(又はその水溶液等)を混合する方法が挙げられる。なお、上記成分を混合する際に、必要に応じて、他の任意成分(第1アニオン及び/又は第2アニオンを含有する物質等)を更に混合してもよい。
また、処理液を製造する際には、必要に応じて、フィルターを用いて処理液をろ過して精製してもよい。
また、処理液は、コバルト原子を含有するコバルト含有物、及び、コバルト原子以外の他の金属原子を含有する金属含有物を含有する被処理物に対して使用されるのも好ましい。
処理液は、容器に収容されて使用時まで保管してもよい。
このような容器と、容器に収容された処理液とをあわせて処理液収容体という。保管された処理液収容体からは、処理液が取り出され使用される。また、処理液は、処理液収容体として運搬してもよい。
容器の内壁は、ポリエチレン樹脂、ポリプロピレン樹脂及びポリエチレン-ポリプロピレン樹脂からなる群より選択される1種以上の樹脂、若しくは、これとは異なる樹脂から形成されることが好ましい。また、容器の内壁は、ステンレス、ハステロイ、インコネル及びモネル等、防錆及び金属溶出防止処理が施された金属から形成されることも好ましい。
内壁がフッ素系樹脂である容器としては、Entegris社製 FluoroPurePFA複合ドラム等が挙げられる。また、特表平3-502677号公報の第4頁等、国際公開第2004/016526号パンフレットの第3頁等、及び、国際公開第99/46309号パンフレットの第9頁及び16頁等に記載の容器も用いることができる。
上記電解研磨された金属材料の製造に用いられる金属材料は、クロム及びニッケルからなる群から選択される少なくとも1種を含有し、クロム及びニッケルの含有量の合計が金属材料全質量に対して25質量%超である金属材料であることが好ましく、例えば、ステンレス鋼、及び、ニッケル-クロム合金が挙げられる。
金属材料におけるクロム及びニッケルの含有量の合計は、金属材料全質量に対して、30質量%以上が好ましい。
なお、金属材料におけるクロム及びニッケルの含有量の合計の上限値としては特に制限されないが、金属材料全質量に対して、90質量%以下が好ましい。
オーステナイト系ステンレス鋼としては、例えば、SUS(Steel Use Stainless)304(Ni含有量8質量%、Cr含有量18質量%)、SUS304L(Ni含有量9質量%、Cr含有量18質量%)、SUS316(Ni含有量10質量%、Cr含有量16質量%)、及び、SUS316L(Ni含有量12質量%、Cr含有量16質量%)が挙げられる。
ニッケル-クロム合金としては、例えば、ハステロイ(商品名、以下同じ。)、モネル(商品名、以下同じ)、及び、インコネル(商品名、以下同じ)が挙げられる。より具体的には、ハステロイC-276(Ni含有量63質量%、Cr含有量16質量%)、ハステロイ-C(Ni含有量60質量%、Cr含有量17質量%)、及び、ハステロイC-22(Ni含有量61質量%、Cr含有量22質量%)が挙げられる。
また、ニッケル-クロム合金は、必要に応じて、上記した合金の他に、更に、ホウ素、ケイ素、タングステン、モリブデン、銅、又は、コバルトを含有していてもよい。
なお、バフ研磨は、電解研磨の前に行われることが好ましい。
また、金属材料は、研磨砥粒のサイズ等の番手を変えて行われる複数段階のバフ研磨、酸洗浄、及び磁性流体研磨等を、1又は2以上組み合わせて処理されたものであってもよい。
処理液は、製造後にガロン瓶又はコート瓶等の容器にボトリングし、輸送又は保管されてもよい。
また、処理液は、濃縮液として準備してもよい。処理液を濃縮液とする場合には、その濃縮倍率は、構成される組成により適宜決められるが、5~2000倍であることが好ましい。つまり、濃縮液は、5~2000倍に希釈して用いられる。
本発明の処理液を用いた被処理物の処理方法(以下、単に「本処理方法」ともいう。)において、上記処理液は、典型的には、金属を含有する材料である金属系材料を含有する被処理物に対して接触させて使用できる。この際、被処理物は、金属系材料を複数種類含有してもよい。また、処理液が、複数種類含有されていてもよい金属系材料のうちの少なくとも一種を溶解するのも好ましい。
金属系材料中の、金属原子の含有量は、金属系材料の全質量に対して、30~100質量%が好ましく、40~100質量がより好ましく、52~100質量%が更に好ましい。
金属系材料としては、例えば、コバルト含有物及び金属含有物等が挙げられる。コバルト含有物及び金属含有物の詳細は後述する。
つまり、処理液は、例えば、エッチング処理液であってもよい。
この場合、処理液は、コバルト含有物のみをエッチングする用途に使用されてもよいし、コバルト含有物と金属含有物との両方をエッチングする用途に使用されてもよい。
図1では被処理物が1つのコバルト含有物部を含有する態様について記載したが、この態様には限定されず、例えば、図2に示すように、基板12と、基板12上に配置された複数の穴部を含有する絶縁膜14と、絶縁膜14の各穴部の内壁に沿って層状に配置された金属含有物部16と、各穴部内に充填されたコバルト含有物部18とを含有する被処理物20であってもよい。つまり、被処理物は、複数個所にわたってコバルト含有物を有し、かつ、複数個所にわたって金属含有物を含有する態様であってもよい。
半導体基板を構成する材料としては、例えば、ケイ素、ケイ素ゲルマニウム、及び、GaAs等の第III-V族化合物、又は、それらの任意の組合せが挙げられる。
基板の大きさ、厚さ、形状、及び、層構造等は、特に制限はなく、所望に応じ適宜選択できる。
図1及び図2において絶縁膜は穴部を含有するが、この態様に制限されず、溝部を含有する絶縁膜であってもよい。
コバルト含有物中の、コバルト原子の含有量は、コバルト含有物の全質量に対して、50~100質量%が好ましく、80~100質量がより好ましく、99~100質量%が更に好ましい。
金属含有物は、上記他の金属原子を含有していていればよく、例えば、金属単体、合金、酸化物、及び、窒化物が挙げられる。
金属含有物としては、処理液の効果がより優れる点で、チタン単体、チタン合金、チタン酸化物、チタン窒化物、タンタル単体、タンタル合金、タンタル酸化物、又は、タンタル窒化物が好ましい。
コバルト含有物及び金属含有物が膜状である場合、その厚みは特に制限されず、用途に応じて適宜選択すればよく、例えば、50nm以下が好ましく、20nm以下がより好ましく、10nm以下が更に好ましい。
コバルト含有物及び金属含有物は、基板の片側の主面上にのみに配置されていてもよいし、両側の主面上に配置されていてもよい。また、コバルト含有物及び金属含有物は、基板の主面全面に配置されていてもよいし、基板の主面の一部に配置されていてもよい。
なお、被処理物が、コバルト含有物に代えて、ルテニウム含有物、タングステン含有物、モリブデン含有物、アルミ含有物、又は、銅含有物を含有する場合、上述の金属含有物における「他の金属原子」も、それぞれ、ルテニウム原子以外の他の金属原子、タングステン原子以外の他の金属原子、モリブデン原子以外の他の金属原子、アルミ原子以外の他の金属原子、及び、銅原子以外の他の金属原子となる。この場合においても金属含有物としては、チタン単体、チタン合金、チタン酸化物、チタン窒化物、タンタル単体、タンタル合金、タンタル酸化物、又は、タンタル窒化物が好ましい。
基板は、曝露された集積回路構造、例えば金属配線及び誘電材料等の相互接続機構を含有していてもよい。相互接続機構に使用する金属及び合金としては、例えば、アルミニウム、銅アルミニウム合金、銅、チタン、タンタル、コバルト、ケイ素、窒化チタン、窒化タンタル、及び、タングステンが挙げられる。基板は、酸化ケイ素、窒化ケイ素、炭化ケイ素、及び/又は、炭素ドープ酸化ケイ素の層を含有していてもよい。
本発明の被処理物の処理方法のより具体的な例としては、少なくともコバルト含有物を含有する被処理物と、上記処理液とを接触させて、コバルト含有物を溶解させる方法が挙げられる。このような被処理物の処理方法を、本発明の被処理物の処理方法の第1態様ともいう。
被処理物と処理液とを接触させる方法は特に制限されず、例えば、タンクに入れた処理液中に被処理物を浸漬する方法、被処理物上に処理液を噴霧する方法、被処理物上に処理液を流す方法、及び、それらの任意の組み合わせが挙げられる。中でも、被処理物を処理液に浸漬する方法が好ましい。
機械式撹拌方法としては、例えば、被処理物上で処理液を循環させる方法、被処理物上で処理液を流過又は噴霧させる方法、及び、超音波又はメガソニックにて処理液を撹拌する方法が挙げられる。
処理時間(処理液と被処理物との接触時間)は特に制限されないが、0.25~10分間が好ましく、0.5~2分間がより好ましい。
処理の際の処理液の温度は特に制限されないが、20~75℃が好ましく、20~65℃がより好ましい。
被処理物が、コバルト含有物に加えて、金属含有物を含有する場合、本処理によって、金属含有物は、コバルト含有物とともに溶解されてもよいし、溶解されなくてもよい。金属含有物が溶解される場合、金属含有物は、意図的に溶解されてもよいし、不可避的に溶解されてもよい。
金属含有物を、意図的には溶解しない場合、金属含有物が不可避的に溶解される量は少ないことが好ましい。金属含有物を意図的には溶解しない場合において、金属含有物が不可避的に溶解される量が少ないことを、処理液が、その金属含有物に対して部材耐性が優れるともいう。
また、本発明の被処理物の処理方法の他の態様としては、以下の第2態様が挙げられる。
すなわち、金属層を含有する被処理物に対して、酸化処理を施して、上記金属層の表層を酸化させて金属酸化層とする工程Aと、上記工程Aで得られた被処理物と、処理液とを接触させて、上記金属酸化層を溶解させる工程Bと、を含有する被処理物の処理方法である。
第2態様は、第1態様の一形態であってもよい。
金属酸化層は、金属単体又は合金の酸化物であり、コバルト酸化物、コバルト合金の酸化物、ルテニウム酸化物、ルテニウム合金の酸化物、タングステン酸化物、タングステン合金の酸化物、モリブデン酸化物、モリブデン合金の酸化物、アルミ酸化物、アルミ合金の酸化物、銅酸化物、又は、銅合金の酸化物からなる層であるのが好ましく、コバルト酸化物又はコバルト合金の酸化物からなる層であるのがより好ましく、コバルト酸化物からなる層であるのが更により好ましい。
金属酸化層の厚みは、例えば、1~10原子層分である。なお、金属及び酸化金属の1原子層の厚みは、1nm以下(例えば、0.3nm~0.4nm)である。つまり、酸化処理は、金属層の表層の、例えば、1~10原子層分を酸化させて金属酸化層とする処理である。
金属酸化層は、金属層よりも処理液に対して溶解性が高い(エッチングされやすい)場合が多い。
つまり、第2態様では、工程Aにおいて金属層の表面を薄い金属酸化層とし、工程Bにおいて処理液を用いて上記金属酸化層(及び、金属酸化層の下層に存在する金属層が不可避的に溶解され得る部分)のみを除去することで、被処理物が含有する金属層のごく薄い表面のみを除去(溶解)し得る。
更に、工程Aと工程Bとを交互に繰り返し実施することで、エッチング量を高精度に制御し得る。
工程Aと工程Bとを交互に行う場合は、工程A及び工程Bはそれぞれ1~20回実施されることが好ましい。
酸化処理は1種を実施してもよいし、2種以上を実施してもよい。
上記酸化溶液とは、上記金属層の表層を酸化させられる溶液であればよい。なお、酸化溶液は、本発明の処理液以外が好ましい。
上記特定溶液は、中でも、水、過酸化水素水、APM、FPM、SPM、HPM、酸素溶存水、並びに、オゾン溶存水からなる群から選択される溶液が好ましい。
過酸化水素水の組成は、例えば、H2O2の含有量が過酸化水素水の全質量に対して、0.5~31質量%であり、3~15質量%がより好ましい。
APMの組成は、例えば、「アンモニア水:過酸化水素水:水=1:1:1」~「アンモニア水:過酸化水素水:水=1:3:45」の範囲内(質量比)が好ましい。
FPMの組成は、例えば、「フッ酸:過酸化水素水:水=1:1:1」~「フッ酸:過酸化水素水:水=1:1:200」の範囲内(質量比)が好ましい。
SPMの組成は、例えば、「硫酸:過酸化水素水:水=3:1:0」~「硫酸:過酸化水素水:水=1:1:10」の範囲内(質量比)が好ましい。
HPMの組成は、例えば、「塩酸:過酸化水素水:水=1:1:1」~「塩酸:過酸化水素水:水=1:1:30」の範囲内(質量比)が好ましい。
なお、これらの好ましい組成比の記載は、アンモニア水は28質量%アンモニア水、フッ酸は49質量%フッ酸、硫酸は98質量%硫酸、塩酸は37質量%塩酸、過酸化水素水は30質量%過酸化水素水である場合における組成比を意図する。
また、体積比は、室温における体積を基準とする。
好適範囲としての[「A:B:C=x:y:z」~「A:B:C=X:Y:Z」]という記載は、[「A:B=x:y」~「A:B=X:Y」]、[「B:C=y:z」~「B:C=Y:Z」]、及び、[「A:C=x:z」~「A:C=X:Z」]の範囲のうちの少なくとも1個(好ましくは2個、より好ましくは全部)を満たすのが好ましいことを示す。
酸素溶存水の組成は、例えば、O2の含有量が酸素溶存水の全質量に対して、1~200質量ppmの水溶液である。
オゾン溶存水の組成は、例えば、O3の含有量がオゾン溶存水の全質量に対して、1~200質量ppmの水溶液である。
過塩素酸は、例えば、HClO4の含有量が溶液の全質量に対して0.001~60質量%の水溶液である。
硝酸は、例えば、HNO3の含有量が溶液の全質量に対して0.001~60質量%の水溶液である。
被処理物と酸化溶液との接触時間は、例えば、0.25~10分間が好ましく、0.5~5分間がより好ましい。
酸化溶液の温度は、20~75℃が好ましく、20~60℃がより好ましい。
ガス処理において、被処理物に接触させる酸化ガスは、中でも、酸素ガス、又は、オゾンガスが好ましい。被処理物に酸素ガス、又は、オゾンガスを接触させる場合、酸素雰囲気下、オゾン雰囲気下、又は、酸素及びオゾンの混合ガス雰囲気下で接触させるのも好ましい。
ガス処理においては、酸化ガスを接触させながら被処理物を加熱(例えば、40~200℃での加熱)するのも好ましい。
中でも、ガス処理は、被処理物に対して、オゾンガスを接触させるオゾン処理、又は、酸素雰囲気下で加熱する酸素中加熱処理が好ましい。
上記オゾン処理では、オゾン雰囲気下でオゾンガスを被処理物に接触させてもよいし、オゾンガスとその他の気体(例えば酸素ガス)との混合ガス雰囲気下でオゾンガスを被処理物に接触させてもよい。また、オゾン処理は、オゾンガスを接触させながら被処理物を加熱する処理であってもよい。
また、工程A(特に液処理をする場合)において、被処理物の金属層の一部が意図的又は不可避的に除去されてもよい。
工程Bにおいて被処理物と処理液とを接触させる方法制限されず、被処理物と酸化溶液とを接触させる方法と同様の例が挙げられる。
被処理物と処理液との接触時間は、例えば、0.25~10分間が好ましく、0.5~5分間がより好ましい。
処理液の温度は、20~75℃が好ましく、20~60℃がより好ましい。
工程Bにおいて、金属層(例えば、表面を覆っていた金属酸化層の除去がされて表層に露出した金属層)の一部又は全部が意図的又は不可避的に除去されてもよい。
工程Bにおいて、被処理物は、金属酸化層及び表面に金属酸化層を形成している金属層以外のその他の金属系材料を含有していてもよく、このような金属系材料の一部又は全部が意図的又は不可避的に除去されてもよい。
なお、上記金属層及び/又は上記その他の金属系材料を、意図的には溶解しない場合、上記金属層及び/又は上記その他の金属系材料が不可避的に溶解される量は少ないことが好ましい。
本発明の被処理物の処理方法の他の態様(第3態様)としては、金属系材料を含有する被処理物にドライエッチング処理を施した後、上記被処理物と処理液とを接触させて、ドライエッチング残渣物を除去する態様が挙げられる。
上記本態様における被処理物が含有する金属系材料は1種単独でも2種以上でもよい。1種単独又は2種以上である金属系材料のうち、少なくとも1種は、コバルト含有物、テニウム含有物、モリブデン含有物、アルミ含有物、又は、銅含有物であるのが好ましく、コバルト含有物であるのがより好ましい。
つまり、本発明の被処理物の処理方法の第3態様としては、コバルト原子を含有するコバルト含有物を含有する被処理物にドライエッチング処理を施した後、上記被処理物と処理液とを接触させて、ドライエッチング残渣物を除去する態様が好ましい。
本態様で、処理液と接触する被処理物は、金属系材料を含有する。また、本態様では、被処理物は、ドライエッチング処理が施された後に処理液と接触させられる。そのため、処理液と接触する時点での被処理物は、表面上にドライエッチング残渣物を含有する。本態様では、このような被処理物の表面上に存在するドライエッチング残渣物を除去する。
このような被処理物の処理方法を、本発明の被処理物の処理方法の第3態様ともいう。
なお、第3態様は、上述の第1態様における、被処理物の構成、及び、処理の目的を、特に限定した一形態であってもよい。
本発明の処理液はこのような被処理物の洗浄用途(残渣物除去用途)にも好適に使用できる。
図3に示す被処理物30は、基板32上に、金属含有膜34、エッチング停止層36、層間絶縁膜38、メタルハードマスク40をこの順に備え、ドライエッチング工程等を経たことで所定位置に金属含有膜34が露出するホール42が形成されている。つまり、図3に示す被処理物は、基板32と、金属含有膜34と、エッチング停止層36と、層間絶縁膜38と、メタルハードマスク40とをこの順で備え、メタルハードマスク40の開口部の位置において、その表面から金属含有膜34の表面まで貫通するホール42を備える積層物である。ホール42の内壁44は、エッチング停止層36、層間絶縁膜38及びメタルハードマスク40からなる断面壁44aと、露出された金属含有膜34からなる底壁44bとで構成され、ドライエッチング残渣物46が付着している。
なお、被処理物におけるメタルハードマスクは、被処理物が更に加工された後でバリアメタルとなってもよい。言い換えると、後の工程でバリアメタルとなる層を、ドライエッチング工程ではメタルハードマスクとして利用してもよい。つまり、バリアメタルをメタルハードマスクとして使用してもよい。
ここで、例えば、上記金属含有膜34及び上記メタルハードマスク40の少なくとも一方がコバルト含有物であるのが好ましい。中でも、上記金属含有膜34がコバルト含有物であり上記メタルハードマスク40が金属含有物であるか、又は、上記金属含有膜34が金属含有物であり上記メタルハードマスク40がコバルト含有物であるのが好ましい。
中でも、上記金属含有膜34がコバルト含有物であり上記メタルハードマスク40が金属含有物であるのが好ましい。
層間絶縁膜は公知の材料が使用できる。
ドライエッチング残渣物は、有機物を含有する主成分とする有機残渣物であってもよい。有機残渣物は、有機物の含有量が50質量%以上である残渣物である。有機残渣物は、実質的に、金属含有物及び/又はコバルト含有物を含有しない残渣物であってもよい。
また、ドライエッチング残渣物は、金属成分を主成分として含有してもよく、金属含有物及び/又はコバルト含有物を含有する金属残渣物であってもよい。金属残渣物は、金属成分の含有量が50質量%超である残渣物である。金属残渣物は、実質的に、有機物を含有しない残渣物であってもよい。
処理液と被処理物との接触方法は、第1態様で上述したのと同様である。
処理液と被処理物とを接触させることで、被処理物上のドライエッチング残渣物が除去される。この場合、同時に、金属系材料(例えば、コバルト含有物等。好ましくは金属含有膜34であるコバルト含有物)が溶解してもよい。この際、金属系材料(コバルト含有物等)の溶解量に制限はない。金属系材料(コバルト含有物等)の溶解は、ホール42の底壁44bにおける金属含有膜34(コバルト含有物等)の一部又は全部を除去するための意図的な溶解であってもよいし、処理液が金属系材料(コバルト含有物等)と接触したことで生じる不可避的な溶解であってもよい。
例えば、上述の第1態様、第2態様、又は、第3態様における被処理物の処理方法は、上記各態様の説明中で記載した手順の後に、更に、リンス工程を含有してもよい。
また、上記リンス工程が、第2態様における工程Aと工程Bとの間に含有されてもよい。
FPM、SPM、APM、及び、HPMとして好ましい条件は、例えば、上述の特定溶液として使用される、FPM、SPM、APM、及び、HPMとしての好ましい条件と同様である。
なお、フッ酸、硝酸、過塩素酸、及び、塩酸は、それぞれ、HF、HNO3、HClO4、及び、HClが、水に溶解した水溶液を意図する。
オゾン水、二酸化炭素水、及び、水素水は、それぞれ、O3、CO2、及び、H2を水に溶解させた水溶液を意図する。
リンス工程の目的を損なわない範囲で、これらのリンス液を混合して使用してもよい。また、リンス液には有機溶剤が含まれていてもよい。
接触させる方法としては、タンクに入れたリンス液中に基板を浸漬する方法、基板上にリンス液を噴霧する方法、基板上にリンス液を流す方法、又はそれらの任意の組み合わせた方法で実施される。
処理の際のリンス液の温度は特に制限されないが、例えば、一般に、16~60℃が好ましく、18~40℃がより好ましい。リンス液として、SPMを用いる場合、その温度は90~250℃が好ましい。
乾燥時間は、用いる特定の方法に応じて変わるが、通例は30秒~数分程度である。
その他の工程としては、例えば、金属配線、ゲート構造、ソース構造、ドレイン構造、絶縁層、強磁性層及び/又は非磁性層等の各構造の形成工程(層形成、エッチング、化学機械研磨、変成等)、レジストの形成工程、露光工程及び除去工程、熱処理工程、洗浄工程、並びに、検査工程等が挙げられる。
本処理方法において、バックエンドプロセス(BEOL:Back end of the line)中で行っても、フロントエンドプロセス(FEOL:Front end of the line)中で行ってもよい。
なお、処理液の適用対象は、例えば、NAND、DRAM(Dynamic Random Access Memory)、SRAM(Static Random Access Memory)、ReRAM(Resistive Random Access Memory)、FRAM(登録商標)(Ferroelectric Random Access Memory)、MRAM(Magnetoresistive Random Access Memory)、又は、PRAM(Phase change Random Access Memory)等であってもよいし、ロジック回路又はプロセッサ等であってもよい。
なお、実施例中、「%」の記載は特に断りのない限り「質量%」を意味し、「ppm」の記載は特に断りのない限り「質量ppm」を意味する。
下記に示す成分を所定の配合で混合して、各試験に適用する処理液をそれぞれ調製した。
以下に示す各処理液に使用される各原料は、高純度グレードを用い、更に事前に蒸留、イオン交換、ろ過、又は、これらを組み合わせて精製した。
・HA:ヒドロキシルアミン
・ヒドラジン
・ピラゾール
・カルボヒドラジド
・セミカルバジド
・チオセミカルバジド
・モノメチルヒドラジド
・t-ブチルヒドラジン
・ジメチルヒドラジン(1,1-ジメチルヒドラジン)
・アミノグアニジン
・メタノール
・イソプロピルアルコール
・1-ブタノール
・1,3-プロパンジオール
・エチレングリコール
・プロピレングリコール
・ジエチレングリコール
・ジプロピレングリコール
・3-メトキシ-3-メチル-1-ブタノール
・3-メトキシ-1-ブタノール
・1-メトキシ-2-ブタノール
・エチレングリコールモノメチルエーテル
・エチレングリコールモノエチルエーテル
・エチレングリコールモノブチルエーテル
・ジエチレングリコールモノメチルエーテル
・ジエチレングリコールモノブチルエーテル
・トリエチレングリコールモノメチルエーテル
・1-メトキシ-2-プロパノール
・アセトン
・シクロヘキサノン
・2-ブタノン
・エチルアセテート
・ブチルアセテート
・プロピレングリコールモノメチルエーテルアセテート
・ベンゾトリアゾール
・5-アミノテトラゾール
・5-フェニルベンゾトリアゾール
・1-アミノベンゾトリアゾール
・5-メチル-1H-ベンゾトリアゾール
・ベンゾトリアゾール-5-カルボン酸
・4-メチルベンゾトリアゾール
・ジエチレントリアミン5酢酸
・エチレンジアミン4酢酸
・トランス-1,2-ジアミノシクロヘキサン4酢酸
・シュウ酸
・マロン酸
・クエン酸
・メタンスルホン酸
・1-ヒドロキシエチリデン-1,1-ジホスホン酸
・ニトリロトリスメチレンホスホン酸
下記原料を適当量添加することで、所定量の第1アニオン及び/又は第2アニオンを処理液中に供給した。
・塩酸水溶液(HClaq:Cl-の供給源)
・亜硝酸/硝酸水溶液(HNO2/HNO3aq:NO2 -及びNO3 -の供給源)
・三酸化二窒素(N2O3:NO2 -の供給源)
・硝酸水溶液(HNO3aq:NO3 -の供給源)
・硫酸水溶液(H2SO4aq:SO4 2-の供給源)
・リン酸水溶液(H3PO4aq:PO4 3-の供給源)
上記亜硝酸/硝酸水溶液は、純水中でH2OとNO2とを反応させて作製した、硝酸と亜硝酸とを含有する水溶液である。
上記三酸化二窒素はH2Oに溶解して亜硝酸を生じ、NO2 -の供給源となる。
・水:超純水を蒸留、フィルターろ過、及び、イオン交換を繰り返し、第1アニオン及び第2アニオンが検出限界未満になるまで精製した水を用いた。
なお、上記検出限界は0.001質量ppm未満であった。検出に当たっては、必要に応じて、検出対象のサンプルから一部の水分を除去して目的物質を濃縮する等の処理を行ってから測定を行った。
・酢酸(酸性側に調整するために使用するpH調整剤)
・1,8-ジアザビシクロ[5.4.0]-7-ウンデセン(塩基性側に調整するために使用するpH調整剤)
処理液を所定のpHにするため、酢酸、及び、1,8-ジアザビシクロ[5.4.0]-7-ウンデセンの一方をpH調整剤として必要量添加した。
なお、pH調整剤の添加量はいずれの処理液でも、処理液の全質量に対して3.0質量%以下であった。
作製した実施例又は比較例の処理液を用いて、以下の試験を行った。
基板の表面に、レジスト膜、メタルハードマスク(TiN層)、エッチング停止層(Al2O3層)、Co層並びに層間絶縁層(ILD)がこの順で積層されている複層基板を準備した。この複層基板に対して、リソグラフィーによるパターン化処理、金属用プラズマエッチング装置を用いたエッチング処理、及び、酸素プラズマアッシングによるレジスト膜の除去処理を行い、評価試験用の複層基板(以下「試験片」とも記載する)を作製した。
各実施例及び各比較例の処理液を用いて、得られた試験片を洗浄(処理)した。
洗浄時間が経過後、試験片をすぐに処理液から取り出し、容量500mLのプラスチックビーカー中に充填され、穏やかに撹拌されている400mLのイオン交換水(水温17℃)に入れた。試験片をイオン交換水中に30秒間浸漬させた後、試験片をすぐに取り出して、17℃のイオン交換水流下で30秒間にわたってリンスした。
この窒素乾燥工程の後、プラスチック製ピンセットの保持部分から試験片を取り外し、試験片を、素子面を上にして蓋付きプラスチック製保管箱に入れ、保管した。
1:有機残渣物除去率が95%以上
2:有機残渣物除去率が80%以上95%未満
3:有機残渣物除去率が75%以上80%未満
4:有機残渣物除去率が50%以上75%未満
5:有機残渣物除去率が50%未満
次いで、各実施例及び各比較例の処理液を用いて保管試験を行い、各処理液の除去性能の経時安定性を評価した。
具体的には、まず、容量が250mLである高密度ポリエチレン製容器に200mLの各処理液を充填して、密閉した。処理液を充填した容器を、60℃の環境下で24時間保管(保管処理)した。
保管処理後の処理液を用いること以外は、上述の有機物残渣物除去性の評価方法に従って有機物残渣物除去性の評価試験を行った。保管処理を施す前の処理液を用いて求められた有機残渣物除去率を100%とした場合における、保管処理を施した後の処理液を用いて求められた有機残渣物除去率の維持率(=[保管処理を施した後の処理液を用いて求められた有機残渣物除去率]÷[保管処理を施す前の処理液を用いて求められた有機残渣物除去率]×100)を計算し、得られた維持率を以下の評価基準に従って分類し、各処理液の安定性を評価した。
なお、いずれの処理液を使用した場合でも、維持率が100%を超えることはなかった。
1:維持率が99%以上
2:維持率が95%以上99%未満
3:維持率が85%以上95%未満
4:維持率が75%以上85%未満
5:維持率が75%未満
市販のシリコンウエハ(直径:12インチ)の一方の表面上に、CVD(Chemical Vapor Deposition)法により金属コバルト層を形成した基板をそれぞれ準備した。金属コバルト層の厚さは20nmとした。
得られた基板を水に40℃で1分間浸漬した後、表に記載の各処理液に40℃で30秒間浸漬する処理を1サイクルとして、金属コバルトが10nm溶解するまでサイクルを繰り返し、処理を行った。
その後、処理後の、金属コバルト層の表面を走査型電子顕微鏡で観察して、処理液によって処理された被処理部の平滑性を1~10の10段階で評価した。
平滑性は「1」が最も良好な評価で、数字が大きくなるにしたがって不良な評価となる。具体的には、観察の結果、金属コバルト層の表面が滑らかで、ラフネスが見られない場合、その処理液における被処理物の平滑性を「1」として評価した。その上で、「10」に近づくに従って、ラフネスが見られるようになり、金属コバルト層の表面が粗くなっていくものとして評価した。「1~8」の評価は実用上好ましく使用可能なレベルであり、「9」の評価は実用上使用可能なレベルであり、「10」の評価は実用上問題があるレベルである。
基板(Si)上に、金属コバルト層、SiN膜、SiO2膜、及び、所定の開口部を含有するバリアメタル(TaN)をこの順で備える被処理物(処理前積層物)を形成した。得られた被処理物を使用し、バリアメタルをマスクとしてプラズマエッチング(ドライエッチング)を実施して、金属コバルト層が露出するまでSiN膜及びSiO2膜のエッチングを行い、ビアホールを形成し、試料1を製造した(図3参照)。この積層物の断面をSEM/EDX(エネルギー分散型X線解析装置付き走査型電子顕微鏡)で確認すると、ホール壁面にはコバルト等の金属を主成分とするプラズマエッチング残渣物(金属残渣物)が認められた。
そして、下記の手順により、金属残渣物除去性を評価した。まず、40℃に調温した各処理液に、用意した上記試料1の切片(約2.0cm×2.0cm)を1分間浸漬(処理)し、所定時間の経過後に試料1の切片を取り出し、直ちに超純水で水洗し、N2乾燥を行った。
洗浄性は「1」が良好な評価で、数字が大きくなるにしたがって不良な評価となる。具体的には、観察の結果、上記金属残渣物が完全に除去されていれば「1」として評価し、上記金属残渣物がほとんど除去されていない場合は「10」として評価した。「1~6」の評価は実用上好ましく使用可能なレベルであり、「7~9」の評価は実用上使用可能なレベルであり、「10」の評価は実用上問題があるレベルである。
以下に、一連の試験Xに使用した処理液の配合及び結果を表1a-1~1n-1、表1a-2~1n-2に示す。
表中、「%」は「質量%」を意味し、「ppm」は「質量ppm」を意味する。
「HA(%)」欄は、各処理液における、処理液全質量に対する、ヒドロキシアミンの含有量(質量%)を示す。
「キレート剤/含有量」、「ベンゾトリアゾール化合物/含有量」、「有機溶剤/含有量」欄は、上段は添加された各成分の種類を示し、下段は各成分の添加量(質量%)を示す。
「ヒドラジン類(対HA100部)」欄は、各処理液における、ヒドロキシルアミン100質量部に対する、ヒドラジン類の合計含有量(質量部)を示す。なお、ヒドラジン類を2種使用している場合、2種のヒドラジン類の各含有質量が等しくなるように調整している。
「アニオン(ppm)」欄は、各処理液における、処理液全質量に対する、各アニオンの含有量(質量ppm)を示す。
「第1アニオン含有量(対HA100部)」欄は、各処理液における、ヒドロキシルアミン100質量部に対する、第1アニオンの合計含有量(質量部)を示す。
「第1第2アニオン含有量(対HA100部)」欄は、各処理液における、ヒドロキシルアミン100質量部に対する、第1アニオンと第2アニオンとの合計含有量(質量部)を示す。
「pH」欄は、各処理液のpHを示す。
各処理液における表中に明記されない成分(残部)は、所定のpHを実現するために添加したpH調整剤と水とからなる。
表1a-1と表1a-2とは、それぞれ、実施例001~049における、処理液の配合と、試験結果とを分割して表示している。
例えば、実施例001の処理液は、ヒドロキシルアミンを処理液の全質量に対して0.1質量%含有し、ヒドラジン類としてヒドラジンを処理液の全質量に対して0.001質量ppm(ヒドロキシルアミンの100質量部に対して0.0001質量部)含有し、第1アニオンは含有しておらず、第2アニオンは含有しておらず、キレート剤は含有しておらず、防食剤は含有しておらず、有機溶媒は含有しておらず、残部はpHが9になるように添加したpH調整剤と水である。実施例001の処理液の試験結果は、有機残渣物除去性の評価が3であり、安定性の評価が3であり、金属残渣除去性の評価が9であり、平滑性の評価が3である。
表1b-1と以降と、表1b-2以降とも、それぞれ同様の関係である。
12 基板
14 絶縁膜
16 金属含有物部
18 コバルト含有物部
30 被処理物
32 基板
34 金属含有膜
36 エッチング停止層
38 層間絶縁膜
40 メタルハードマスク
42 ホール
46 ドライエッチング残渣物
44 内壁
44a 断面壁
44b 底壁
Claims (27)
- 水と、
ヒドロキシルアミンと、
ヒドラジン、ヒドラジン塩、及び、ヒドラジン誘導体からなる群から選択される1種以上のヒドラジン類と、を含有し、
前記ヒドロキシルアミン100質量部に対する、前記ヒドラジン類の合計含有量が1質量部以下である、処理液。 - 前記ヒドロキシルアミン100質量部に対する、前記ヒドラジン類の合計含有量が0.0001質量部以上である、請求項1に記載の処理液。
- 前記ヒドロキシルアミン100質量部に対する、前記ヒドラジン類の合計含有量が0.005~0.5質量部である、請求項1又は2に記載の処理液。
- 前記ヒドラジン誘導体が、一般式(A)で表される化合物、一般式(B)で表される化合物、ピラゾール環を有する化合物、及び、これらの塩からなる群から選択される1種以上である、請求項1~3のいずれか1項に記載の処理液。
H2N-N-RN 2 (A)
H2N-N=X (B)
一般式(A)中、2つのRNは、それぞれ独立に、水素原子又は置換基を表す。2つのRNが互いに結合して環を形成していてもよい。ただし、2つのRNの少なくとも一方は、水素原子以外である。
一般式(B)中、Xは二価の基を表す。 - 前記ヒドラジン類が、ヒドラジンを含有する、請求項1~4のいずれか1項に記載の処理液。
- 更に、Cl-、NO2 -、及び、NO3 -からなる群から選択される1種以上の第1アニオンを含有する、請求項1~5のいずれか1項に記載の処理液。
- Cl-、NO2 -、及び、NO3 -からなる3種の前記第1アニオンを含有する、請求項6に記載の処理液。
- 前記ヒドロキシルアミン100質量部に対する、前記第1アニオンの合計含有量が0.0001~30質量部である、請求項6又は7に記載の処理液。
- 更に、SO4 2-及びPO4 3-からなる群から選択される1種以上の第2アニオンを含有し、
前記ヒドロキシルアミン100質量部に対する、前記第1アニオンと前記第2アニオンとの合計含有量が0.0001~30質量部である、請求項6~8のいずれか1項に記載の処理液。 - NO2 -、及び、NO3 -の合計含有質量が、Cl-の含有質量よりも多い、請求項6~9のいずれか1項に記載の処理液。
- 更に、キレート剤を含有する、請求項1~10のいずれか1項に記載の処理液。
- 前記キレート剤が、カルボン酸基、ホスホン酸基、及び、スルホン酸基からなる群から選択される官能基を含有する、請求項11に記載の処理液。
- 前記キレート剤が、ジエチレントリアミン五酢酸、エチレンジアミン四酢酸、トランス-1,2-ジアミノシクロヘキサン四酢酸、シュウ酸、マロン酸、コハク酸、クエン酸、メタンスルホン酸、1-ヒドロキシエチリデン-1,1-ジホスホン酸、及び、ニトリロトリスメチレンホスホン酸からなる群から選択される1種以上である、請求項11又は12に記載の処理液。
- 更に、防食剤を含有する、請求項1~13のいずれか1項に記載の処理液。
- 前記防食剤が、ベンゾトリアゾール類である、請求項14に記載の処理液。
- 前記ベンゾトリアゾール類が、更に置換基を含有してもよいアルキル基、更に置換基を含有してもよいアリール基、ハロゲン原子、更に置換基を含有してもよいアミノ基、ニトロ基、更に置換基を含有してもよいアルコキシ基、及び、ヒドロキシル基からなる群から選択される1種以上の置換基によって置換されていてもよいベンゾトリアゾールである、請求項15に記載の処理液。
- 前記防食剤が、ベンゾトリアゾール、5-アミノテトラゾール、1-ヒドロキシベンゾトリアゾール、5-フェニルチオール-ベンゾトリアゾール、5-クロロベンゾトリアゾール、4-クロロベンゾトリアゾール、5-ブロモベンゾトリアゾール、4-ブロモベンゾトリアゾール、5-フルオロベンゾトリアゾール、4-フルオロベンゾトリアゾール、ナフトトリアゾール、トリルトリアゾール、5-フェニル-ベンゾトリアゾール、5-ニトロベンゾトリアゾール、4-ニトロベンゾトリアゾール、3-アミノ-5-メルカプト-1,2,4-トリアゾール、2-(5-アミノ-ペンチル)-ベンゾトリアゾール、1-アミノ-ベンゾトリアゾール、5-メチル-1H-ベンゾトリアゾール、ベンゾトリアゾール-5-カルボン酸、4-メチルベンゾトリアゾール、4-エチルベンゾトリアゾール、5-エチルベンゾトリアゾール、4-プロピルベンゾトリアゾール、5-プロピルベンゾトリアゾール、4-イソプロピルベンゾトリアゾール、5-イソプロピルベンゾトリアゾール、4-n-ブチルベンゾトリアゾール、5-n-ブチルベンゾトリアゾール、4-イソブチルベンゾトリアゾール、5-イソブチルベンゾトリアゾール、4-ペンチルベンゾトリアゾール、5-ペンチルベンゾトリアゾール、4-ヘキシルベンゾトリアゾール、5-ヘキシルベンゾトリアゾール、5-メトキシベンゾトリアゾール、5-ヒドロキシベンゾトリアゾール、ジヒドロキシプロピルベンゾトリアゾール、1-[N,N-ビス(2-エチルヘキシル)アミノメチル]-ベンゾトリアゾール、5-t-ブチルベンゾトリアゾール、5-(1’,1’-ジメチルプロピル)-ベンゾトリアゾール、5-(1’,1’,3’-トリメチルブチル)ベンゾトリアゾール、5-n-オクチルベンゾトリアゾール、及び、5-(1’,1’,3’,3’-テトラメチルブチル)ベンゾトリアゾールからなる群から選択される1種以上である、請求項14に記載の処理液。
- 更に、アルコール系溶剤、ケトン系溶剤、エステル系溶剤、及び、エーテル系溶剤からなる群から選択される1種以上の有機溶剤を含有する、請求項1~17のいずれか1項に記載の処理液。
- pHが6~11である、請求項1~18のいずれか1項に記載の処理液。
- コバルト原子を含有するコバルト含有物、及び、コバルト原子以外の他の金属原子を含有する金属含有物を含有する被処理物に対して使用される、請求項1~19のいずれか1項に記載の処理液。
- 前記コバルト含有物が、コバルト単体、コバルト合金、コバルト酸化物、又は、コバルト窒化物である、請求項20に記載の処理液。
- コバルト原子を含有するコバルト含有物を含有する被処理物と、請求項1~21のいずれか1項に記載の処理液とを接触させて、前記コバルト含有物を溶解させる、被処理物の処理方法。
- 金属層を含有する被処理物に対して、
水、過酸化水素水、アンモニア及び過酸化水素の混合水溶液、フッ酸及び過酸化水素水の混合水溶液、硫酸及び過酸化水素水の混合水溶液、塩酸及び過酸化水素水の混合水溶液、酸素溶存水、並びに、オゾン溶存水からなる群から選択される溶液を接触させる液処理、
オゾンガスを接触させるオゾン処理、
酸素雰囲気下で加熱する酸素中加熱処理、又は、
酸素ガスを用いたプラズマ処理、を施して、
前記金属層の表層を酸化させて金属酸化層とする工程Aと、
前記工程Aで得られた被処理物と、請求項1~19のいずれか1項に記載の処理液とを接触させて、前記金属酸化層を溶解させる工程Bと、を含有する被処理物の処理方法。 - 前記工程Aと前記工程Bとを交互に繰り返し実施する、請求項23に記載の被処理物の処理方法。
- 前記金属層が、コバルト単体又はコバルト合金であるコバルト含有物からなる、請求項23又は24に記載の被処理物の処理方法。
- 金属系材料を含有する被処理物にドライエッチング処理を施した後、
前記被処理物と請求項1~19のいずれか1項に記載の処理液とを接触させて、ドライエッチング残渣物を除去する、被処理物の処理方法。 - 前記金属系材料がコバルト原子を含有するコバルト含有物である、請求項26に記載の被処理物の処理方法。
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