Seal composition and seal

Abstract

The present disclosure relates to a seal composition containing a fluoroelastomer, a silicone polymer having a vinyl group, and a crosslinking agent, a seal containing a crosslinked product of the seal composition, a gate valve seal for a semiconductor manufacturing apparatus containing the seal, and a semiconductor manufacturing apparatus. According to the present disclosure, a seal composition capable of exerting an improved 100% modulus, a seal containing a crosslinked product of the seal composition, and a gate valve seal for a semiconductor manufacturing apparatus and a semiconductor manufacturing apparatus containing the seal are provided.

Description

Technical Field

[0001] This invention relates to sealing compositions, and more particularly to a full range of sealing components, including gate valve seals for semiconductor manufacturing apparatuses containing the sealing components, and semiconductor manufacturing apparatuses. Background Technology

[0002] In Japanese Patent Application Publication No. 2000-119468 (Patent Document 1), a composition comprising a crosslinkable fluorinated elastomer was proposed as a composition for manufacturing a seal.

[0003] Existing technical documents Patent documents Patent Document 1: Japanese Patent Application Publication No. 2000-119468 Summary of the Invention

[0004] The problem that the invention aims to solve However, when crosslinked compositions containing fluoroelastomers are used as dynamic seals, 100% modulus is sometimes insufficient.

[0005] The object of the present invention is to provide a sealing composition capable of achieving an enhanced 100% modulus, a sealing element comprising a crosslinked thereof, a gate valve seal for a semiconductor manufacturing apparatus, and a semiconductor manufacturing apparatus.

[0006] Solution for solving the problem The present invention provides the following sealing composition, sealing element, gate valve seal for semiconductor manufacturing apparatus, and semiconductor manufacturing apparatus.

[0007] [1] A sealing composition comprising a fluoroelastomer, a vinyl-based silicone polymer, and a crosslinking agent.

[0008] [2] The sealing composition according to [1], wherein the silicone polymer comprises at least one selected from the group consisting of vinylmethyl polysiloxane, fluorovinylmethyl polysiloxane and phenylvinylmethyl polysiloxane.

[0009] [3] The sealing composition according to [1] or [2], wherein the content of the silicone polymer is more than 1 part by mass and less than 500 parts by mass relative to 100 parts by mass of the fluoroelastomer.

[0010] [4] The sealing composition according to any one of [1] to [3], wherein the crosslinking agent comprises at least one selected from the group consisting of peroxide compounds, polyol compounds and polyamine compounds.

[0011] [5] The sealing composition according to any one of [1] to [4], wherein the content of the crosslinking agent is 1 to 6 parts by weight relative to 100 parts by weight of the fluoroelastomer.

[0012] [6] The sealing composition according to any one of [1] to [5], wherein it further comprises a perfluoropolyether compound.

[0013] [7] The sealing composition according to [6], wherein the content of the perfluoropolyether compound is 0.5 to 30 parts by weight relative to 100 parts by weight of the fluoroelastomer.

[0014] [8] A sealing composition according to any one of [1] to [7], wherein it further comprises: a filler in a quantity of 1 to 30 parts by weight relative to 100 parts by weight of the fluoroelastomer.

[0015] [9] The sealing composition according to [8], wherein the filler comprises silicon dioxide.

[0016]

[10] The sealing composition according to [8], wherein the filler comprises a fluoropolymer, and the fluoropolymer comprises polytetrafluoroethylene.

[0017]

[11] A seal comprising a crosslinked material of a seal composition as described in any one of [1] to

[10] .

[0018]

[12] A gate valve seal for a semiconductor manufacturing apparatus, comprising the seal as described in

[11] .

[0019]

[13] A semiconductor manufacturing apparatus comprising a seal as described in

[11] .

[0020] Invention Effects According to the present invention, it is possible to provide a sealing composition exhibiting an enhanced 100% modulus, a sealing element containing a crosslink thereof, a gate valve seal for a semiconductor manufacturing apparatus, and a semiconductor manufacturing apparatus. Detailed Implementation

[0021] The embodiments of the present invention will be described below, but the present invention is not limited to the following embodiments.

[0022] <Sealing Composition> One aspect of the present invention is a sealing composition for manufacturing seals for semiconductor manufacturing apparatuses. The sealing composition comprises a fluoroelastomer, a vinyl-based silicone polymer (hereinafter also referred to as vinyl polysiloxane), and a crosslinking agent.

[0023] (Fluoroelastics) Fluoroelastics are cross-linked rubber components capable of forming elastomers (cross-linked rubber) with cross-linked structures through cross-linking reactions. They are composed of polymers or copolymers containing at least one of hydrogen atoms or monomers containing both hydrogen and fluorine atoms as structural units, or fluorine-based thermoplastic elastomers containing hydrogen atoms. Cross-linked rubber refers to a substance that exhibits rubber elasticity by using cross-linking agents or the like to induce cross-linking reactions between the molecular chains of the cross-linked rubber component (fluoroelastic), thereby giving it a cross-linked structure.

[0024] Specific examples of fluoroelastomers include: vinylidene fluoride (VDF)-hexafluoropropylene (HFP) copolymers; vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymers; tetrafluoroethylene (TFE)-propylene (Pr) copolymers; vinylidene fluoride (VDF)-propylene (Pr)-tetrafluoroethylene (TFE) copolymers; ethylene (E)-tetrafluoroethylene (TFE)-perfluoromethyl vinyl ether (PMVE) copolymers; vinylidene fluoride (VDF)-tetrafluoroethylene (TFE)-perfluoromethyl vinyl ether (PMVE) copolymers; and so on. A single fluoroelastomer can be used, or two or more can be used in combination.

[0025] The Mooney viscosity of the fluoroelastomer at 121°C can be, for example, 20 or higher. From the viewpoint of achieving good 100% modulus, elongation, and tensile strength of the obtained seal, the Mooney viscosity of the fluoroelastomer at 121°C is preferably 25 or higher, more preferably 40 or higher, and even more preferably 56 or higher. The Mooney viscosity can be measured according to JIS K6300-1:2013.

[0026] There are no particular restrictions on fluorinated thermoplastic elastomers containing hydrogen atoms. For example, "DAI-EL Thermoplastic" (manufactured by Daikin Industries, Ltd.) and "Cefral Soft" (manufactured by Central Glass Co., Ltd.) are both trade names.

[0027] (Silicone polymers containing vinyl groups) Vinyl polysiloxanes can be polymers or copolymers composed of structural units derived from siloxane compounds. Vinyl polysiloxanes may have vinyl groups at at least one location at the end of the main chain and in all of the side chains, or they may have vinyl groups at the end of the main chain and in all of the side chains. In vinyl polysiloxanes, the ratio of terminal groups bonded to silicon atoms to vinyl groups in the side chains can be, for example, 0.01 to 15 mol%. Vinyl polysiloxanes may be modified with halogen elements, for example, or may have aromatic monovalent hydrocarbon groups. The degree of polymerization of vinyl polysiloxanes can be, for example, 100 or more, preferably 1000 or more, more preferably 2000 or more, and even more preferably 3000 or more. The degree of polymerization of vinyl polysiloxanes can be, for example, 10000 or less. The degree of polymerization can be determined, for example, by analyzing the number-average degree of polymerization of polystyrene using gel permeation chromatography (GPC) with toluene or the like as the developing solvent.

[0028] Vinyl polysiloxane may contain a structural unit (first structural unit) represented by the following formula (1). [In the formula, R] 1 Each of the following can independently represent a substituted or unsubstituted aromatic monovalent hydrocarbon group, a substituted or unsubstituted unsaturated hydrocarbon group or a saturated hydrocarbon group without an aromatic hydrocarbon group, an alkoxy group, a hydroxyl group or a hydrogen atom. Vinyl polysiloxanes may contain one or more first structural units.

[0029] Examples of unsubstituted aromatic monovalent hydrocarbon groups include aryl groups such as phenyl and tolyl, and aralkyl groups such as benzyl and phenethyl. Substituted unsubstituted aromatic monovalent hydrocarbon groups can be groups in which some or all of the hydrogen atoms in the groups exemplified above as unsubstituted aromatic monovalent hydrocarbon groups are replaced by halogen atoms such as fluorine or chlorine; examples include chlorophenyl.

[0030] Examples of unsubstituted saturated hydrocarbon groups that do not contain aromatic hydrocarbon groups include alkyl groups such as methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl, pentyl, hexyl, cyclohexyl, octyl, decyl, and dodecyl. Examples of unsubstituted unsaturated hydrocarbon groups that do not contain aromatic hydrocarbon groups include alkenyl, allyl, propenyl, isopropenyl, butenyl, and isobutylenyl. Examples of substituted unsaturated or saturated hydrocarbon groups that do not contain aromatic hydrocarbon groups are groups in which some or all of the hydrogen atoms in the groups exemplified above as unsubstituted unsaturated or saturated hydrocarbon groups without aromatic hydrocarbon groups are replaced by halogen atoms such as fluorine or chlorine, for example, chloromethyl and 3,3,3-trifluoropropyl.

[0031] Examples of alkoxy groups include methoxy, ethoxy, propoxy, and butoxy.

[0032] Vinyl polysiloxane may contain structural units represented by the following formula (2) (hereinafter also referred to as second structural units). [In the formula, R] 2 and R 3 Independently representing unsubstituted or substituted aromatic monovalent hydrocarbon groups, unsubstituted or substituted unsaturated or saturated hydrocarbon groups without aromatic hydrocarbon groups, alkoxy groups, hydroxyl groups, or hydrogen atoms, wherein R 2 and R 3 [None of these are vinyl]. Vinyl polysiloxanes may contain one or more second structural units.

[0033] As R 2 and R 3 Examples of unsubstituted or substituted aromatic monovalent hydrocarbon groups, unsubstituted or substituted unsaturated or saturated hydrocarbon groups without aromatic hydrocarbon groups, and alkoxy groups are applicable to the above examples other than vinyl groups.

[0034] Vinyl polysiloxanes can have a (R) terminal at the main chain. 4 3Si-R 5 - represents the group (hereinafter also referred to as the terminal group) [where R] 4 Independently representing unsubstituted or substituted aromatic monovalent hydrocarbon groups, unsubstituted or substituted unsaturated or saturated hydrocarbon groups without aromatic hydrocarbon groups, alkoxy or hydroxyl groups, R 5 [Independently representing alkylene groups with 1 to 5 oxygen and carbon atoms]. As R 4 Examples of unsubstituted or substituted aromatic monovalent hydrocarbon groups, unsubstituted or substituted unsaturated or saturated hydrocarbon groups without aromatic hydrocarbon groups, and alkoxy groups are applicable to the above examples. As R 4 Alkyl groups having 1 to 5 carbon atoms, such as methylene, ethylene, and propylene. 4 Preferably, it contains methyl, methoxy, or hydroxyl groups. 5 Preferably, it contains oxygen atoms and ethylene. When the vinyl polysiloxane has vinyl groups at the ends of its main chain, R... 4 At least one of them is vinyl.

[0035] Vinyl polysiloxane is preferably a compound represented by the following formula (3). [In the formula, R] 1 R 2 R 3 R 4 and R 5Applying the above definition, n and o independently represent integers greater than or equal to 1. The sum of n and o can be, for example, 100 or more, preferably 1000 or more, more preferably 2000 or more, and even more preferably 3000 or more. The sum of n and o can be, for example, less than or equal to 10000.

[0036] Vinyl polysiloxane is more preferably a compound represented by the following formula (4), formula (5), or formula (6). [In the formula, R] 4 'Independently representing unsubstituted or substituted unsaturated or saturated hydrocarbon groups, alkoxy or hydroxyl groups, which do not contain aromatic hydrocarbon groups, and p and q independently representing integers greater than 1.' [In the formula, R] 4 ''Independently represent unsubstituted or substituted unsaturated or saturated hydrocarbon groups, alkoxy or hydroxyl groups that do not contain aromatic hydrocarbon groups, and r, s and t independently represent integers greater than 1]. [In the formula, R] 4 Applying the above definitions, u, v, and w independently represent integers greater than 1. In equation (4), R 4 The unsubstituted unsaturated or saturated hydrocarbon groups, alkoxy groups, and hydroxyl groups that do not contain aromatic hydrocarbon groups in ' are subject to the above provisions regarding R'. 4 The definition of R. In equation (5), R 4 The unsubstituted or substituted unsaturated or saturated hydrocarbon groups, alkoxy groups, and hydroxyl groups in '' that do not contain aromatic hydrocarbon groups are subject to the above provisions regarding R. 4 The definition of . The sum of p and q in equation (4), the sum of r, s and t in equation (5), and the sum of u, v and w in equation (6) can be, for example, 100 or more, preferably 1000 or more, more preferably 2000 or more, and even more preferably 3000 or more. The sum of p and q in equation (4), the sum of r, s and t in equation (5), and the sum of u, v and w in equation (6) can be, for example, 10000 or less.

[0037] Vinyl polysiloxanes can be polymers or copolymers containing a first structural unit. For example, vinyl polysiloxanes can be obtained by polymerizing a polymerizable component containing a first structural unit. Alternatively, vinyl polysiloxanes can be obtained by copolymerizing a copolymerizable component containing a first structural unit with other copolymerizable components (e.g., copolymerizable components containing a second structural unit). For example, the compound shown in formula (6) can be obtained by copolymerizing a dimethylsiloxane copolymerizable component, a diphenylsiloxane copolymerizable component, and a methylvinylsiloxane copolymerizable component.

[0038] The vinyl polysiloxane preferably comprises at least one selected from the group consisting of vinyl methyl polysiloxane, fluorovinyl methyl polysiloxane, and phenylvinyl methyl silicone. Examples of vinyl methyl polysiloxanes include, for example, compounds shown in formula (4). Examples of fluorovinyl methyl polysiloxanes include, for example, compounds shown in formula (5). Examples of phenylvinyl methyl polysiloxanes include, for example, compounds shown in formula (6). These vinyl polysiloxanes, as described below, can also be used in the form of silica-filled silicone rubber compounds. Examples of commercially available products include “KE-186-U”, “KE-183-U”, “KE-136Y-U”, and “SE-955-U” manufactured by Dow Toray Industries, Ltd.

[0039] The sealing composition may contain only one vinyl-based silicone polymer, or two or more. Furthermore, the sealing composition may contain other polysiloxane compounds besides vinyl-based silicone polymers, such as dimethyl silicone. Preferably, all silicone polymers contained in the sealing composition are vinyl-based silicone polymers. Additionally, without prejudice to the purpose of the invention, it may also be used as a blend with other rubbers.

[0040] The content of the silicone polymer is, for example, 1 part by mass or more and 500 parts by mass or less relative to 100 parts by mass of the fluoroelastomer. When the content of the silicone polymer is within the above range, there is a tendency for the 100% modulus of the obtained seal to be easily increased. From the viewpoint of 100% modulus, the content of the silicone polymer is preferably 5 to 500 parts by mass, more preferably 5 to 100 parts by mass, even more preferably 5 to 50 parts by mass, and particularly preferably 5 to 30 parts by mass. Furthermore, from the viewpoint of balancing the 100% modulus and elongation of the obtained seal, the content of the silicone polymer is preferably 25 parts by mass or less, more preferably 1 part by mass or more and 25 parts by mass or less, and even more preferably 2 parts by mass or more and 25 parts by mass or less.

[0041] (Cross-linking agent) As a crosslinking agent, at least one selected from the group consisting of peroxide compounds, polyol compounds, and polyamine compounds can be used. As a peroxide compound, there are no particular limitations on any substance that can be used in organosilicon polymers; examples include benzoyl peroxide, p-chlorobenzoyl peroxide, 2,4-dichlorobenzoyl peroxide, di-tert-butyl peroxide, tert-butylcumyl peroxide, dicumyl peroxide, 1,1-di(tert-butylperoxy)-3,3,5-trimethylcyclohexane, 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane, 2,5-dimethyl-2,5-di(tert-butylperoxy)hexyne-3, 1,3-di(tert-butylperoxyisopropyl)benzene, 2,5-dimethyl-2,5-di(benzoyl peroxide)hexane, tert-butyl perbenzoate, tert-butyl isopropyl peroxide, and n-butyl-4,4-di(tert-butylperoxy)valerate, etc. Vulcanizing agents may contain one or more peroxide compounds.

[0042] Examples of polyol compounds include: 2,2-bis(4-hydroxyphenyl)propane (bisphenol A), 2,2-bis(4-hydroxyphenyl)perfluoropropane (bisphenol AF), resorcinol, 1,3-dihydroxybenzene, 1,7-dihydroxynaphthalene, 2,7-dihydroxynaphthalene, 1,6-dihydroxynaphthalene, 4,4'-dihydroxybiphenyl, 4,4'-dihydroxystilbene, 2,6-dihydroxyanthracene, hydroquinone, catechol, 2,2-bis(4-hydroxyphenyl)butane (bisphenol B), 4,4-bis(4-hydroxyphenyl)valerate, 2,2-bis(4-hydroxyphenyl)tetrafluorodichloropropane, 4,4-dihydroxydiphenyl sulfone, 4,4'-dihydroxydiphenyl ketone, tris(4-hydroxyphenyl)methane, 3,3',5,5'-tetrachlorobisphenol A, 3,3',5,5'-tetrabromobisphenol A, etc. These polyhydroxy aromatic compounds can also be alkali metal salts, alkaline earth metal salts, etc. Crosslinking agents can contain one or more polyol compounds.

[0043] Examples of polyamine compounds include hexamethylenediamine carbamate, N,N'-dicinnamylidene-1,6-hexamethylenediamine, and 4,4'-bis(aminocyclohexyl)methane carbamate. Among these, considering the crosslinking properties of the thermoplastic fluoropolymer (A) and the physical properties of the resulting crosslinked body, particularly its compression set, examples of polyamine compounds (b-2) include N,N'-dicinnamylidene-1,6-hexamethylenediamine. The crosslinking agent may contain one or more polyamine compounds.

[0044] The content of the crosslinking agent in the sealing composition may be, for example, 0.5 to 6 parts by weight relative to 100 parts by weight of the fluoroelastomer, preferably 1.5 to 4 parts by weight, and more preferably 2 to 4 parts by weight.

[0045] (Perfluoropolyether compounds) The sealing composition may further comprise a perfluoropolyether compound. The perfluoropolyether compound can be a low molecular weight compound such as an oligomer or a high molecular weight compound such as a polymer. From the viewpoint of 100% modulus and plasma resistance, it is preferable to include a perfluoropolyether polymer. For example, the perfluoropolyether polymer may have groups at the ends of the main chain capable of crosslinking with an organosilicon polymer. Commercially available perfluoropolyether polymers can be used. Examples of commercially available perfluoropolyether polymers include SIFEL8070A / B and X71-906 (both manufactured by Shin-Etsu Chemical Industry Co., Ltd.). The content of the perfluoropolyether compound in the sealing composition may be, for example, 0.5 to 30 parts by weight relative to 100 parts by weight of the fluoroelastomer, preferably 1 to 25 parts by weight, and more preferably 2 to 20 parts by weight.

[0046] (Other ingredients) The sealing composition may contain other components besides those mentioned above, such as pigments, fillers, anti-aging agents, antioxidants, vulcanization accelerators, processing aids (stearic acid, etc.), stabilizers, tackifiers, silane coupling agents, plasticizers, flame retardants, release agents, waxes, lubricants, and other additives. Other examples of additives include viscosity reducers (anti-sticking agents) such as fluorinated oils (e.g., perfluoroethers). Additives may be used individually or in combination with two or more.

[0047] Examples of pigments include, for example, at least one selected from the group consisting of inorganic pigments and organic pigments. Examples of inorganic pigments include, for example, white pigments (e.g., silica, zinc white, lead white, zinc barium white, titanium dioxide, precipitated barium sulfate, and barite powder), red pigments (e.g., red lead oxide, iron oxide red), yellow pigments (e.g., chrome yellow, zinc yellow), blue pigments (e.g., ultramarine blue, Prussian blue, yttrium indium manganese blue), and black pigments (e.g., carbon black). Examples of organic pigments include, for example, azo pigments (azo lake pigments, insoluble azo pigments, condensed azo pigments, etc.); anthraquinone pigments, thioindole pigments, perinone pigments, perylene pigments, quinacridone pigments, isoindoline pigments, isoindoline pigments, dioxazine pigments, quinoline pigments, diketopyrrolopyrrole pigments, and other polycyclic pigments, phthalocyanine pigments, etc. As organic pigments, organic pigments classified as pigments in the color index can be used. Preferably, the pigments used are organic pigments that do not contain metal elements. If organic pigments that do not contain metal elements are used, there is no concern about the dispersion of substances originating from metal elements, even if the seal is sometimes used in harsh ozone environments such as those used in semiconductor applications, resulting in the etching of the annular seal. When the seal composition contains pigments, the pigment content in the seal composition can be, for example, 0.05 to 3 parts by weight relative to 100 parts by weight of the fluoroelastomer.

[0048] Examples of fillers include silica, quartz powder, clay, talc, diatomaceous earth, barium sulfate, mica, graphite, aluminum hydroxide, aluminum silicate, calcium silicate, hydrotalcite, calcium oxide, titanium oxide, zinc oxide, iron oxide, aluminum oxide, magnesium carbonate, calcium carbonate, zinc carbonate, carbon black, granular or powdered resins (fluororesins, etc.), metal powders, glass powders, ceramic powders, etc. When the sealing composition contains a filler, it is advantageous from the viewpoint of improving the mechanical strength of the seal. The filler is preferably at least one selected from the group consisting of silica, carbon black, and fluororesins. From the viewpoint of 100% modulus and plasma resistance, the filler preferably contains silica or fluororesins.

[0049] Examples of silica include fumed silica, precipitated silica, and fused silica. When the sealing composition contains silica, the silica content relative to 100 parts by weight of the fluoroelastomer can be, for example, 6 to 120 parts by weight. When the sealing composition contains silica, a silicone rubber compound incorporating silica into an organosilicon polymer can be used. As a silicone rubber compound, "KE-186-U" manufactured by Shin-Etsu Chemical Co., Ltd., and "SE-955-U" manufactured by Dow Toray Industries, Ltd., can be used directly. Furthermore, without prejudice to the purpose of this invention, it can also be used as a blend rubber with other rubbers.

[0050] Examples of carbon black include MT carbon black. From the viewpoint of preventing filler dispersion during use in semiconductor manufacturing equipment, the sealing composition preferably does not contain metallic fillers. When the sealing composition contains carbon black, the carbon black content relative to 100 parts by weight of the fluoroelastomer can be, for example, 1 to 30 parts by weight.

[0051] When the filler contains fluororesin, it can be included in the sealing composition, for example, as fluororesin particles. When the filler contains fluororesin, the content of the fluororesin-containing filler in the sealing composition can be, for example, 1 to 30 parts by weight relative to 100 parts by weight of the fluoroelastomer.

[0052] Fluoropolymers used as fillers containing fluoropolymers are resins with fluorine atoms within their molecules. Examples include polytetrafluoroethylene (PTFE), tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), tetrafluoroethylene-hexafluoropropylene copolymer (FEP), tetrafluoroethylene-ethylene copolymer (ETFE), polychlorotrifluoroethylene (PCTFE), chlorotrifluoroethylene-ethylene copolymer (ECTFE), polyvinylidene fluoride (PVDF), polyvinylidene fluoride (PVF), vinylidene fluoride-hexafluoropropylene copolymer (VDF-HFP copolymer), and vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene copolymer (VDF-HFP-TFE copolymer). A single fluoropolymer can be used, or two or more can be used in combination.

[0053] Among the above, from the viewpoint of preventing the resin from melting at high temperatures and damaging properties such as compression set, it is preferable to use fluoropolymers with relatively high melting points such as PFA and PTFE.

[0054] Fluoropolymers used as fillers can also be substances containing functional groups. Functional groups can be introduced, for example, by copolymerizing monomers containing such functional groups. When the monomers containing the aforementioned crosslinking sites are copolymerized, crosslinking of the fluoropolymer and the perfluoroelastomer also occurs through the aforementioned crosslinking agent, thus further improving the mechanical strength of the crosslinked sealant composition. Examples of fluoropolymers containing functional groups include polytetrafluoroethylene containing nitrile groups, as described in Japanese Patent Application Publication No. 2013-177631. Furthermore, fluoropolymers can also be modified fluoropolymers such as "TFM-modified PTFE" (manufactured by DYNEON Corporation).

[0055] When the sealing composition contains a silicone polymer and a fluoropolymer filler, the compounding method of the silicone polymer and the fluoropolymer can be, for example, 1) a method of compounding the silicone polymer and the fluoropolymer using a mixing roller; 2) a method of melt compounding the silicone polymer and the fluoropolymer using a mixer, a twin-screw extruder or similar device.

[0056] When the sealing composition contains a filler, the content of the filler in the sealing composition (the total content in cases of two or more) may be, for example, 1 to 160 parts by mass relative to 100 parts by mass of the fluoroelastomer, preferably 1 to 100 parts by mass, and more preferably 1 to 80 parts by mass.

[0057] The sealing composition can be prepared by uniformly mixing fluoroelastomers, silicone polymers, crosslinking agents, and pigments, silica, etc., as needed. Existing known equipment such as mixing rollers, pressure kneaders, and internal mixers (Banbury mixers) can be used as the mixing machine. The components can be mixed in one step, or the components other than those participating in the crosslinking reaction (crosslinking accelerators, crosslinking delayers, crosslinking agents, etc.) can be pre-mixed uniformly, and then the components participating in the crosslinking reaction are mixed, i.e., mixing is carried out in multiple stages.

[0058] The seal of the present invention comprises a crosslinked product of the above-described sealing composition. The seal can be manufactured by crosslinking (vulcanizing) the seal with a rubber composition and molding. The crosslinking and molding methods can employ existing known methods such as injection molding, compression molding, and transfer molding.

[0059] The heating temperature during molding (primary crosslinking temperature) can be, for example, above 100°C and below 220°C, and the heating time (primary crosslinking time) can be, for example, above 0.5 minutes and below 120 minutes. Secondary crosslinking can also be performed after vulcanization molding. The secondary crosslinking temperature can be, for example, above 120°C and below 280°C, and the secondary crosslinking time can be, for example, above 0.5 hours and below 24 hours.

[0060] After primary or secondary crosslinking, further crosslinking can be achieved by irradiating the seal with radiation. Electron beams or gamma rays are preferred. The irradiation dose can be, for example, 20–120 kGy, preferably 40–60 kGy.

[0061] The 100% modulus (MPa) of the seal can be, for example, 1 to 12 MPa, preferably 2 to 5 MPa. By keeping the hardness of the seal within the above range, there is a tendency to improve the ease of installation into a semiconductor manufacturing device and to improve the sealing performance.

[0062] The hardness (type A hardness tester hardness) of the seal can be, for example, 54 or higher, preferably 60 to 90. By keeping the hardness of the seal within the above range, there is a tendency to improve the ease of installation into a semiconductor manufacturing device and to improve the sealing performance.

[0063] The tensile strength (MPa) of the seal can be, for example, 3 to 24 MPa, preferably 5 to 19 MPa.

[0064] The elongation (%) of the seal can be, for example, 100 to 400% or more, preferably 180 to 280, and more preferably 180 to 250.

[0065] The 100% modulus (MPa), hardness, tensile strength (MPa), and elongation (%) of the seal can be determined according to the methods described in the section of the embodiments described later.

[0066] Another aspect of the present invention is a seal comprising a crosslinked material of the above-described sealing composition. The seal of the present invention can be a seal for a semiconductor manufacturing apparatus, preferably a gate valve seal for a vacuum chamber in a semiconductor manufacturing apparatus, and particularly preferably a gate valve seal for a vacuum chamber in a semiconductor manufacturing apparatus undergoing plasma processing. Examples of seal applications include various types of seals such as rings, gaskets, and washers.

[0067] Another aspect of the present invention is a semiconductor manufacturing apparatus including the aforementioned sealing element. In addition to semiconductor manufacturing apparatuses, the semiconductor manufacturing apparatus of the present invention also includes, for example, liquid crystal panel manufacturing apparatuses, plasma panel manufacturing apparatuses, plasma display panel manufacturing apparatuses, plasma-addressable liquid crystal panel manufacturing apparatuses, organic EL panel manufacturing apparatuses, field emission display panel manufacturing apparatuses, solar cell substrate manufacturing apparatuses, semiconductor transport apparatuses, etc.

[0068] Example The present invention will be further described in detail below through examples. Unless otherwise specified, "%" and "parts" in the examples refer to mass percentage and mass parts.

[0069] <Examples 1-24, Comparative Examples 1-3, and Reference Examples 1-2> Prepare the sealing composition and then manufacture the seals in the following order. First, according to the formulations shown in Tables 1 to 5 (in which the amount of each formulation is in parts by mass), mix the specified amounts of each compounding agent using a two-roll mill.

[0070] Next, the obtained sealing composition was pressurized at 120°C for 20 minutes and then subjected to thermal secondary crosslinking at 200°C for 4 hours to obtain the sealing component.

[0071] It should be noted that in Example 11, the seal was radiocrosslinked by irradiating it with 40 kGy of gamma rays.

[0072] [Table 1] The details of the complexing components in Table 1 are as follows.

[0073] Fluoroelastic 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, manufactured by Daikin Industries, Ltd. "DAI-EL G-912" (Mounney viscosity at 121°C: 56).

[0074] Fluoroelastic 2: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, manufactured by Solvay Japan Co., Ltd., "TECNOFLON P459" (Mounney viscosity at 121°C: 24).

[0075] Organosilicon polymer 1: Fluorinated vinylmethyl polysiloxane, manufactured by Shin-Etsu Chemical Industry Co., Ltd., "FE-251-U".

[0076] Organosilicon polymer 2: Vinylmethyl polysiloxane, manufactured by Shin-Etsu Chemical Industry Co., Ltd., "KE-931-U".

[0077] Crosslinking agent 1: 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane, manufactured by Nippon Oil Co., Ltd. as "Perhexa25B".

[0078] Co-crosslinking agent: Triallyl isocyanurate (TAIC), manufactured by Mitsubishi Chemical Corporation.

[0079] [Table 2] The details of the complexing components in Table 2 are as follows.

[0080] Fluoroelastic 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, manufactured by Daikin Industries, Ltd. "DAI-EL G-912" (Mounney viscosity at 121°C: 56).

[0081] Organosilicon polymer 3: phenyl vinyl methyl polysiloxane, manufactured by Shin-Etsu Chemical Industry Co., Ltd., "KE-186-U".

[0082] Crosslinking agent 1: 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane, manufactured by Nippon Oil Co., Ltd. as "Perhexa25B".

[0083] Co-crosslinking agent: Triallyl isocyanurate (TAIC), manufactured by Mitsubishi Chemical Corporation.

[0084] [Table 3] The details of the complexing components in Table 3 are as follows.

[0085] Fluoroelastic 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, manufactured by Daikin Industries, Ltd. "DAI-EL G-912" (Mounney viscosity at 121°C: 56).

[0086] Organosilicon polymer 3: phenyl vinyl methyl polysiloxane, manufactured by Shin-Etsu Chemical Industry Co., Ltd., "KE-186-U".

[0087] Crosslinking agent 1: 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane, manufactured by Nippon Oil Co., Ltd. as "Perhexa25B".

[0088] Co-crosslinking agent: Triallyl isocyanurate (TAIC), manufactured by Mitsubishi Chemical Corporation.

[0089] PFPE1: A compoundable perfluoropolyether compound, manufactured by Shin-Etsu Chemical Co., Ltd., "X71-906".

[0090] PFPE2: A perfluoropolyether compound, manufactured by Shin-Etsu Chemical Co., Ltd. as "SIFEL8070A".

[0091] PFPE3: A perfluoropolyether compound, manufactured by Shin-Etsu Chemical Industry Co., Ltd. as "SIFEL8070B".

[0092] PFPE4: A gel-like perfluoropolyether compound (a reactant of "SIFEL8070A" and "SIFEL8070B" manufactured by Shin-Etsu Chemical Industry Co., Ltd.).

[0093] [Table 4] The details of the complexing components in Table 4 are as follows.

[0094] Fluoroelastic 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, manufactured by Daikin Industries, Ltd. "DAI-EL G-912" (Mounney viscosity at 121°C: 56).

[0095] Organosilicon polymer 3: phenyl vinyl methyl polysiloxane, manufactured by Shin-Etsu Chemical Industry Co., Ltd., "KE-186-U".

[0096] Crosslinking agent 1: 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane, manufactured by Nippon Oil Co., Ltd. as "Perhexa25B".

[0097] Co-crosslinking agent: Triallyl isocyanurate (TAIC), manufactured by Mitsubishi Chemical Corporation.

[0098] PFPE4: A gel-like perfluoropolyether compound (a reactant of "SIFEL8070A" and "SIFEL8070B" manufactured by Shin-Etsu Chemical Industry Co., Ltd.).

[0099] Filler 1: Silica (SiO2), manufactured by AEROSIL Corporation of Japan, "AEROSIL RX200".

[0100] Filler 2: Fluoropolymer particles (PTFE), manufactured by Daikin Industries, Ltd., "Lubron L-5".

[0101] [Table 5] The details of the complexing components in Table 5 are as follows.

[0102] Fluoroelastic 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, manufactured by Daikin Industries, Ltd. "DAI-EL G-912" (Mounney viscosity at 121°C: 56).

[0103] Fluoroelastic 2: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, manufactured by Solvay Japan Co., Ltd., "TECNOFLON P459" (Mounney viscosity at 121°C: 24).

[0104] Organosilicon polymer 2: Vinylmethyl polysiloxane, manufactured by Shin-Etsu Chemical Industry Co., Ltd., "KE-931-U".

[0105] Organosilicon polymer 3: phenyl vinyl methyl polysiloxane, manufactured by Shin-Etsu Chemical Industry Co., Ltd., "KE-186-U".

[0106] Crosslinking agent 1: 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane, manufactured by Nippon Oil Co., Ltd. as "Perhexa25B".

[0107] Crosslinking agent 2: 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane, manufactured by Shin-Etsu Chemical Industry Co., Ltd., "C-8".

[0108] Crosslinking agent 3: p-Toluyl peroxide, manufactured by Shin-Etsu Chemical Industry Co., Ltd., "C-23".

[0109] Co-crosslinking agent: Triallyl isocyanurate (TAIC), manufactured by Mitsubishi Chemical Corporation.

[0110] PFPE4: A gel-like perfluoropolyether compound (a reactant of "SIFEL8070A" and "SIFEL8070B" manufactured by Shin-Etsu Chemical Industry Co., Ltd.).

[0111] (Evaluation of seals) The obtained cross-linked molded articles (sealants) were evaluated as follows. The results are shown in Tables 1 to 6.

[0112] [1] Determination of normal physical properties.

[0113] Hardness (Type A hardness tester hardness) was determined according to JIS K6253:2012 using a Type A hardness tester. Tensile testing was conducted according to JIS K 6251, with a specimen shape of No. 3 dumbbell, using a Schubert tensile testing machine to determine tensile strength (MPa), elongation (%), and 100% modulus (MPa).

[0114] As shown in Tables 1-5, the 100% increase in modulus was confirmed in Examples 1-24 compared to Comparative Examples 1-3.

Claims

1. A sealing composition comprising a fluoroelastomer, a vinyl-based silicone polymer, and a crosslinking agent.

2. The sealing composition according to claim 1, wherein, The organosilicon polymer comprises at least one selected from the group consisting of vinylmethyl polysiloxane, fluorovinylmethyl polysiloxane, and phenylvinylmethyl polysiloxane.

3. The sealing composition according to claim 1 or 2, wherein, The content of the organosilicon polymer is more than 1 part by mass and less than 500 parts by mass relative to 100 parts by mass of the fluoroelastomer.

4. The sealing composition according to any one of claims 1 to 3, wherein, The crosslinking agent comprises at least one selected from the group consisting of peroxide compounds, polyol compounds, and polyamine compounds.

5. The sealing composition according to any one of claims 1 to 4, wherein, The content of the crosslinking agent is 1 to 6 parts by mass relative to 100 parts by mass of the fluoroelastomer.

6. The sealing composition according to any one of claims 1 to 5, wherein, It further includes perfluoropolyether compounds.

7. The sealing composition according to claim 6, wherein, The content of the perfluoropolyether compound is 0.5 to 30 parts by weight relative to 100 parts by weight of the fluoroelastomer.

8. The sealing composition according to any one of claims 1 to 7, wherein, It further comprises: a filler in the form of 1 to 30 parts by weight relative to 100 parts by weight of the fluoroelastomer.

9. The sealing composition according to claim 8, wherein, The filler contains silicon dioxide.

10. The sealing composition according to claim 8, wherein, The filler comprises a fluoropolymer, which comprises polytetrafluoroethylene.

11. A seal comprising a crosslinked compound of the seal composition as described in any one of claims 1 to 10.

12. A gate valve seal for a semiconductor manufacturing apparatus, comprising the seal as claimed in claim 11.

13. A semiconductor manufacturing apparatus comprising the seal as claimed in claim 11.

Images