WO2020040042A1 - Solution chimique et récipient pour solution chimique - Google Patents

Solution chimique et récipient pour solution chimique Download PDF

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Publication number
WO2020040042A1
WO2020040042A1 PCT/JP2019/032088 JP2019032088W WO2020040042A1 WO 2020040042 A1 WO2020040042 A1 WO 2020040042A1 JP 2019032088 W JP2019032088 W JP 2019032088W WO 2020040042 A1 WO2020040042 A1 WO 2020040042A1
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Prior art keywords
mass
content
oxide particles
chemical solution
metal component
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PCT/JP2019/032088
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English (en)
Japanese (ja)
Inventor
上村　哲也
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富士フイルム株式会社
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Application filed by 富士フイルム株式会社 filed Critical 富士フイルム株式会社
Priority to JP2020538347A priority Critical patent/JPWO2020040042A1/ja
Publication of WO2020040042A1 publication Critical patent/WO2020040042A1/fr
Priority to JP2022152895A priority patent/JP7416883B2/ja
Priority to JP2023220184A priority patent/JP2024026548A/ja

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Classifications

    • 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
    • G03F7/16—Coating processes; Apparatus therefor
    • 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
    • G03F7/30—Imagewise removal using liquid means
    • G03F7/32—Liquid compositions therefor, e.g. developers
    • 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
    • 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
    • G03F7/004—Photosensitive materials
    • G03F7/038—Macromolecular compounds which are rendered insoluble or differentially wettable
    • 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
    • G03F7/004—Photosensitive materials
    • G03F7/039—Macromolecular compounds which are photodegradable, e.g. positive electron resists

Definitions

  • the present invention relates to a drug solution and a drug solution container.
  • a semiconductor device by a wiring forming process including photolithography, a pre-wet solution, a resist solution (composition for forming a resist film), a developing solution, a rinsing solution, a stripping solution, and chemical mechanical polishing (CMP).
  • a chemical solution containing water and / or an organic solvent is used as a slurry, a cleaning solution after CMP, or a diluent thereof.
  • miniaturization of patterns has been progressing due to the progress of photolithography technology.
  • pattern miniaturization pattern formation using an ultraviolet light, a KrF excimer laser, an ArF excimer laser, EUV (extreme ultraviolet light), or the like as an exposure light source has been attempted.
  • EUV extreme ultraviolet light
  • Patent Literature 1 discloses, as a conventional chemical solution used for pattern formation, “a method for producing an organic treatment solution for patterning a chemically amplified resist film capable of reducing generation of particles in a pattern formation technique (paragraph [0010]). ) "Is disclosed.
  • the present inventors have conducted intensive studies to solve the above-described problems, and as a result, have found that the above-described problems can be solved by the following configuration.
  • a chemical solution containing an organic solvent and a metal component contains titanium oxide particles, and titanium ions, To the content of titanium ions, the mass ratio of the content of titanium oxide particles is 10 0 to 10 12, the drug solution.
  • the chemical according to (1) wherein the content of titanium ions is 0.10 to 100 mass ppt based on the total mass of the chemical.
  • the chemical solution according to (1) or (2), wherein the content of the titanium oxide particles is 5% by mass or more and less than 99% by mass with respect to the content of the titanium component in the metal component.
  • the metal component contains iron ions, The chemical solution according to any one of (1) to (4), wherein the content of iron ions is 0.10 to 100 mass ppt with respect to the total mass of the chemical solution.
  • the metal component contains iron oxide particles, The chemical solution according to any one of (1) to (5), wherein the content of the iron oxide particles is 5% by mass or more and less than 99% by mass based on the content of the iron component in the metal component.
  • the metal component contains iron oxide particles, The chemical solution according to any one of (1) to (6), wherein the proportion of the iron oxide particles having a particle size of 0.5 to 17 nm is 60% by mass or more and less than 98% by mass.
  • the metal component contains iron oxide particles and iron ions, To the content of iron ions, the mass ratio of the content of the iron oxide particles is 10 0 to 10 12, the drug solution according to any one of (1) to (7).
  • the metal component contains aluminum ions, The chemical solution according to any one of (1) to (8), wherein the content of aluminum ions is 0.10 to 100 mass ppt with respect to the total mass of the chemical solution.
  • the metal component contains aluminum oxide particles, The chemical solution according to any one of (1) to (9), wherein the content of the aluminum oxide particles is 5% by mass or more and less than 99% by mass based on the content of the aluminum component in the metal component.
  • the metal component contains aluminum oxide particles, The chemical solution according to any one of (1) to (10), wherein a proportion of the aluminum oxide particles having a particle size of 0.5 to 17 nm is 60% by mass or more and less than 98% by mass. (12)
  • the metal component contains aluminum oxide particles and aluminum ions, To the content of aluminum ions, the mass ratio of the content of aluminum oxide particles is 10 0 to 10 12, the drug solution according to any one of (1) to (11).
  • the metal component contains copper oxide particles, The chemical solution according to any one of (1) to (12), wherein the content of the copper oxide particles is 5% by mass or more and less than 99% by mass with respect to the content of the copper component in the metal component.
  • the metal component contains copper oxide particles, The chemical solution according to any one of (1) to (13), wherein the proportion of the copper oxide particles having a particle size of 0.5 to 17 nm is 60% by mass or more and less than 98% by mass.
  • the metal component contains copper oxide particles and copper ions, To the content of copper ions, the mass ratio of the content of copper oxide particles is 10 0 to 10 12, the drug solution according to any one of (1) to (14).
  • It It further contains organic impurities, The chemical solution according to any one of (1) to (15), wherein the content of the organic impurities is 1,000 to 100,000 mass ppt based on the total mass of the chemical solution.
  • the organic solvent is propylene glycol monomethyl ether acetate, propylene glycol monomethyl ether, cyclohexanone, ethyl lactate, propylene carbonate, isopropanol, 4-methyl-2-pentanol, butyl acetate, propylene glycol monoethyl ether, propylene glycol monopropyl Ether, methyl methoxypropionate, cyclopentanone, ⁇ -butyrolactone, diisoamyl ether, isoamyl acetate, dimethyl sulfoxide, N-methylpyrrolidone, diethylene glycol, ethylene glycol, dipropylene glycol, propylene glycol, ethylene carbonate, sulfolane, cycloheptanone , 2-heptanone, butyl butyrate
  • a numerical range represented by using “to” means a range including numerical values described before and after “to” as a lower limit and an upper limit.
  • ppm means “parts-per-million (10 ⁇ 6 )”
  • ppb means “parts-per-billion (10 ⁇ 9 )”
  • ppt means “Parts-per-trillion (10 ⁇ 12 )” means “parts-per-quadrillion (10 ⁇ 15 )”.
  • the notation that does not indicate substitution or unsubstitution means a group containing a substituent together with a group having no substituent within a range not impairing the effect of the present invention.
  • the “hydrocarbon group” includes not only a hydrocarbon group having no substituent (unsubstituted hydrocarbon group) but also a hydrocarbon group having a substituent (substituted hydrocarbon group). This is the same for each compound.
  • “radiation” in the present invention means, for example, far ultraviolet rays, extreme ultraviolet (EUV), X-rays, or electron beams. In the present invention, light means actinic rays or radiation.
  • the term “exposure” in the present invention includes not only exposure with far ultraviolet rays, X-rays or EUV, but also drawing with particle beams such as electron beams or ion beams.
  • the present inventors presume the mechanism as follows. In addition, the following mechanism is speculation, and even when the effect of the present invention is obtained by a different mechanism, it is included in the scope of the present invention.
  • the present inventors when the chemical solution contains titanium oxide particles and titanium ions, the silicon substrate or silicon substrate with a silicon oxide film (hereinafter referred to as these) by the mass ratio (mass of titanium oxide particles / mass of oxide ions). It has been found that the likelihood of occurrence of metal residue defects (residues derived from metal components) on the “specific substrate” is different.
  • the mass ratio when the mass ratio is too large, in other words, when the ratio of the titanium oxide particles is too large, it is considered that metal residue defects derived from the titanium oxide particles tend to increase on a specific substrate.
  • the mass ratio when the mass ratio is too small, in other words, when the ratio of titanium ions is too large, the oxidation-reduction reaction easily proceeds with other metal ions which are more noble than titanium ions, and particles of other metals. It is considered that (for example, oxide particles of another metal) increase and metal residue defects easily increase on a specific substrate.
  • the chemical solution of the present invention is a chemical solution containing an organic solvent and a metal component, wherein the metal component contains titanium oxide particles, and titanium ions, with respect to the content of titanium ions, the content of titanium oxide particles.
  • mass ratio is 10 0 to 10 12.
  • the chemical solution of the present invention contains an organic solvent.
  • an organic solvent is intended to mean a liquid organic compound contained at a content exceeding 10,000 mass ppm per component with respect to the total mass of the chemical solution. That is, in this specification, a liquid organic compound contained in an amount exceeding 10,000 ppm by mass with respect to the total mass of the chemical solution corresponds to an organic solvent.
  • the term “liquid” means a liquid at 25 ° C. and atmospheric pressure.
  • the content of the organic solvent in the chemical solution is not particularly limited, but is preferably 98.0% by mass or more, more preferably more than 99.0% by mass, and more preferably 99.90% by mass or more based on the total mass of the chemical solution. Preferably, it is more than 99.95% by mass. The upper limit is less than 100% by mass.
  • One type of organic solvent may be used alone, or two or more types may be used. When two or more organic solvents are used, the total content is preferably within the above range.
  • the type of the organic solvent is not particularly limited, and a known organic solvent can be used.
  • the organic solvent include alkylene glycol monoalkyl ether carboxylate, alkylene glycol monoalkyl ether, alkyl lactate, alkyl alkoxypropionate, cyclic lactone (preferably having 4 to 10 carbon atoms), and monoketone compound optionally having a ring. (Preferably having 4 to 10 carbon atoms), alkylene carbonate, alkyl alkoxyacetate, alkyl pyruvate, dialkyl sulfoxide, cyclic sulfone, dialkyl ether, monohydric alcohol, glycol, alkyl acetate, and N-alkylpyrrolidone. .
  • organic solvent examples include propylene glycol monomethyl ether acetate (PGMEA), propylene glycol monomethyl ether (PGME), cyclohexanone (CHN), ethyl lactate (EL), propylene carbonate (PC), isopropanol (IPA), and 4-methyl-2.
  • PGMEA propylene glycol monomethyl ether acetate
  • PGME propylene glycol monomethyl ether
  • CHN propylene glycol monomethyl ether
  • EL ethyl lactate
  • PC propylene carbonate
  • IPA isopropanol
  • MIBC -Pentanol
  • nBA butyl acetate
  • propylene glycol monoethyl ether propylene glycol monopropyl ether, methyl methoxypropionate, cyclopentanone, ⁇ -butyrolactone, diisoamyl ether, isoamyl acetate, dimethyl sulfoxide, N- Methylpyrrolidone, diethylene glycol, ethylene glycol, dipropylene glycol, propylene glycol, ethylene carbonate, sulfolane, cycloheptanone, Heptanone, butyl butyrate, isobutyl isobutyrate, isoamyl ether, and one or more selected from the group consisting of undecane is preferred.
  • Examples of using two or more organic solvents include a combination of PGMEA and PGME, and a combination of PGMEA and PC.
  • the kind and content of the organic solvent in the chemical solution can be measured using a gas chromatograph mass spectrometer.
  • the chemical solution contains a metal component.
  • the metal component is composed of metal-containing particles and metal ions.
  • the content of the metal component indicates the total content of the metal-containing particles and metal ions.
  • the metal-containing particles only need to include metal atoms, and examples thereof include metal oxide particles, metal nitride particles, and metal particles.
  • the metal particles mean particles made of metal.
  • the metal component contained in the chemical solution contains titanium oxide particles and titanium ions.
  • a mass ratio of 10 0 to 10 12 of the content of titanium oxide particles, on a silicon substrate or a silicon oxide film, and more hardly generates points composites residue defects residual metal defects or later in the mass ratio is preferably from 10 1 to 10 10, more preferably from 10 2 to 10 10, more preferably 10 3 to 10 8, more preferably 10 3 to 10 7.
  • the content of titanium ions is not particularly limited, and is often 0.01 to 150 mass ppt. Among them, the content of titanium ions is 0.10 to 100 mass ppt, based on the total mass of the chemical solution, in that metal residue defects or composite residue defects described later are less likely to occur on a silicon substrate or a silicon oxide film. , And more preferably 1.0 to 70 mass ppt.
  • the content of the titanium oxide particles is not particularly limited, and is often 1% by mass or more and less than 100% by mass with respect to the content of the titanium component in the metal component. Among them, on the silicon substrate or on the silicon oxide film, metal residue defects or composite residue defects described below are less likely to occur, the content of the titanium oxide particles is relative to the content of the titanium component in the metal component. It is preferably from 5% by mass to less than 99% by mass, more preferably from 30 to 90% by mass.
  • the titanium component is a component containing a titanium atom, and includes titanium-containing particles and titanium ions. For example, the content of the titanium component indicates the total content of the titanium-containing particles and titanium ions.
  • the titanium-containing particles only need to contain titanium atoms, and examples thereof include titanium oxide particles, titanium nitride particles, and titanium particles.
  • the titanium particles mean particles made of titanium metal.
  • the ratio of particles having a particle size of 0.5 to 17 nm is not particularly limited, and is often 40% by mass or more and less than 100% by mass. Above all, the ratio of particles having a particle size of 0.5 to 17 nm among titanium oxide particles is 60%, because metal residue defects or composite residue defects described later are less likely to occur on a silicon substrate or a silicon oxide film. It is preferably at least 80% by mass and less than 98% by mass, more preferably from 60 to 95% by mass.
  • the metal component contained in the chemical solution may contain iron ions.
  • the content of iron ions is not particularly limited, and is often 0.01 to 200 mass ppt based on the total mass of the chemical solution. Above all, the content of iron ions is 0.1 to 100 mass ppt with respect to the total mass of the chemical solution in that metal residue defects or composite residue defects described later are less likely to occur on a silicon substrate or a silicon oxide film. , And more preferably 1.0 to 90 mass ppt.
  • the metal component contained in the chemical solution may contain iron oxide particles.
  • the content of the iron oxide particles is not particularly limited, and is often 1% by mass or more and less than 100% by mass with respect to the content of the iron component in the metal component. Among them, on the silicon substrate or on the silicon oxide film, metal residue defects or composite residue defects described below are less likely to occur, the content of the iron oxide particles is relative to the content of the iron component in the metal component. It is preferably from 5% by mass to less than 99% by mass, more preferably from 10 to 95% by mass.
  • the iron component is a component containing an iron atom, and includes iron-containing particles and iron ions. For example, when referring to the iron component content, it indicates the total content of the iron-containing particles and iron ions.
  • the iron-containing particles only need to contain iron atoms, and examples thereof include iron oxide particles, iron nitride particles, and iron particles.
  • the iron particles mean particles made of metallic iron.
  • the ratio of particles having a particle size of 0.5 to 17 nm is not particularly limited, and is often 40% by mass or more and less than 100% by mass. Among them, the ratio of particles having a particle diameter of 0.5 to 17 nm among iron oxide particles is 60, because metal residue defects or composite residue defects described later are less likely to be formed on a silicon substrate or a silicon oxide film. It is preferably at least 80% by mass and less than 98% by mass, more preferably from 60 to 95% by mass.
  • the mass ratio of the content of iron oxide particles to the content of iron ions in the chemical solution is not particularly limited, and is often 10 ⁇ 2 to 10 14 .
  • the mass ratio is preferably from 10 0 to 10 12 , more preferably from 10 2 to 10 10 , in that metal residue defects or composite residue defects described later are less likely to be formed on the silicon substrate or the silicon oxide film.
  • 10 3 to 10 8 are more preferable, and 10 3 to 10 7 is particularly preferable.
  • the metal component contained in the chemical solution may contain aluminum ions.
  • the content of the aluminum ion is not particularly limited, and is often 0.01 to 200 mass ppt with respect to the total mass of the chemical solution. Above all, the content of aluminum ions is 0.1 to 100 mass ppt with respect to the total mass of the chemical solution in that metal residue defects or composite residue defects described later are less likely to occur on a silicon substrate or a silicon oxide film. , And more preferably 1.0 to 90 mass ppt.
  • the metal component contained in the chemical solution may contain aluminum oxide particles.
  • the content of the aluminum oxide particles is not particularly limited, and is often 1% by mass or more and less than 100% by mass with respect to the content of the aluminum component in the metal component. Among them, on the silicon substrate or on the silicon oxide film, metal residue defects or composite residue defects described below are less likely to occur, the content of the aluminum oxide particles is relative to the content of the aluminum component in the metal component. It is preferably from 5% by mass to less than 99% by mass, more preferably from 10 to 95% by mass.
  • the aluminum component is a component containing an aluminum atom, and includes aluminum-containing particles and aluminum ions. For example, when referring to the content of the aluminum component, it indicates the total content of the aluminum-containing particles and aluminum ions.
  • the aluminum-containing particles only need to contain aluminum atoms, and examples thereof include aluminum oxide particles, aluminum nitride particles, and aluminum particles.
  • the aluminum particles mean particles made of metallic aluminum.
  • the ratio of particles having a particle size of 0.5 to 17 nm is not particularly limited, and is often 40% by mass or more and less than 100% by mass. Above all, the ratio of particles having a particle size of 0.5 to 17 nm among aluminum oxide particles is 60%, because metal residue defects or composite residue defects described later are less likely to be formed on a silicon substrate or a silicon oxide film. It is preferably at least 80% by mass and less than 98% by mass, more preferably from 60 to 95% by mass.
  • the mass ratio of the content of aluminum oxide particles to the content of aluminum ions in the chemical solution is not particularly limited, and is often 10 ⁇ 2 to 10 14 .
  • the mass ratio is preferably from 10 0 to 10 12 , more preferably from 10 2 to 10 10 , in that metal residue defects or composite residue defects described later are less likely to be formed on the silicon substrate or the silicon oxide film.
  • 10 3 to 10 8 are more preferable, and 10 3 to 10 7 is particularly preferable.
  • the metal component contained in the chemical solution may contain components of other metal atoms than those described above.
  • Other metal atoms include, for example, Na (sodium), K (potassium), Ca (calcium), Cu (copper), Mg (magnesium), Mn (manganese), Li (lithium), Cr (chromium), Ni (Nickel) and Zr (zirconium).
  • the metal component contained in the chemical solution may contain copper oxide particles.
  • the content of the copper oxide particles is not particularly limited, and is often 1% by mass or more and less than 100% by mass with respect to the content of the copper component in the metal component. Among them, on the silicon substrate or on the silicon oxide film, metal residue defects or composite residue defects described below are less likely to occur, the content of the copper oxide particles is relative to the content of the copper component in the metal component. It is preferably from 5% by mass to less than 99% by mass, more preferably from 10 to 95% by mass.
  • the copper component is a component containing a copper atom, and includes copper-containing particles and copper ions. For example, when referring to the content of the copper component, it indicates the total content of the copper-containing particles and copper ions.
  • the copper-containing particles only need to contain copper atoms, and examples thereof include copper oxide particles, copper nitride particles, and copper particles.
  • the copper particles mean particles made of metallic copper.
  • the ratio of the particles having a particle size of 0.5 to 17 nm is not particularly limited, and is often 40% by mass or more and less than 100% by mass.
  • the proportion of particles having a particle diameter of 0.5 to 17 nm among copper oxide particles is 60%, because metal residue defects or composite residue defects described later are less likely to be formed on a silicon substrate or a silicon oxide film. It is preferably at least 80% by mass and less than 98% by mass, more preferably from 60 to 95% by mass.
  • the mass ratio of the content of copper oxide particles to the content of copper ions in the chemical solution is not particularly limited, and is often 10 ⁇ 2 to 10 14 .
  • the mass ratio is preferably from 10 0 to 10 12 , more preferably from 10 2 to 10 10 , in that metal residue defects or composite residue defects described later are less likely to be formed on the silicon substrate or the silicon oxide film.
  • 10 3 to 10 8 are more preferable, and 10 3 to 10 7 is particularly preferable.
  • the metal component may be a metal component inevitably included in each component (raw material) included in the chemical solution, or may be a metal component inevitably included in the production, storage, and / or transfer of the treatment liquid. May be intentionally added.
  • the content of the metal component is not particularly limited, the metal residue defect or the composite residue defect described below is less likely to be formed on the silicon substrate or the silicon oxide film, and thus the content is 10 to 500,000 mass% based on the total mass of the chemical solution. ppt is preferred.
  • the types and contents of metal ions and metal-containing particles in a chemical solution can be measured by an SP-ICP-MS method (Single Nano Particle Inductively Coupled Plasma Mass Spectrometry).
  • the SP-ICP-MS method uses an apparatus similar to a normal ICP-MS method (inductively coupled plasma mass spectrometry), and differs only in data analysis. Data analysis of the SP-ICP-MS method can be performed by commercially available software.
  • the content of a metal component to be measured is measured regardless of its existing form. Therefore, the total mass of the metal-containing particles to be measured and the metal ions is determined as the content of the metal component.
  • the content of metal-containing particles can be measured. Therefore, by subtracting the content of the metal-containing particles from the content of the metal component in the sample, the content of the metal ion in the sample can be calculated.
  • Agilent 8800 triple quadrupole ICP-MS inductively coupled plasma mass spectrometry, option # 200 for semiconductor analysis, option # 200
  • Agilent Technologies, Inc. is described in Examples. Can be measured by the following method.
  • Agilent 8900 manufactured by Agilent Technologies can be used as an apparatus other than the above.
  • the method described in paragraphs 0015 to 0067 of JP-A-2009-188333 (hereinafter, also referred to as “specific method”) is used.
  • the number of particles of 0.5 to 10 nm remaining on the substrate is counted by a specific method, and the converted value of the 20 nm particles from SNP-ICP-MS is used for the count.
  • the conversion value differs for each metal, this conversion is performed for each metal.
  • the specific method of conversion is as follows.
  • the converted value Becomes 10. That is, when the number of 1 nm titanium oxide particles confirmed by the specific method is 100, the number is calculated as 1000 (100 ⁇ 10) in the chemical based on 10 times the converted value.
  • the number of particles having a size of 10 nm or less in the present invention is estimated by this conversion method regardless of the type of metal.
  • the chemical may contain organic impurities.
  • the content of the organic impurities in the chemical solution is not particularly limited, but is preferably from 1,000 to 100,000 mass ppt based on the total mass of the chemical solution from the viewpoint that stain-like residue defects described later are less likely to be formed on the silicon substrate.
  • the organic impurity is an organic compound different from the organic solvent, and means an organic compound contained at a content of 10000 ppm by mass or less based on the total mass of the organic solvent. That is, in the present specification, an organic compound contained at a content of 10,000 mass ppm or less based on the total mass of the organic solvent corresponds to an organic impurity and does not correspond to an organic solvent.
  • Organic impurities are often mixed with or added to a chemical solution during the process of refining a substance to be purified to obtain a chemical solution.
  • organic impurities include a plasticizer, an antioxidant, and a compound derived from these (typically, a decomposition product).
  • the drug solution may contain water.
  • Water is not included in the organic impurities.
  • the water is not particularly limited, and for example, distilled water, ion-exchanged water, pure water, and the like can be used.
  • Water may be added to the chemical solution, or may be unintentionally mixed into the chemical solution in the process of manufacturing the chemical solution. Examples of the case of being unintentionally mixed in the manufacturing process of the chemical solution include, for example, the case where water is contained in a raw material (for example, an organic solvent) used for manufacturing the chemical solution, and the mixing in the manufacturing process of the chemical solution ( For example, contamination) is not limited to the above.
  • the content of water in the chemical is not particularly limited, but is preferably 2.0% by mass or less, more preferably 500% by mass or less, based on the total mass of the chemical.
  • the lower limit is not particularly limited, but may be 0% by mass.
  • the water content in the chemical solution means the water content measured using an apparatus based on the Karl Fischer moisture measurement method.
  • the chemical solution of the present invention is preferably used for manufacturing a semiconductor device. Especially, it is preferable to manufacture a semiconductor chip using the chemical solution of the present invention. Specifically, in a semiconductor device manufacturing process including a lithography process, an etching process, an ion implantation process, and a peeling process, an organic material is processed after each process or before moving to the next process. Specifically, it is suitably used as a pre-wet liquid, a developing liquid, a rinsing liquid, a polishing liquid or the like. In addition, the chemical solution may be used as a diluting solution of the resin contained in the resist film forming composition (in other words, a solvent).
  • the above-mentioned chemical solution can be used for other uses other than the production of semiconductor devices, and can also be used as a developer and a rinse for polyimide, a resist for sensors, a resist for lenses, and the like.
  • the above chemical solution can be used as a solvent for medical use or cleaning use.
  • it can be suitably used for cleaning pipes, containers, and substrates (for example, wafers and glass).
  • a cleaning liquid a pipe cleaning liquid and a container cleaning liquid, etc.
  • a liquid such as the above-mentioned pre-wet liquid.
  • the chemical solution is suitably used for a pre-wet solution, a developing solution, a rinsing solution, a polishing solution, and a composition for forming a resist film.
  • a pre-wet liquid when applied to a pre-wet liquid, a developing liquid and a rinsing liquid, more excellent effects are exhibited.
  • a developing liquid and a rinsing liquid when the exposure light source is EUV, a more excellent effect is exhibited.
  • a pipe cleaning liquid used for pipes used for transferring these liquids more excellent effects are exhibited.
  • the method for producing the chemical solution is not particularly limited, and a known production method can be used. Above all, in that a chemical solution exhibiting a better effect of the present invention can be obtained, the method for producing a chemical solution has a filtration step of filtering a substance to be purified containing an organic solvent using a filter to obtain a chemical solution. preferable.
  • the material to be purified used in the filtration step may be procured by purchasing or the like, or may be obtained by reacting the raw materials. It is preferable that the material to be purified has a low impurity content. Examples of such a commercially available product to be purified include a commercially available product called “high-purity grade product”.
  • the method of obtaining the object to be purified typically, the object to be purified containing an organic solvent
  • a known method can be used.
  • a method of reacting acetic acid and n-butanol in the presence of sulfuric acid to obtain butyl acetate reacting ethylene, oxygen, and water in the presence of Al (C 2 H 5 ) 3 Reacting cis-4-methyl-2-pentene in the presence of Ipc2BH (Diisopinocampheylborane) to obtain 4-methyl-2-pentanol; propylene oxide, methanol and acetic acid Is reacted in the presence of sulfuric acid to obtain PGMEA (propylene glycol 1-monomethyl ether 2-acetate); acetone and hydrogen are reacted in the presence of copper oxide-zinc oxide-aluminum oxide to give IPA (isopropyl). alcohol) by reacting lactic acid and ethanol to obtain lactic acid. And the like; a method of obtaining a chill.
  • the method for producing a drug solution of the present invention preferably includes a filtration step of filtering the above-mentioned substance to be purified using a filter to obtain a drug solution.
  • the method of filtering the object to be purified using a filter is not particularly limited, and the object to be purified is passed through a filter unit having a housing and a filter cartridge housed in the housing with or without pressurization ( Is preferable.
  • the pore size of the filter is not particularly limited, and a filter having a pore size usually used for filtering a substance to be purified can be used.
  • the pore diameter of the filter is preferably 200 nm or less, more preferably 20 nm or less, still more preferably 10 nm or less, and more preferably 5 nm or less, in that the number of particles (metal particles and the like) contained in the drug solution can be easily controlled in a desired range. Is particularly preferred.
  • the lower limit is not particularly limited, but is generally preferably 1 nm or more from the viewpoint of productivity.
  • the pore diameter of a filter means the pore diameter determined by the bubble point of isopropanol (IPA).
  • the pore diameter of the filter be 5.0 nm or less, since the number of particles contained in the drug solution can be more easily controlled.
  • a filter having a pore size of 5.0 nm or less is also referred to as a “micropore size filter”.
  • the micropore size filter may be used alone, or may be used with a filter having another pore size. Among them, it is preferable to use a filter having a larger pore diameter from the viewpoint of better productivity. That is, when two or more filters are used, it is preferable that at least one filter has a pore diameter of 5.0 nm or less.
  • the object to be purified which has been filtered through a filter having a larger pore diameter in advance, is passed through a micropore size filter, clogging of the micropore size filter can be prevented. That is, when one filter is used, the pore diameter of the filter is preferably 5.0 nm or less, and when two or more filters are used, the pore diameter of the filter having the smallest pore diameter is 5.0 nm. The following is preferred.
  • the form in which two or more types of filters having different pore diameters are sequentially used is not particularly limited, and examples thereof include a method of sequentially arranging the above-described filter units along a pipe through which a substance to be purified is transferred.
  • a larger pressure may be applied to a filter having a smaller pore size as compared with a filter having a larger pore size.
  • a pressure regulating valve, a damper, etc. are arranged between the filters to make the pressure applied to the filter having a small pore diameter constant, or a filter unit containing the same filter is placed along the pipeline. It is preferable to increase the filtration area by arranging them in parallel. This makes it possible to more stably control the number of particles in the chemical solution.
  • the material of the filter is not particularly limited, and known materials for the filter can be used. Specifically, when it is a resin, polyamide such as nylon (for example, 6-nylon and 6,6-nylon); polyolefin such as polyethylene and polypropylene; polystyrene; polyimide; polyamideimide; Polytetrafluoroethylene, perfluoroalkoxyalkane, perfluoroethylene propene copolymer, ethylene / tetrafluoroethylene copolymer, ethylene-chlorotrifluoroethylene copolymer, polychlorotrifluoroethylene, polyvinylidene fluoride, and polyvinyl fluoride Fluorocarbon; polyvinyl alcohol; polyester; cellulose; cellulose acetate and the like.
  • polyamide such as nylon (for example, 6-nylon and 6,6-nylon)
  • polyolefin such as polyethylene and polypropylene
  • polystyrene polyimide
  • polyamideimide poly
  • nylon especially, 6,6-nylon is preferred
  • polyolefin especially, polyethylene is preferred
  • polyolefin are preferred in that they have better solvent resistance and the resulting chemical has more excellent defect suppression performance.
  • At least one selected from the group consisting of (meth) acrylate and polyfluorocarbon (among others, polytetrafluoroethylene (PTFE) and perfluoroalkoxyalkane (PFA) is preferable) is preferable.
  • PTFE polytetrafluoroethylene
  • PFA perfluoroalkoxyalkane
  • a polymer eg, nylon grafted UPE obtained by graft copolymerizing a polyamide (eg, nylon-6 or nylon-6,6, etc.) with a polyolefin (eg, UPE (ultra high molecular weight polyethylene) described below) is used as a filter.
  • a polyamide eg, nylon-6 or nylon-6,6, etc.
  • a polyolefin eg, UPE (ultra high molecular weight polyethylene) described below
  • the filter may be a surface-treated filter.
  • the method for surface treatment is not particularly limited, and a known method can be used. Examples of the surface treatment method include chemical modification treatment, plasma treatment, hydrophobic treatment, coating, gas treatment, and sintering.
  • Plasma treatment is preferable because the surface of the filter becomes hydrophilic.
  • the water contact angle on the surface of the filter that has been hydrophilized by plasma treatment is not particularly limited, but the static contact angle at 25 ° C. measured by a contact angle meter is preferably 60 ° or less, more preferably 50 ° or less, 30 ° or less is more preferable.
  • a method of introducing an ion exchange group into a filter is preferable. That is, a filter having an ion exchange group is preferable as the filter.
  • the ion exchange group include a cation exchange group and an anion exchange group.
  • the cation exchange group include a sulfonic acid group, a carboxy group, and a phosphate group, and examples of the anion exchange group include a quaternary ammonium group.
  • the method for introducing the ion-exchange group into the filter is not particularly limited, and examples thereof include a method in which a compound containing an ion-exchange group and a polymerizable group is allowed to react with the filter and typically grafted.
  • the method of introducing the ion exchange group is not particularly limited, but the filter is irradiated with ionizing radiation ( ⁇ -ray, ⁇ -ray, ⁇ -ray, X-ray, electron beam, etc.) to generate an active portion (radical).
  • ionizing radiation ⁇ -ray, ⁇ -ray, ⁇ -ray, X-ray, electron beam, etc.
  • the filter after the irradiation is immersed in the monomer-containing solution, and the monomer is graft-polymerized on the filter.
  • a polymer obtained by polymerizing this monomer is grafted on the filter.
  • the produced polymer can be brought into contact with a compound containing an anion exchange group or a cation exchange group to introduce an ion exchange group into the polymer.
  • the filter may have a structure in which a woven or nonwoven fabric having an ion exchange group formed by a radiation graft polymerization method is combined with a conventional glass wool, woven or nonwoven fabric filter material.
  • the material constituting the filter having an ion exchange group is not particularly limited, and examples thereof include a polyfluorocarbon and a material in which an ion exchange group is introduced into polyolefin, and a material in which an ion exchange group is introduced into polyfluorocarbon is more preferable.
  • the pore diameter of the filter having an ion exchange group is not particularly limited, it is preferably 1 to 30 nm, more preferably 5 to 20 nm.
  • the filter having an ion-exchange group may also serve as the filter having the smallest pore diameter described above, or may be used separately from the filter having the smallest pore diameter.
  • the filtration step uses a filter having an ion exchange group and a filter having no ion exchange group and having a minimum pore diameter. Is preferred.
  • the material of the filter having the smallest pore diameter already described is not particularly limited, but from the viewpoint of solvent resistance and the like, generally, polyfluorocarbon, and at least one selected from the group consisting of polyolefins are preferable. More preferred.
  • the filter used in the filtration step two or more types of filters having different materials may be used.
  • polyolefins, polyfluorocarbons, polyamides, and filters made of materials having ion exchange groups introduced therein may be used. Two or more kinds selected from the group may be used.
  • the pore structure of the filter is not particularly limited, and may be appropriately selected according to the components in the object to be purified.
  • the pore structure of a filter means a pore size distribution, a positional distribution of pores in a filter, and a shape of pores, and is typically controlled by a filter manufacturing method. It is possible.
  • a porous film can be obtained by sintering a powder of a resin or the like, and a fiber film can be obtained by forming by a method such as electrospinning, electroblowing, and meltblowing. These have different pore structures.
  • a “porous membrane” refers to a membrane that retains components in an object to be purified, such as gels, particles, colloids, cells, and poly-oligomers, but a component that is substantially smaller than the pores passes through the pores.
  • the retention of components in the object to be purified by the porous membrane may depend on operating conditions, such as surface velocity, use of surfactant, pH, and combinations thereof, and the pore size of the porous membrane, It may depend on the structure and the size of the particles to be removed, and the structure (hard particles or gels, etc.).
  • non-sieving membranes include, but are not limited to, nylon-6 membranes and nylon membranes such as nylon-6,6 membranes.
  • non-sieving retention mechanism refers to retention caused by mechanisms such as filter pressure drop or interference, diffusion, and adsorption that are not related to pore size.
  • Non-sieve retention includes retention mechanisms, such as obstruction, diffusion, and adsorption, that remove particles to be removed from the object to be purified, regardless of the filter pressure drop or filter pore size.
  • the adsorption of particles to the filter surface can be mediated, for example, by intermolecular van der Waals forces and electrostatic forces.
  • An interfering effect occurs when particles traveling in a non-sieving membrane layer having a tortuous path are not turned fast enough to avoid contact with the non-sieving membrane.
  • Particle transport by diffusion results primarily from random or Brownian motion of small particles, which creates a certain probability that the particles will collide with the filter media. If there is no repulsion between the particles and the filter, the non-sieve retention mechanism can be active.
  • UPE (ultra high molecular weight polyethylene) filters are typically sieved membranes.
  • a sieve membrane means a membrane that mainly captures particles via a sieve holding mechanism, or a membrane that is optimized for capturing particles via a sieve holding mechanism.
  • Typical examples of sieving membranes include, but are not limited to, polytetrafluoroethylene (PTFE) membranes and UPE membranes.
  • PTFE polytetrafluoroethylene
  • the “sieve holding mechanism” refers to holding the result due to the removal target particles being larger than the pore diameter of the porous membrane.
  • the sieve retention is improved by forming a filter cake (agglomeration of the particles to be removed on the surface of the membrane). The filter cake effectively performs the function of a secondary filter.
  • the material of the fiber membrane is not particularly limited as long as it is a polymer capable of forming the fiber membrane.
  • the polymer include polyamide and the like.
  • the polyamide include nylon 6, nylon 6,6, and the like.
  • the polymer forming the fiber membrane may be poly (ether sulfone).
  • the surface energy of the fibrous membrane is preferably higher than the polymer which is the material of the porous membrane on the secondary side.
  • An example of such a combination is a case where the material of the fiber membrane is nylon and the porous membrane is polyethylene (UPE).
  • the method for producing the fiber membrane is not particularly limited, and a known method can be used.
  • Examples of the method for producing a fiber membrane include electrospinning, electroblowing, and meltblowing.
  • the pore structure of the porous membrane is not particularly limited, and examples of the pore shape include a lace shape, a string shape, and a node shape.
  • Can be The distribution of pore sizes in the porous membrane and the distribution of positions in the membrane are not particularly limited.
  • the size distribution may be smaller and the distribution position in the film may be symmetric. Further, the size distribution may be larger and the distribution position in the film may be asymmetric (the above film is also referred to as “asymmetric porous film”).
  • asymmetric porous membrane the size of the pores varies in the membrane, and typically the pore size increases from one surface of the membrane to the other surface of the membrane.
  • the surface on the side with many pores having a large pore diameter is called “open side”, and the surface on the side with many pores with small pore diameter is also called “tight side”.
  • the asymmetric porous membrane include a membrane in which the size of pores is minimized at a certain position within the thickness of the membrane (this is also referred to as an “hourglass shape”).
  • the primary side is made to have a larger-sized pore using the asymmetric porous membrane, in other words, if the primary side is made to be the open side, a pre-filtration effect can be produced.
  • the porous membrane may include thermoplastic polymers such as PESU (polyethersulfone), PFA (perfluoroalkoxyalkane, copolymer of ethylene tetrafluoride and perfluoroalkoxyalkane), polyamide, and polyolefin. , Polytetrafluoroethylene and the like. Among them, ultrahigh molecular weight polyethylene is preferable as the material of the porous membrane. Ultra-high molecular weight polyethylene means a thermoplastic polyethylene having an extremely long chain, and preferably has a molecular weight of 1,000,000 or more, typically 2,000,000 to 6,000,000.
  • a filter used in the filtration step two or more types of filters having different pore structures may be used, or a filter of a porous membrane and a filter of a fiber membrane may be used in combination. Specific examples include a method using a nylon fiber membrane filter and a UPE porous membrane filter.
  • the filter is sufficiently washed before use.
  • impurities contained in the filter are likely to be brought into the chemical solution.
  • At least one selected from the group consisting of a filter material, a pore diameter, and a pore structure passes the material to be purified through two or more types of different filters.
  • a multi-stage filtration step The object to be purified may be passed through the same filter a plurality of times, or the object to be purified may be passed through a plurality of filters of the same type.
  • a filter capable of selectively removing metal components such as “Purasol SN 200 nm” (metal component removal filter).
  • the material of the liquid contacting portion of the purification device used in the filtration step is not particularly limited, but non-metallic materials (fluorinated resin And the like, and at least one selected from the group consisting of electrolytically polished metal materials (such as stainless steel) (hereinafter, these are collectively referred to as “corrosion-resistant materials”).
  • non-metallic materials fluorinated resin And the like, and at least one selected from the group consisting of electrolytically polished metal materials (such as stainless steel) (hereinafter, these are collectively referred to as “corrosion-resistant materials”).
  • the wetted part of a production tank is formed of a corrosion-resistant material, which means that the production tank itself is made of a corrosion-resistant material, or the inner wall of the production tank is coated with a corrosion-resistant material.
  • Non-metallic materials include, for example, polyethylene resin, polypropylene resin, polyethylene-polypropylene resin, and fluorine-based resin (for example, ethylene tetrafluoride resin, ethylene tetrafluoride-perfluoroalkyl vinyl ether copolymer resin, ethylene tetrafluoride -Propylene hexafluoride copolymer resin, ethylene tetrafluoride-ethylene copolymer resin, ethylene trifluoride-ethylene copolymer resin, vinylidene fluoride resin, ethylene trifluoride ethylene copolymer resin, and vinyl fluoride resin And the like, but not limited thereto.
  • fluorine-based resin for example, ethylene tetrafluoride resin, ethylene tetrafluoride-perfluoroalkyl vinyl ether copolymer resin, ethylene tetrafluoride -Propylene hexafluoride copolymer resin, ethylene
  • the metal material is not particularly limited, and a known material can be used.
  • the metal material include a metal material in which the total content of chromium and nickel is more than 25% by mass based on the total mass of the metal material, and among them, 30% by mass or more is more preferable.
  • the upper limit of the total content of chromium and nickel in the metal material is not particularly limited, but is generally preferably 90% by mass or less.
  • the metal material include stainless steel and a nickel-chromium alloy.
  • the stainless steel is not particularly limited, and a known stainless steel can be used. Among them, alloys containing nickel at 8% by mass or more are preferable, and austenitic stainless steels containing nickel at 8% by mass or more are more preferable.
  • austenitic stainless steel include SUS (Steel Use Stainless) 304 (Ni content 8% by mass, Cr content 18% by mass), SUS304L (Ni content 9% by mass, Cr content 18% by mass), SUS316 ( Ni content 10% by mass, Cr content 16% by mass) and SUS316L (Ni content 12% by mass, Cr content 16% by mass) and the like.
  • the nickel-chromium alloy is not particularly limited, and a known nickel-chromium alloy can be used. Among them, a nickel-chromium alloy having a nickel content of 40 to 75% by mass and a chromium content of 1 to 30% by mass is preferable. Examples of the nickel-chromium alloy include Hastelloy (trade name, the same applies hereinafter), Monel (trade name, the same applies hereinafter), and Inconel (trade name, the same applies 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), and Hastelloy C-276 22 (Ni content 61% by mass, Cr content 22% by mass).
  • the nickel-chromium alloy may further contain boron, silicon, tungsten, molybdenum, copper, cobalt, and the like, if necessary, in addition to the above alloy.
  • the method of electropolishing the metal material is not particularly limited, and a known method can be used.
  • a known method can be used.
  • the methods described in paragraphs [0011] to [0014] of JP-A-2015-227501 and paragraphs [0036] to [0042] of JP-A-2008-264929 can be used.
  • the metal material has a higher chromium content in the passivation layer on the surface than a chromium content in the matrix due to electrolytic polishing. Therefore, it is presumed that the use of a refining device in which the liquid contact portion is formed from a metal material which has been electropolished, makes it difficult for metal-containing particles to flow out into the object to be purified.
  • the metal material may be buffed.
  • the buffing method is not particularly limited, and a known method can be used.
  • the size of the abrasive grains used for the buffing finish is not particularly limited, but is preferably # 400 or less from the viewpoint that irregularities on the surface of the metal material tend to be smaller.
  • the buff polishing is preferably performed before the electrolytic polishing.
  • the method for producing a chemical solution may further include a step other than the filtration step.
  • the steps other than the filtration step include, for example, a distillation step, a reaction step, and a charge removal step.
  • the distillation step is a step of distilling an object to be purified containing an organic solvent to obtain a distilled object to be purified.
  • the method for distilling the object to be purified is not particularly limited, and a known method can be used.
  • a distillation column is arranged on the primary side of a purification device provided for a filtration step, and a distilled product to be purified is introduced into a production tank.
  • the liquid contact portion of the distillation column is not particularly limited, but is preferably formed of the corrosion-resistant material described above.
  • the reaction step is a step of reacting the raw materials to produce a purified product containing an organic solvent as a reactant.
  • the method for producing the object to be purified is not particularly limited, and a known method can be used. Typically, there is a method in which a reaction tank is arranged on the primary side of a production tank (or a distillation column) of a purification device provided for a filtration step, and a reactant is introduced into the production tank (or a distillation column). At this time, the liquid contact portion of the production tank is not particularly limited, but is preferably formed of the corrosion-resistant material described above.
  • the charge elimination step is a step of removing charges from the object to be purified to reduce the charged potential of the object to be purified.
  • the static elimination method is not particularly limited, and a known static elimination method can be used.
  • Examples of the charge removal method include a method of contacting the object to be purified with a conductive material.
  • the contact time for contacting the object to be purified with the conductive material is preferably from 0.001 to 60 seconds, more preferably from 0.001 to 1 second, even more preferably from 0.01 to 0.1 second.
  • the conductive material include stainless steel, gold, platinum, diamond, and glassy carbon.
  • ⁇ Purification of the object to be purified is preferably performed in a clean room, in which the opening of the container, the cleaning of the container and the device, the storage of the solution, and the analysis are all performed.
  • the clean room is preferably a clean room having a class 4 or higher cleanliness specified by International Standard ISO1464-1: 2015 specified by the International Organization for Standardization. Specifically, it is preferable to satisfy any one of ISO class 1, ISO class 2, ISO class 3, and ISO class 4, more preferably to satisfy ISO class 1 or ISO class 2, and to satisfy ISO class 1. Is more preferred.
  • the storage temperature of the drug solution is not particularly limited, but the storage temperature is preferably 4 ° C. or higher from the viewpoint that impurities and the like contained in a small amount in the drug solution are less likely to be eluted and, as a result, a superior effect of the present invention can be obtained.
  • the drug solution produced by the above purification method may be stored in a container and stored until use.
  • a combination of such a container and a drug solution contained in the container is referred to as a drug solution container.
  • the medicinal solution is taken out from the stored medicinal solution container and used.
  • the container As a container for storing the chemical solution, it is preferable that the container has a high degree of cleanness and a small amount of impurities eluted for use in semiconductor device manufacturing.
  • Specific examples of usable containers include, but are not limited to, “Clean Bottle” series manufactured by Aicello Chemical Co., Ltd. and “Pure Bottle” manufactured by Kodama Resin Kogyo.
  • a multi-layer bottle having a six-layer structure made of six kinds of resins or a seven-layer structure made of six kinds of resins is used for the purpose of preventing impurities from being mixed into the chemical solution (contamination). Is also preferred. Examples of these containers include those described in JP-A-2015-123351.
  • the liquid-contact part of this container may be a corrosion-resistant material (preferably, electropolished stainless steel or fluorine resin) or glass described above. It is preferable that 90% or more of the area of the liquid contact part is made of the above-mentioned material, and it is more preferable that all of the liquid contact part is made of the above-mentioned material from the viewpoint that the superior effects of the present invention can be obtained.
  • the porosity of the liquid medicine container in the container is preferably 2 to 80% by volume, more preferably 2 to 50% by volume, and still more preferably 5 to 30% by volume. Note that the porosity is calculated according to equation (1).
  • Formula (1): Porosity ⁇ 1 ⁇ (volume of drug solution in container / volume of container) ⁇ ⁇ 100
  • the container volume is synonymous with the internal volume (capacity) of the container.
  • the purified product purified by distillation is stored in a storage tank, and the purified product stored in the storage tank is passed through filters 1 to 5 shown in Table 1 in this order and filtered. Stored in tank.
  • the object to be purified stored in the storage tank is filtered through the filters 6 to 7 shown in Table 1, and the object to be purified after being filtered through the filter 7 is circulated upstream of the filter 6, and then filtered again.
  • a circulating filtration process of filtering at 6 to 7 was performed. After the circulation filtration treatment, the drug solution was stored in the container.
  • water was added to the chemical so that the water content became a predetermined value.
  • liquid contact parts of various devices for example, distillation towers, pipes, storage tanks, etc.
  • various devices for example, distillation towers, pipes, storage tanks, etc.
  • ⁇ Content of metal component The content of metal components (metal ions, metal-containing particles) in the chemical solution was measured by a method using ICP-MS and SP-ICP-MS. The following equipment was used. ⁇ Manufacturer: PerkinElmer ⁇ Model: NexION350S The following analysis software was used for the analysis. ⁇ Syngisix nano application module dedicated to “SP-ICP-MS” ⁇ Syngisix for ICP-MS software However, since the metal-containing particles of 10 nm or less cannot be measured by SP-ICP-MS, the above-mentioned specific method was used.
  • GC / MS gas chromatography mass spectrometer
  • ⁇ Test> (Pre-wet liquid or rinse liquid)
  • a chemical solution is spin-discharged onto a silicon substrate having a diameter of 300 mm or a silicon substrate having a silicon oxide film having a diameter of 300 mm (a silicon substrate whose surface is covered with a silicon oxide film). Then, 0.5 cc of each chemical solution was discharged. Thereafter, the substrate was spin-dried. Next, using a wafer inspection apparatus “SP-5” manufactured by KLA-Tencor, the number of defects present on the substrate after the application of the chemical was measured (this is referred to as a measured value).
  • the metal residue defect is a residue derived from a metal component
  • the composite residue defect is a residue derived from a composite of an organic substance and a metal component
  • the stain residue defect is a residue derived from an organic substance. If both the “metal residue on Si” and the “metal residue on SiO 2 ” are “D” or more, they are suitably used as a pre-wet liquid or a rinsing liquid.
  • a resist pattern was formed by the following operation.
  • An actinic ray-sensitive or radiation-sensitive resin composition described below is applied to a silicon substrate having a diameter of 300 mm or a silicon substrate having a silicon oxide film having a diameter of 300 mm, and prebaked (PB) at 100 ° C. for 60 seconds.
  • PB prebaked
  • a resist film having a thickness of 150 nm was formed.
  • Acid-decomposable resin represented by the following formula (weight average molecular weight (Mw): 7500): the numerical value described in each repeating unit means mol%): 100 parts by mass
  • the polymer type quencher has a weight average molecular weight (Mw) of 5000.
  • Mw weight average molecular weight
  • Hydrophobic resin shown below 4 parts by mass (mass ratio was 0.5: 0.5 in order from the left)
  • the hydrophobic resin on the left side has a weight average molecular weight. (Mw) is 7000, and the weight average molecular weight (Mw) of the right hydrophobic resin is 8000.
  • the numerical value described in each repeating unit means a molar ratio.
  • the wafer on which the resist film was formed was subjected to pattern exposure at 25 mJ / cm 2 using an ArF excimer laser scanner (Numerical Aperture: 0.75). Then, it heated at 120 degreeC for 60 second. Subsequently, each developing solution (chemical solution) was developed by paddle for 30 seconds. Next, the wafer was rotated at 4000 rpm for 30 seconds to form a negative resist pattern. Then, the obtained negative resist pattern was heated at 200 ° C. for 300 seconds. Through the above steps, an L / S pattern (average pattern width: 45 nm) having a line / space ratio of 1: 1 was obtained. In the space portion of the obtained sample, the presence or absence of the above-described metal residue defect, composite residue defect, and spot-like residue defect was evaluated according to the above method.
  • the difference in pressure between the filters was 0.01 to 0.03 MPa.
  • "Usage 1" in the “Usage” column means that the above test was carried out using the chemical solutions described in each of Examples and Comparative Examples as a pre-wet liquid and a rinsing liquid.
  • “Use 2” in the “use” column means that the above test was performed using the chemicals described in each of the examples and comparative examples as a developer.
  • “metal residue on Si” indicates the evaluation result of metal residue defect on the silicon substrate, and “composite residue on Si” indicates the result of composite residue defect on the silicon substrate.
  • the column of "Ti oxide particles / Ti ion” indicates the mass ratio of the content of titanium oxide particles to the content of titanium ions.
  • the “Ti ion amount (mass ppt)” column indicates the content (mass ppt) of titanium ions with respect to the total mass of the chemical solution.
  • the column of “Fe oxide particles / Fe ions” indicates the mass ratio of the content of iron oxide particles to the content of iron ions.
  • the “Fe ion amount (mass ppt)” column indicates the iron ion content (mass ppt) based on the total mass of the chemical solution.
  • the column “Al oxide particles / Al ions” indicates the mass ratio of the content of aluminum oxide particles to the content of aluminum ions.
  • the “Al ion amount (mass ppt)” column indicates the content (mass ppt) of aluminum ions with respect to the total mass of the chemical solution.
  • the column “Ratio of Ti oxide particles (% by mass)” indicates the content (% by mass) of the titanium oxide particles with respect to the content of the titanium component in the metal component.
  • the column “Fe oxide particle ratio (% by mass)” represents the content (% by mass) of the iron oxide particles with respect to the content of the iron component in the metal component.
  • the “Al oxide particle ratio (% by mass)” column indicates the content (% by mass) of the aluminum oxide particles with respect to the content of the aluminum component in the metal component.
  • the column “Ratio of 0.5 to 17 nm Ti oxide particles (% by mass)” indicates the ratio (% by mass) of the titanium oxide particles having a particle size of 0.5 to 17 nm.
  • the column “Ratio of 0.5 to 17 nm Fe oxide particles (% by mass)” indicates the ratio (% by mass) of iron oxide particles having a particle size of 0.5 to 17 nm.
  • the column “Ratio of 0.5 to 17 nm Al oxide particles (% by mass)” indicates the ratio (% by mass) of particles having a particle size of 0.5 to 17 nm among aluminum oxide particles.
  • the column “Cu oxide particle ratio (% by mass)” indicates the content (% by mass) of the copper oxide particles with respect to the content of the copper component in the metal component.
  • the column “Ratio of 0.5 to 17 nm Cu oxide particles (% by mass)” indicates the ratio (% by mass) of particles having a particle size of 0.5 to 17 nm among the copper oxide particles.
  • the “moisture content” column indicates the water content (mass ppb) in the drug solution with respect to the total weight of the drug solution.
  • E + number represents “10 numbers ”, for example, “3.5E + 04” represents “3.5 ⁇ 10 4 ”.
  • “> 99” indicates more than 99.
  • “ ⁇ 1” represents less than 1.
  • “ ⁇ 500 ppb” represents less than 500 mass ppb.
  • Table 1 the data relating to each of the examples and the comparative examples are shown in Table 1 [Part 1] ⁇ 1> to ⁇ 6>, Table 1 [Part 2] ⁇ 1> to ⁇ 6>, Table 1 [Part 3] ⁇ 1> to ⁇ 6> and Table 1 [Part 4], which are shown in each row of ⁇ 1> to ⁇ 6>.
  • Example 1 as shown in Table 1 [Part 1] ⁇ 1>, CyHe was used as the organic solvent, and as shown in Table 1 [Part 1] ⁇ 2>, the filter 2 was “IEX 15 nm”.
  • the medicinal solution of the present invention could provide a predetermined effect.
  • comparison of Examples 1 to 8 confirmed that the effect was more excellent when the mass ratio of the content of titanium oxide particles to the content of titanium ions was 10 1 to 10 10 .
  • Examples 9 and 10 it was confirmed that the effect was more excellent when the mass ratio of the content of iron oxide particles to the content of iron ions was 10 0 to 10 12 .
  • Examples 11 and 12 to the content of aluminum ions, when the mass ratio of the content of aluminum oxide particles is 10 0 to 10 12, it was confirmed that more effective is excellent.
  • the content of titanium ion (or iron ion or aluminum ion) was 0.10 to 100 with respect to the total mass of the chemical solution. It was confirmed that the effect was more excellent when the mass was ppt. Further, according to Examples 16 and 17 (37 and 38, 58 and 59, 79 and 80), the content of the titanium oxide particles (or the iron oxide particles and the aluminum oxide particles) was reduced by the content of the titanium component in the metal component. On the other hand, when the content was 5% by mass or more and less than 99% by mass, it was confirmed that the effect was more excellent.
  • Examples 18 and 19 (39 and 40, 60 and 61, 81 and 82), of titanium oxide particles (or iron oxide particles and aluminum oxide particles), particles having a particle size of 0.5 to 17 nm were obtained.
  • the proportion was 60% by mass or more and less than 98% by mass, it was confirmed that the effect was more excellent.
  • Examples 20 and 21 (41 and 42, 62 and 63, 83 and 84), the effect is more excellent when the content of organic impurities is 1000 to 100000 mass ppt with respect to the total mass of the chemical solution. Was confirmed.
  • Example 22 After cleaning the container (EP-SUS) and various devices used in the ⁇ purification procedure> using the chemical solution of Example 22 (100 L), the separately prepared chemical solution of Example 22 was passed through the washed device, The solution was collected in a washed container, and a solution A was obtained in the container. After cleaning the container (EP-SUS) and various devices used in ⁇ Purification Procedure> using the chemical solution (100 L) of Example 38, the chemical solution of Example 22 separately prepared was poured into the above-described washed device. Then, the solution was collected in a washed container, and a solution B was obtained in the container. When the “metal residue defect on Si” was evaluated using the solution A and the solution B, better results were obtained with the solution A.
  • a resist composition 1 was obtained by mixing each component with the following composition.
  • Photoacid generator (B-1) The following compounds were used as the photoacid generator (B-1).
  • the resist composition 1 was applied on a silicon wafer having a diameter of 300 mm, and baked (PB: Prebake) at 100 ° C. for 60 seconds to form a resist film having a thickness of 30 nm.
  • the resist film was exposed through a reflective mask using an EUV exposure machine (manufactured by ASML; NXE3350, NA 0.33, Dipole 90 °, outer sigma 0.87, inner sigma 0.35). Thereafter, heating (PEB: Post Exposure Bake) was performed at 85 ° C. for 60 seconds. Next, a developing solution (butyl acetate / manufactured by FETW) was sprayed for 30 seconds by a spray method for development, and a rinsing liquid was discharged onto a silicon wafer for 20 seconds by a spin coating method to be rinsed.
  • EUV exposure machine manufactured by ASML; NXE3350, NA 0.33, Dipole 90 °, outer sigma 0.87, inner sigma 0.35.
  • heating PEB: Post Exposure Bake
  • a developing solution butyl acetate / manufactured by FETW
  • a rinsing liquid was discharged onto a silicon wafer for 20 seconds by a spin coating method to be rinsed.
  • the silicon wafer was rotated at a rotation speed of 2000 rpm for 40 seconds to form a line-and-space pattern having a space width of 20 nm and a pattern line width of 15 nm.
  • the rinsing liquid the chemical liquid used in Example 44 described above was used.

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  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Power Engineering (AREA)
  • Materials For Photolithography (AREA)
  • Photosensitive Polymer And Photoresist Processing (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
  • Electrodes Of Semiconductors (AREA)
  • Materials For Medical Uses (AREA)

Abstract

L'invention concerne : une solution chimique qui est moins susceptible de provoquer des défauts de résidu métallique lorsqu'elle est mise en contact avec un substrat de silicium ou avec un substrat de silicium doté d'un film d'oxyde de silicium ; et un récipient pour solution chimique. Cette solution chimique consiste en une solution chimique contenant un solvant organique et un composant métallique, le composant métallique contenant des particules d'oxyde de titane et des ions de titane, et le rapport en masse de la teneur en particules d'oxyde de titane par rapport à la teneur en ions de titane se situant entre 100 et 1012, de manière inclusive.
PCT/JP2019/032088 2018-08-21 2019-08-16 Solution chimique et récipient pour solution chimique WO2020040042A1 (fr)

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JPWO2020040042A1 (ja) 2021-08-10
TWI815952B (zh) 2023-09-21

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