WO2021215263A1 - エラストマー組成物及びそれからなるシール材 - Google Patents

エラストマー組成物及びそれからなるシール材 Download PDF

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Publication number
WO2021215263A1
WO2021215263A1 PCT/JP2021/014937 JP2021014937W WO2021215263A1 WO 2021215263 A1 WO2021215263 A1 WO 2021215263A1 JP 2021014937 W JP2021014937 W JP 2021014937W WO 2021215263 A1 WO2021215263 A1 WO 2021215263A1
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Prior art keywords
mass
sealing material
parts
comparative example
silica
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English (en)
French (fr)
Japanese (ja)
Inventor
裕明 安田
隆男 伊東
龍平 竹田
武広 浜村
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Mitsubishi Cable Industries Ltd
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Mitsubishi Cable Industries Ltd
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Priority to US17/920,002 priority Critical patent/US20230174763A1/en
Priority to KR1020227036418A priority patent/KR102803202B1/ko
Priority to CN202180027743.6A priority patent/CN115443305B/zh
Publication of WO2021215263A1 publication Critical patent/WO2021215263A1/ja
Anticipated expiration legal-status Critical
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/16Homopolymers or copolymers or vinylidene fluoride
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L21/00Compositions of unspecified rubbers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L61/00Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
    • C08L61/04Condensation polymers of aldehydes or ketones with phenols only
    • C08L61/06Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/10Materials in mouldable or extrudable form for sealing or packing joints or covers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/10Materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K3/1006Materials in mouldable or extrudable form for sealing or packing joints or covers characterised by the chemical nature of one of its constituents
    • C09K3/1009Fluorinated polymers, e.g. PTFE
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16JPISTONS; CYLINDERS; SEALINGS
    • F16J15/00Sealings
    • F16J15/02Sealings between relatively-stationary surfaces
    • F16J15/06Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
    • F16J15/10Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with non-metallic packing
    • F16J15/102Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with non-metallic packing characterised by material
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/20Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/14Peroxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/34Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477Six-membered rings
    • C08K5/3492Triazines
    • C08K5/34924Triazines containing cyanurate groups; Tautomers thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/14Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/18Spheres
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00Crosslinking
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/10Materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2003/1087Materials or components characterised by specific uses
    • C09K2003/1096Cylinder head gaskets
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2200/00Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2200/02Inorganic compounds
    • C09K2200/0243Silica-rich compounds, e.g. silicates, cement, glass
    • C09K2200/0247Silica
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2200/00Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2200/06Macromolecular organic compounds, e.g. prepolymers
    • C09K2200/0615Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09K2200/0635Halogen-containing polymers, e.g. PVC
    • C09K2200/0637Fluoro-containing polymers, e.g. PTFE
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2200/00Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2200/06Macromolecular organic compounds, e.g. prepolymers
    • C09K2200/0645Macromolecular organic compounds, e.g. prepolymers obtained otherwise than by reactions involving carbon-to-carbon unsaturated bonds
    • C09K2200/067Condensation polymers of aldehydes or ketones
    • C09K2200/0672Phenol-aldehyde condensation polymers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2200/00Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2200/06Macromolecular organic compounds, e.g. prepolymers
    • C09K2200/068Containing also other elements than carbon, oxygen or nitrogen in the polymer main chain
    • C09K2200/0685Containing silicon

Definitions

  • the present disclosure relates to an elastomer composition and a sealing material comprising the elastomer composition.
  • Elastomer compositions with various properties are known and are used according to the purpose.
  • hardness, tensile strength, compression fracture resistance, compression set, and the like are important.
  • Patent Document 1 discloses that the resistance to compression fracture is enhanced by reducing the crosslink density of rubber. Further, Patent Document 2 discloses that the resistance to compression fracture is enhanced by controlling the molecular weight of rubber.
  • the crushing rate is limited when using the sealing material to avoid compression failure.
  • the crushing rate may be larger than expected.
  • the coefficient of linear expansion of rubber increases and the strength decreases, so that compression fracture is likely to occur.
  • An object of the present disclosure is to realize desirable properties such as compression fracture characteristics and compression set, with respect to the elastomer composition and the sealing material using the elastomer composition.
  • the elastomer composition of the present disclosure contains an elastomer, a powdered phenolic resin, and powdered silica. Further, the sealing material of the present disclosure is obtained by cross-linking the elastomer composition of the present disclosure. Further, the sealing material of the present disclosure is a sealing material used in a semiconductor manufacturing apparatus.
  • the elastomer composition of the present embodiment contains an elastomer, a powdered phenolic resin, and powdered silica.
  • an elastomer composition containing both a phenol resin and silica it is possible to produce an article having excellent compression fracture resistance and compression set.
  • articles include sealing materials for obtaining airtightness in mechanical devices, particularly sealing materials used in semiconductor manufacturing equipment.
  • a fluoroelastomer and a silicone elastomer are desirable. It may consist of only one of these, or may include both. Other types of elastomers may be contained, with these elastomers as the main component (50% by mass or more). For the purpose of achieving excellent compression fracture resistance and compression set, it is desirable to contain a fluoroelastomer, and it is more desirable to use only a fluoroelastomer.
  • fluorine elastomer examples include a copolymer of vinylidene fluoride (VDF) and hexafluoropropylene (HFP) (binary FKM), vinylidene fluoride (VDF), hexafluoropropylene (HFP), and tetrafluoroethylene (HFP).
  • VDF vinylidene fluoride
  • HFP hexafluoropropylene
  • HFP tetrafluoroethylene
  • Copolymer with (TFE) (ternary FKM), copolymer with tetrafluoroethylene (TFE) and propylene (Pr) (FEP), vinylidene fluoride (VDF), propylene (Pr) and tetrafluoroethylene (Pr) Copolymer with TFE), Copolymer with ethylene (E) and tetrafluoroethylene (TFE) (ETFE), Copolymer with ethylene (E), tetrafluoroethylene (TFE) and perfluoromethylvinyl ether (PMVE) Polymers, copolymers of vinylidene fluoride (VDF) and tetrafluoroethylene (TFE) and perfluoromethyl vinyl ether (PMVE), copolymers of vinylidene fluoride (VDF) and perfluoromethyl vinyl ether (PMVE), Examples thereof include a copolymer of tetrafluoroethylene (TFE) and perfluoroalkyl ether (
  • binary FKM binary FKM
  • ternary FKM FEPM
  • FFKM perfluoropolyether
  • a polyol cross-linking and a peroxide (organic peroxide) cross-linking are known, but either of them can be used.
  • Polyol cross-linking is superior to peroxide cross-linking in terms of compression set.
  • HF is generated during the cross-linking reaction, so it is necessary to add MgO, Ca (OH) 2, etc. in order to absorb this.
  • the fluoroelastomer crosslinked with a polyol contains more metals than the fluoroelastomer crosslinked with peroxide, and tends to generate dust easily in a plasma environment.
  • peroxide cross-linking is preferable as the sealing material for semiconductor manufacturing equipment.
  • peroxide cross-linking is preferable from the viewpoint of chemical resistance and steam property (which tends to decrease due to metal oxide).
  • the fluoroelastomer crosslinked with a polyol the effect of improving the compression set is realized by blending the phenol resin powder, so the case of crosslinking the polyol is not excluded.
  • Peroxide is a thermal cross-linking agent that cross-links rubber components when heated to a predetermined temperature.
  • Specific examples include 1,1-bis (t-butylperoxy) -3,5,5-trimethylcyclohexane, 2,5-dimethylhexane-2,5-dihydroperoxide, di-t-butyl peroxide, and the like.
  • t-butylcumyl peroxide dicumyl peroxide, ⁇ , ⁇ -bis (t-butylperoxy) -p-diisopropylbenzene, 2,5-dimethyl-2,5-di (t-butylperoxy) hexane, 2,5-Dimethyl-2,5-di (t-butylperoxy) -hexin-3, benzoyl peroxide, t-butylperoxybenzene, t-butylperoxymaleic acid, t-butylperoxyisopropyl carbonate, Examples thereof include t-butylperoxybenzoate.
  • the peroxide it is preferable to use one or more of these, and from the viewpoint of obtaining excellent physical properties, 2,5-dimethyl-2,5-di (t-butylperoxy) hexane should be used. Is more preferable.
  • bisphenols are preferable. Specifically, for example, 2,2-bis (4-hydroxyphenyl) propane [bisphenol A], 2,2-bis (4-hydroxyphenyl) perfluoropropane [bisphenol AF], bis (4-hydroxyphenyl).
  • Polyhydroxyaromatics such as sulfone [bisphenol S], bisphenol A-bis (diphenyl phosphate), 4,4'-dihydroxydiphenyl, 4,4'-dihydroxydiphenylmethane, 2,2-bis (4-hydroxyphenyl) butane. Examples include compounds.
  • bisphenol A, bisphenol AF and the like are preferable from the viewpoint of obtaining excellent physical properties. These may be in the form of alkali metal salts or alkaline earth metal salts.
  • silicone rubber examples include methyl vinyl silicone rubber, methyl vinyl phenyl silicone rubber, fluorosilicone rubber and the like. As the silicone rubber, it is preferable that one or more of these are used. Cross-linking of the silicone rubber may be carried out by using an organic peroxide, by condensation polymerization, or by using a platinum catalyst.
  • the average particle size is preferably 20 ⁇ m or less, more preferably 10 ⁇ m or less, and even more preferably 6 ⁇ m or less.
  • the average particle size refers to the 50% particle size measured by the laser diffraction / scattering method.
  • the phenol resin has been reacted.
  • the extract content when heated and recirculated in methanol is 10% by mass or less.
  • a phenol resin having a free phenol content of 500 ppm or less is preferable.
  • the amount of the phenol resin blended is preferably 1 part by mass or more, more preferably 3 parts by mass or more, and further preferably 5 parts by mass or more with respect to 100 parts by mass of the rubber component.
  • the blending amount of the phenol resin is preferably 30 parts by mass or less, more preferably 25 parts by mass or less, and further preferably 15 parts by mass or less.
  • silica is also preferably used as a powder.
  • Silica preferably has a specific surface area of 90 m 2 / g or more as measured by the BET method.
  • synthetic amorphous silica such as dry silica and wet silica is preferable, dry silica such as hydrophilic dry silica and hydrophobic dry silica is more preferable, and hydrophobic dry silica is further preferable.
  • silica may be surface-treated.
  • it may be surface-treated with a silane coupling agent to introduce a methyl group, a dimethyl group, a trimethyl group, or the like.
  • the amount of silica blended is preferably 1 part by mass or more, more preferably 3 parts by mass or more, and further preferably 5 parts by mass or more with respect to 100 parts by mass of the rubber component.
  • the blending amount of silica is preferably 30 parts by mass or less, more preferably 25 parts by mass or less, and further preferably 15 parts by mass or less.
  • the fluoroelastomer composition constituting the sealing material of the present embodiment may further contain a hydrogen site protectant.
  • a hydrogen site protectant is a compound that binds to a carbon radical generated by breaking the carbon-hydrogen bond of a rubber component when irradiated with radiation during the production of a rubber product.
  • the hydrogen site protectant is a compound having a perfluoro skeleton having an alkenyl group bonded to a carbon radical of a rubber component in the molecule, and / or a siloxane skeleton having an alkenyl group having an alkenyl group bonded to a carbon radical of a rubber component in the molecule. It is preferable to contain the compound of.
  • the alkenyl group include a vinyl group, an allyl group, a butenyl group, a pentenyl group, a hexenyl group, a heptenyl group and the like.
  • the alkenyl group is preferably a vinyl group among these.
  • Examples of the compound having a perfluoroskeleton having an alkenyl group in the molecule include a compound having a perfluoropolyether structure and a compound having a perfluoroalkylene structure.
  • Examples of the compound having a siloxane skeleton having an alkenyl group in the molecule include a polymer of methylvinylsiloxane, a polymer of dimethylsiloxane, a copolymer of dimethylsiloxane and methylvinylsiloxane, and dimethylsiloxane, methylvinylsiloxane and methylphenyl. Examples thereof include a copolymer with siloxane.
  • an organopolysiloxane containing an alkenyl group in the molecule which is an addition-polymerized liquid silicone rubber, can be mentioned. As the hydrogen site protectant, it is preferable to use one or more of these.
  • the content of the hydrogen site protectant is preferably 1 part by mass or more, more preferably 5 parts by mass or more, and preferably 20 parts by mass with respect to 100 parts by mass of the rubber component from the viewpoint of enhancing plasma resistance. Hereinafter, it is more preferably 15 parts by mass or less.
  • the uncrosslinked fluororubber composition can be prepared using an open rubber kneader such as an open roll or a closed rubber kneader such as a kneader. Of these, excellent kneading workability can be obtained particularly in an open type rubber kneader such as an open roll.
  • an article such as a sealing material from the above fluororubber composition
  • processing using a mold is performed. That is, a predetermined amount of the uncrosslinked fluororubber composition according to the present embodiment is filled in the cavity of the preheated mold, then molded, and then in that state, a predetermined molding temperature and a predetermined molding pressure are used. Hold for the molding time of. At this time, the uncrosslinked fluororubber composition is formed into the shape of the cavity, and the rubber component is crosslinked by the crosslinking agent to lose its plasticity.
  • This molding may be press molding or injection molding.
  • the molding temperature is, for example, 150 ° C. or higher and 180 ° C. or lower.
  • the molding pressure is, for example, 0.1 MPa or more and 25 MPa or less.
  • the molding time is, for example, 3 minutes or more and 20 minutes or less.
  • the rubber product can be obtained by opening the mold, taking out the molded product from the inside, and cooling the molded product.
  • the molded product taken out from the mold may be further heat-treated at a heating temperature of 150 ° C. or higher and 250 ° C. or lower and a heating time of 2 hours or more and 24 hours or less.
  • the sealing material manufactured as described above can be used to obtain airtightness in mechanical devices.
  • it can be used under high temperature and high pressure conditions, and can be effectively used in semiconductor manufacturing equipment and the like.
  • Examples 1 to 7 and Comparative Examples 1 to 15 will be described with respect to the elastomer composition of the present disclosure and a sealing material for a semiconductor manufacturing apparatus using the same.
  • the formulations and properties are also shown in Tables 1 to 3, respectively.
  • Example 2 The blending amounts of the phenol resin powder (Belpearl R100) and silica (Aerosil R972) are both 10 parts by mass (relative to 100 parts by mass of fluororubber.
  • the mass parts of the compounding agent are the same as those with respect to 100 parts by mass of the rubber component.
  • the sealing material of Example 2 was produced in the same manner as in Example 1 except that the above was omitted.
  • Example 3 The sealing material of Example 3 was prepared in the same manner as in Example 1 except that the amount of the phenol resin powder (Belpearl R100) was 25 parts by mass and the amount of silica (Aerosil R972) was 5 parts by mass.
  • Example 4 The sealing material of Example 4 was prepared in the same manner as in Example 1 except that the amount of the phenol resin powder (Belpearl R100) was 5 parts by mass and the amount of silica (Aerosil R972) was 25 parts by mass.
  • Example 5 The sealing material of Example 5 was prepared in the same manner as in Example 1 except that the amounts of the phenol resin powder (Belpearl R100) and silica (Aerosil R972) were both 25 parts by mass.
  • Example 6 2.5 parts by mass of cross-linking agent and catalyst (Chemers, trade name: Curative V-50), as an acid receiving agent, with respect to 100 parts by mass of FKM (manufactured by Chemers, trade name: Byton A-50), which is a fluororubber component.
  • FKM manufactured by Chemers, trade name: Byton A-50
  • Byton A-50 which is a fluororubber component.
  • Magnesium oxide manufactured by Kyowa Chemical Industry Co., Ltd., trade name: Kyowa Mug 150
  • calcium hydroxide manufactured by Omi Chemical Industry Co., Ltd., trade name: Calbit
  • phenol resin powder Belpearl R100
  • Example 7 Organic peroxide as a cross-linking material (manufactured by Shin-Etsu Chemical Co., Ltd., manufactured by Shin-Etsu Chemical Co., Ltd.) Product name: C-88) 2 parts by mass and 10 parts by mass of phenol resin powder (Belpearl R100) were added and kneaded by an open roll. The kneaded compound was press molded at 160 ° C. for 10 minutes. Then, secondary cross-linking was carried out in a gear oven at 200 ° C. for 4 hours. The obtained sealing material was used as the sealing material of Example 7.
  • the silica content in VMQ is calculated by using the weight of the residue when the silicone rubber is thermally decomposed in a nitrogen atmosphere as the silica weight.
  • Comparative Example 1 The sealing material of Comparative Example 1 was prepared in the same manner as in Example 1 except that the amount of the phenol resin powder (Belpearl R100) and silica (Aerosil R972) was 0 parts by mass (that is, not added).
  • Comparative Example 2 The sealing material of Comparative Example 2 was produced in the same manner as in Comparative Example 1 except that the amount of the phenol resin powder (Belpearl R100) blended was 10 parts by mass.
  • Comparative Example 3 The sealing material of Comparative Example 3 was produced in the same manner as in Comparative Example 1 except that the amount of the phenol resin powder (Belpearl R100) blended was 25 parts by mass.
  • Comparative Example 4 The sealing material of Comparative Example 4 was prepared in the same manner as in Comparative Example 1 except that the amount of the phenol resin powder (Belpearl R100) blended was 50 parts by mass.
  • Comparative Example 5 As the phenol resin powder, the sealing material of Comparative Example 5 was produced in the same manner as in Comparative Example 2 except that Belpearl R800 (trade name, manufactured by Air Water Belpearl Co., Ltd.) was used instead of Belpearl R100.
  • the average particle size of Belpearl R800 is 22 ⁇ m.
  • Comparative Example 6 The sealing material of Comparative Example 6 was prepared in the same manner as in Comparative Example 1 except that the blending amount of silica (Aerosil R972) was 10 parts by mass.
  • Comparative Example 7 The sealing material of Comparative Example 7 was prepared in the same manner as in Comparative Example 1 except that the amount of silica (Aerosil R972) blended was 25 parts by mass.
  • Comparative Example 8 An attempt was made to prepare a sealing material of Comparative Example 8 in the same manner as in Comparative Example 1 except that the amount of silica (Aerosil R972) was 25 parts by mass, but roll kneading was not possible when about 40 parts by mass of silica was added. It became possible and could not be produced.
  • the amount of silica (Aerosil R972) was 25 parts by mass, but roll kneading was not possible when about 40 parts by mass of silica was added. It became possible and could not be produced.
  • Comparative Example 9 A sealing material of Comparative Example 9 was produced in the same manner as in Comparative Example 1 except that 25 parts by mass of carbon black (manufactured by Cancarb, trade name Thermax N990) was further added.
  • Comparative Example 10 A sealing material of Comparative Example 10 was prepared in the same manner as in Comparative Example 1 except that 10 parts by mass of carbon black (Thermax N990) and 10 parts by mass of phenol resin powder (Belpearl R100) were further added.
  • Comparative Example 11 A sealing material of Comparative Example 11 was prepared in the same manner as in Comparative Example 1 except that 10 parts by mass of carbon black (Thermax N990) and 10 parts by mass of silica (Aerosil R972) were further added.
  • Comparative Example 12 The sealing material of Comparative Example 12 was prepared in the same manner as in Example 6 except that the amount of the phenol resin powder (Belpearl R100) and silica (Aerosil R972) was 0 parts by mass (that is, not added).
  • Comparative Example 13 The sealing material of Comparative Example 13 was prepared in the same manner as in Comparative Example 12 except that the amount of the phenol resin powder (Belpearl R100) blended was 10 parts by mass.
  • Comparative Example 14 The sealing material of Comparative Example 14 was prepared in the same manner as in Comparative Example 12 except that the amount of silica (Aerosil R972) blended was 10 parts by mass.
  • Comparative Example 15 The sealing material of Comparative Example 15 was prepared in the same manner as in Example 7 except that the amount of the phenol resin powder (Belpearl R100) blended was 0 parts by mass (that is, not added).
  • the compression set of the prepared sealing material was measured by a test piece in which the AS-214 O-ring was cut in half based on JIS K6262.
  • the heating conditions were 150 ° C. and 72 hours for Example 5 and Comparative Example 15, and 200 ° C. and 72 hours for others.
  • the compression rate was 25%.
  • compression fracture resistance The compression fracture resistance of the prepared sealing material was measured in the same manner as the measurement of compression set, except that the compression rate was 50% and the heating conditions were 180 ° C. for 4 hours without cutting the O-ring. Each was performed on 3 test pieces, and the number of cracks not generated was recorded.
  • Table 1 shows the formulation of the elastomer composition and the test evaluation results for Examples 1 to 5 and Comparative Examples 1 to 11.
  • Comparative Example 1 is an example in which neither phenol resin nor silica is blended. The test piece was cracked three times by the compression fracture resistance test, and the compression fracture resistance was low.
  • Comparative Examples 2 to 4 in which only the phenol resin is blended, there is a tendency that the compression fracture resistance is improved by increasing the blending amount.
  • the blending amount was 50 parts by mass, it was cracked once in three tests.
  • Example 1 in which the total blending amount of the phenol resin and silica is 10 parts by mass in total, cracking is prevented. Therefore, the compression fracture resistance cannot be sufficiently improved by simply increasing the blending amount, and the use of both the phenol resin and silica is effective.
  • Comparative Example 6 the compression set is 36%, whereas in Example 2, it is 18%. Since the blending amount of silica is the same in these two examples, it has been shown that the compression set is improved by blending the phenol resin. The same is shown from the comparison between Comparative Example 7 and Example 4. The compression set tends to deteriorate when silica is blended, but the deterioration is suppressed by further blending a phenol resin.
  • Comparative examples 9 to 11 are examples in which carbon black is blended. Some improvement in compression fracture resistance (compared to Comparative Example 1) is seen, but it is insufficient. Comparative Example 10 in which the phenol resin is further blended is superior to Comparative Example 9 or 11, but is not as good as the examples.
  • the tensile strength is around 20, which is a desirable value.
  • the tensile strength of Examples 1 to 5 is 20 or more. That is, with respect to the tensile strength, when both phenol resin and silica are blended as a filler, there is an effect equivalent to that of carbon black, which is a general filler. Therefore, the compressive fracture resistance can be improved without deteriorating the tensile strength.
  • Comparative Example 5 differs from Example 2 only in the average particle size of the phenol resin.
  • the average particle size of the phenol resin is about 1.5 ⁇ m, and in Comparative Example 5, it is about 22 ⁇ m.
  • Example 6 and Comparative Examples 12 to 14 are examples in which a fluororubber crosslinked with a polyol is used.
  • Example 6 In Example 6 in which the phenol resin and silica were blended together, no cracks were generated in the compression fracture resistance test. On the other hand, in Comparative Examples 12 to 14 in which one or both of the phenol resin and silica were blended, cracks were generated.
  • Example 7 and Comparative Example 15 are examples in which silicone rubber is used. Although not shown directly in Table 3, the silicone rubber used contains silica. Therefore, both Example 7 and Comparative Example 15 contain silica, and the difference is whether or not they contain a phenol resin.
  • Example 7 no cracks occurred in the compression fracture resistance test. On the other hand, in Comparative Example 15, cracking occurred once in three tests. Therefore, it was shown that even when silicone rubber is used, the compression fracture resistance is improved by blending both the phenol resin and silica.
  • the elastomer composition and the sealing material of the present disclosure are excellent in properties such as compression fracture property and compression set, they are useful for use under conditions where the requirements for these properties are strict. Further, since the elastomer composition of the present disclosure is excellent in properties such as compression fracture property and compression set, it is useful for molding into, for example, a hose, a tube, a transfer pad, and a transfer roller.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Sealing Material Composition (AREA)
  • Gasket Seals (AREA)
PCT/JP2021/014937 2020-04-21 2021-04-08 エラストマー組成物及びそれからなるシール材 Ceased WO2021215263A1 (ja)

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