Sealing material composition and sealing material
The sealing material composition, featuring a fluoroelastomer, silicone polymer, and crosslinking agent, addresses the issue of insufficient 100% modulus in sealants, resulting in enhanced performance for semiconductor manufacturing equipment.
Patent Information
- Application Number
- JP2023192368
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2023-11-10
- Publication Date
- 2025-05-22
AI Technical Summary
Sealants containing crosslinked fluoroelastomers often have insufficient 100% modulus, which can affect their performance in dynamic sealing applications.
A sealing material composition comprising a fluoroelastomer, a silicone polymer with a vinyl group, and a crosslinking agent, with specific ratios and types of components to enhance the 100% modulus.
The composition achieves improved 100% modulus, elongation, and tensile strength, making it suitable for use in gate seals for semiconductor manufacturing equipment.
Smart Images

Figure 2025079590000001 
Figure 2025079590000002 
Figure 2025079590000003
Abstract
Description
[Technical field]
[0001] The present invention relates to a sealing material composition, and further relates to a sealing material, sealing materials in general including a gate seal for semiconductor manufacturing equipment containing the same, and semiconductor manufacturing equipment. [Background technology]
[0002] Patent Document 1 proposes a composition containing a crosslinkable fluorine-containing elastomer as a composition used for producing a sealing material. [Prior art documents] [Patent documents]
[0003] [Patent Document 1] JP 2000-119468 A Summary of the Invention [Problem to be solved by the invention]
[0004] However, when a sealant containing a crosslinked product of a composition containing a fluoroelastomer is used as a dynamic sealant, the 100% modulus may not be sufficient.
[0005] An object of the present invention is to provide a sealing material composition capable of exhibiting an improved 100% modulus, a sealing material containing a crosslinked product thereof, a gate seal for semiconductor manufacturing equipment, and semiconductor manufacturing equipment. [Means for solving the problem]
[0006] The present invention provides the following sealing material composition, sealing material, gate seal for semiconductor manufacturing equipment, and semiconductor manufacturing equipment. [1] A sealant composition comprising a fluoroelastomer, a silicone polymer having a vinyl group, and a crosslinking agent. [2] The sealing material composition according to [1], wherein the silicone polymer comprises at least one selected from the group consisting of vinyl methyl silicone, fluorovinyl methyl silicone, and phenyl vinyl methyl silicone. [3] The sealing material composition according to [1] or [2], wherein the content of the silicone polymer is 1 part by mass or more and 500 parts by mass or less per 100 parts by mass of the fluoroelastomer. [4] The sealing material composition according to any one of [1] to [3], wherein the crosslinking agent includes at least one selected from the group consisting of peroxide-based compounds, polyol-based compounds, and polyamine-based compounds. [5] The sealing material composition according to any one of [1] to [4], wherein the content of the crosslinking agent is 1 to 6 parts by mass based on 100 parts by mass of the fluoroelastomer. [6] The sealing material composition according to any one of [1] to [5], further comprising a perfluoropolyether compound. [7] The sealing material composition according to [6], wherein the content of the perfluoropolyether compound is 0.5 to 30 parts by mass based on 100 parts by mass of the fluoroelastomer. [8] The sealing material composition according to any one of [1] to [7], further comprising 1 to 30 parts by mass of a filler relative to 100 parts by mass of the fluoroelastomer. [9] The sealant composition according to [8], wherein the filler contains silica.
[10] The sealing material composition according to [8], wherein the filler contains a fluororesin, and the fluororesin contains polytetrafluoroethylene.
[11] A sealant comprising a crosslinked product of the sealant composition according to any one of [1] to
[10] .
[12] A gate seal for semiconductor manufacturing equipment, comprising the sealing material according to
[11] .
[13] A semiconductor manufacturing device comprising the sealing material according to
[11] . Effect of the Invention
[0007] The present invention provides a sealing material composition capable of exhibiting an improved 100% modulus, a sealing material containing the crosslinked product thereof, a gate seal for semiconductor manufacturing equipment, and semiconductor manufacturing equipment. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0008] Hereinafter, an embodiment of the present invention will be described, however, the present invention is not limited to the following embodiment.
[0009] <Sealing material composition> A sealant composition according to one embodiment of the present invention is a sealant composition for producing a sealant for semiconductor manufacturing equipment. The sealant composition contains a fluorine elastomer, a silicone polymer having a vinyl group (hereinafter also referred to as vinyl silicone), and a crosslinking agent.
[0010] (Fluoroelastomer) A fluoroelastomer is a crosslinkable rubber component capable of forming an elastomer (crosslinked rubber) having a crosslinked structure by a crosslinking reaction, and is made of a polymer or copolymer having at least one constituent unit that is a monomer containing hydrogen atoms or that contains hydrogen atoms and fluorine atoms, or a fluorothermoplastic elastomer containing hydrogen atoms. Crosslinked rubber is a rubber that exhibits rubber elasticity by causing a crosslinking reaction between molecular chains of a crosslinkable rubber component (fluoroelastomer) using a crosslinking agent or the like to give it a crosslinked structure.
[0011] Specific examples of fluorine elastomers 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)-perfluoromethylvinylether (PMVE) copolymers; vinylidene fluoride (VDF)-tetrafluoroethylene (TFE)-perfluoromethylvinylether (PMVE) copolymers, vinylidene fluoride (VDF)-perfluoromethylvinylether (PMVE) copolymers, etc. Only one type of fluorine elastomer may be used, or two or more types may be used in combination.
[0012] The Mooney viscosity of the fluoroelastomer at a temperature of 121° C. may be, for example, not less than 20. From the viewpoint of ensuring that the 100% modulus, elongation and tensile strength of the resulting sealing material are all good, the Mooney viscosity of the fluoroelastomer at a temperature of 121° C. is preferably not less than 25, more preferably not less than 40, and even more preferably not less than 56. The Mooney viscosity can be measured in accordance with JIS K6300-1:2013.
[0013] The fluorine-based thermoplastic elastomer containing hydrogen atoms is not particularly limited, and examples thereof that can be used include "Daiel Thermoplastic" (manufactured by Daikin Industries, Ltd.) and "Cefral Soft" (manufactured by Central Glass Co., Ltd.), both of which are trade names.
[0014] (Silicone polymer having vinyl groups) The vinyl silicone may be a polymer or copolymer made of a structural unit derived from a siloxane compound. The vinyl silicone may have a vinyl group at least one of the terminal of the main chain and the side chain, or may have a vinyl group at all of the terminal of the main chain and the side chain. The vinyl silicone may have a ratio of vinyl groups in the terminal groups and the side chains bonded to silicon atoms of, for example, 0.01 to 15 mol%. The vinyl silicone may be modified with, for example, a halogen element, and may have an aromatic monovalent hydrocarbon group. The polymerization degree of the vinyl silicone may be, for example, 100 or more, preferably 1000 or more, more preferably 2000 or more, and even more preferably 3000 or more. The polymerization degree of the vinyl silicone may be, for example, 10000 or less. The polymerization degree can be determined, for example, as a number average polymerization degree in terms of polystyrene in gel permeation chromatography (GPC) analysis using toluene or the like as a developing solvent.
[0015] Vinyl silicone has the following formula (1): [ka] [In the formula, R 1 each independently represents a substituted or unsubstituted aromatic monovalent hydrocarbon group, a substituted or unsubstituted unsaturated or saturated hydrocarbon group not containing an aromatic hydrocarbon group, an alkoxy group, a hydroxy group, or a hydrogen atom. The vinyl silicone can contain one type or two or more types of the first constitutional unit.
[0016] Examples of the unsubstituted aromatic monovalent hydrocarbon group include aryl groups such as phenyl group and tolyl group, and aralkyl groups such as benzyl group and phenylethyl group. Examples of the substituted unsubstituted aromatic monovalent hydrocarbon group include groups in which some or all of the hydrogen atoms of the groups exemplified as the unsubstituted aromatic monovalent hydrocarbon groups above are substituted with halogen atoms such as fluorine and chlorine, and examples of the substituted unsubstituted aromatic monovalent hydrocarbon group include chlorophenyl group.
[0017] Examples of the unsubstituted saturated hydrocarbon group that does not contain an aromatic hydrocarbon group include alkyl groups such as methyl group, ethyl group, propyl group, isopropyl group, butyl group, isobutyl group, tert-butyl group, pentyl group, hexyl group, cyclohexyl group, octyl group, decyl group, dodecyl group, etc. Examples of the unsubstituted unsaturated hydrocarbon group that does not contain an aromatic hydrocarbon group include alkenyl groups such as vinyl group, allyl group, propenyl group, isopropenyl group, butenyl group, isobutenyl group, etc. Examples of the substituted unsaturated or saturated hydrocarbon group that does not contain an aromatic hydrocarbon group may be a group in which some or all of the hydrogen atoms of the groups exemplified as the unsubstituted unsaturated or saturated hydrocarbon group that does not contain an aromatic hydrocarbon group are substituted with halogen atoms such as fluorine and chlorine, and examples thereof include chloromethyl group, 3,3,3-trifluoropropyl group, etc.
[0018] Examples of the alkoxy group include methoxy group, ethoxy group, propoxy group, butoxy group, etc.
[0019] Vinyl silicone is represented by the following formula (2):
Chemical formula
[0020] R 2 and R 3As examples of the unsubstituted or substituted aromatic monovalent hydrocarbon group, the unsubstituted or substituted unsaturated or saturated hydrocarbon group not containing an aromatic hydrocarbon group, and the alkoxy group in the above, the examples except for the vinyl group are applicable.
[0021] Vinyl silicone has a main chain end with (R 4 ) 3 Si-R 5 -[wherein, R 4 each independently represents an unsubstituted or substituted aromatic monovalent hydrocarbon group, an unsubstituted or substituted unsaturated or saturated hydrocarbon group not containing an aromatic hydrocarbon group, an alkoxy group, or a hydroxy group; R 5 R independently represents an oxygen atom or an alkylene group having 1 to 5 carbon atoms (hereinafter also referred to as a terminal group). 4 The above-mentioned examples are applicable to the unsubstituted or substituted aromatic monovalent hydrocarbon group, the unsubstituted or substituted unsaturated or saturated hydrocarbon group not containing an aromatic hydrocarbon group, and the alkoxy group in R. 4 Examples of the alkylene group having 1 to 5 carbon atoms in R include a methylene group, an ethylene group, and a propylene group. 4 R is preferably a methyl group, a methoxy group, or a hydroxy group. 5 is preferably an oxygen atom or an ethylene group. When the vinyl silicone has a vinyl group at the end of the main chain, at least one of R4 is a vinyl group.
[0022] The vinyl silicone is preferably a compound represented by the following formula (3): [ka] [In the formula, R 1 , R 2 , R 3 , R 4 and R 5 is defined as above, n and o each independently represent an integer of 1 or more. The sum of n and o may 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 may be, for example, 10000 or less.
[0023] As the vinyl silicone, a compound represented by the following formula (4): [ka] [In the formula, R 4 ' each independently represents an unsubstituted or substituted unsaturated or saturated hydrocarbon group not containing an aromatic hydrocarbon group, an alkoxy group or a hydroxy group; p and q each independently represent an integer of 1 or more. A compound represented by the following formula (5): [ka] [In the formula, R 4 '' each independently represent an unsubstituted or substituted unsaturated or saturated hydrocarbon group not containing an aromatic hydrocarbon group, an alkoxy group, or a hydroxy group; r, s and t each independently represent an integer of 1 or more. A compound represented by the following formula (6): [ka] [In the formula, R 4 is defined as above, u, v and w each independently represent an integer of 1 or more. In formula (4), R 4 The unsubstituted unsaturated or saturated hydrocarbon group, alkoxy group, and hydroxy group not including an aromatic hydrocarbon group in ' are defined as R 4 The definition of R applies. 4The unsubstituted or substituted unsaturated or saturated hydrocarbon group, alkoxy group, and hydroxy group not including an aromatic hydrocarbon group in R 4 The definitions for p and q in formula (4), r, s and t in formula (5), and u, v and w in formula (6) may each 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 formula (4), the sum of r, s and t in formula (5), and the sum of u, v and w in formula (6) may each be, for example, 10000 or less.
[0024] The vinyl silicone may be a polymer or copolymer containing the first constitutional unit. The vinyl silicone can be obtained, for example, by polymerizing a polymerizable component containing the first constitutional unit. Alternatively, the vinyl silicone can be obtained by copolymerizing a copolymerizable component containing the first constitutional unit with another copolymerizable component (for example, a copolymerizable component containing the second constitutional unit, etc.). For example, the compound represented by formula (6) can be obtained by copolymerizing a dimethylsiloxane-based copolymerization component, a diphenylsiloxane-based copolymerization component, and a methylvinylsiloxane-based copolymerization component.
[0025] The vinyl silicone preferably includes at least one selected from the group consisting of vinyl methyl silicone, fluorovinyl methyl silicone, and phenyl vinyl methyl silicone. Examples of vinyl methyl silicone include compounds represented by formula (4). Examples of fluorovinyl methyl silicone include compounds represented by formula (5). Examples of phenyl vinyl methyl silicone include compounds represented by formula (6). These vinyl silicones can also be used in the form of silicone rubber compounds filled with silica, as described below. Examples of commercially available products include "KE-186-U", "KE-183-U", "KE-136Y-U", and "SE-955-U" manufactured by Dow Toray Co., Ltd.
[0026] The sealant composition may contain one or more silicone polymers having a vinyl group. The sealant composition may also contain other polysiloxane compounds other than the silicone polymer having a vinyl group, such as dimethyl silicone. It is preferable that all silicone polymers contained in the sealant composition are silicone polymers having a vinyl group. In addition, the sealant composition may also be used as a blend rubber with other rubbers within a range that does not impede the object of the present invention.
[0027] The content of the silicone polymer is, for example, 1 part by mass or more and 500 parts by mass or less per 100 parts by mass of the fluoroelastomer. When the content of the silicone polymer is within the above range, the 100% modulus of the resulting sealing material tends to be improved. 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. Moreover, from the viewpoint of achieving both 100% modulus and elongation of the resulting sealing material, 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.
[0028] (Crosslinking agent) As the crosslinking agent, for example, at least one selected from the group consisting of peroxide-based compounds, polyol-based compounds, and polyamine-based compounds can be used. The peroxide-based compound is not particularly limited as long as it can be used for silicone polymers, and examples thereof 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(benzoylperoxy)hexane, tert-butylperoxybenzoate, tert-butylperoxyisopropylcarbonate, and n-butyl-4,4-di(tert-butylperoxy)valerate. The vulcanizing agent can contain one or more peroxide-based compounds.
[0029] Examples of the polyol compound 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'-dihydroxydiphenyl, 4,4'-dihydroxystilbene, 2,6-dihydroxyanthracene, hydroquinone, catechol, 2,2-bis(4-hydroxyphenyl)butane (bisphenol B), 4,4-bis(4-hydroxyphenyl)valeric acid, 2,2-bis(4-hydroxyphenyl)tetrafluorodichloropropane, 4,4-dihydroxydiphenyl sulfone, 4,4'-dihydroxydiphenyl ketone, tri(4-hydroxyphenyl)methane, 3,3',5,5'-tetrachlorobisphenol A, 3,3',5,5'-tetrabromobisphenol A, and the like. These polyhydroxy aromatic compounds may be alkali metal salts, alkaline earth metal salts, or the like. The crosslinking agent can contain one or more polyol compounds.
[0030] Examples of the polyamine compound include hexamethylenediamine carbamate, N,N'-dicinnylidene-1,6-hexamethylenediamine, and 4,4'-bis(aminocyclohexyl)methane carbamate. Among these, from the viewpoints of the crosslinkability of the thermoplastic fluororesin (A) and the physical properties of the resulting crosslinked product, particularly the compression set characteristics, examples of the polyamine compound (b-2) include N,N'-dicinnylidene-1,6-hexamethylenediamine. The crosslinking agent can contain one or more polyamine compounds.
[0031] The content of the crosslinking agent in the sealant composition may be, for example, 0.5 to 6 parts by mass, preferably 1.5 to 4 parts by mass, more preferably 2 to 4 parts by mass, based on 100 parts by mass of the fluororubber.
[0032] (Perfluoropolyether-based compound) The sealing material composition may further contain a perfluoropolyether compound. The perfluoropolyether compound may be a low molecular weight compound such as an oligomer, or a high molecular weight compound such as a polymer. Among them, from the viewpoint of 100% modulus and plasma resistance, a perfluoropolyether polymer is preferably contained. The perfluoropolyether polymer may have, for example, a group capable of crosslinking with a silicone polymer at the end of the main chain. Commercially available perfluoropolyether polymers may be used. Examples of commercially available perfluoropolyether polymers include SIFEL8070A / B and X71-906 (both manufactured by Shin-Etsu Chemical Co., Ltd.). The content of the perfluoropolyether compound in the sealing material composition may be, for example, 0.5 to 30 parts by mass, preferably 1 to 25 parts by mass, more preferably 2 to 20 parts by mass, relative to 100 parts by mass of the fluoroelastomer.
[0033] (Other ingredients) The sealing material composition may contain other components than the above components, such as additives such as pigments, fillers, antioxidants, antioxidants, vulcanization accelerators, processing aids (stearic acid, etc.), stabilizers, tackifiers, silane coupling agents, plasticizers, flame retardants, mold release agents, waxes, and lubricants. Another example of the additive is a tackiness reducing (preventing) agent such as fluorine-based oil (e.g., perfluoroether, etc.). Only one type of additive may be used, or two or more types may be used in combination.
[0034] Examples of the pigment include at least one selected from the group consisting of inorganic pigments and organic pigments. Examples of the inorganic pigment include white pigments (e.g., silica, zinc oxide, white lead, lithopone, titanium dioxide, precipitated barium sulfate, baryte powder, etc.), red pigments (e.g., red lead, red iron oxide, etc.), yellow pigments (e.g., yellow lead, zinc yellow, etc.), blue pigments (e.g., ultramarine blue, Prussian blue, YInMn blue, etc.), and black pigments (e.g., carbon black, etc.). Examples of the organic pigment include azo pigments (azo lake pigments, insoluble azo pigments, condensed azo pigments, etc.); anthraquinone pigments, thioindigo pigments, perinone pigments, perylene pigments, quinacridone pigments, isoindolinone pigments, isoindoline pigments, dioxazine pigments, quinophthalone pigments, polycyclic pigments such as diketopyrrolopyrrole pigments, phthalocyanine pigments, etc. As the organic pigment, an organic pigment classified as a pigment in the Color Index can be used. The pigment preferably used is an organic pigment that does not contain a metal element. The organic pigment that does not contain a metal element does not cause substances derived from metal elements to scatter even if the sealing material is used in a severe ozone environment such as for semiconductor applications and the annular sealing material is etched. When the sealing material composition contains a pigment, the content of the pigment in the sealing material composition may be, for example, 0.05 to 3 parts by mass per 100 parts by mass of the fluoroelastomer.
[0035] Examples of the filler 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, alumina, magnesium carbonate, calcium carbonate, zinc carbonate, carbon black, granular or powdered resin (such as fluororesin), metal powder, glass powder, ceramic powder, etc. When the sealing material composition contains a filler, it is advantageous from the viewpoint of improving the mechanical strength of the sealing material. The filler is preferably at least one selected from the group consisting of silica, carbon black, and fluororesin. From the viewpoint of 100% modulus and plasma resistance, the filler preferably contains silica and fluororesin.
[0036] Examples of silica include fumed silica, precipitated silica, and fused silica. When the sealing material composition contains silica, the content of silica in the sealing material composition may be, for example, 6 to 120 parts by mass per 100 parts by mass of fluoroelastomer. When the sealing material composition contains silica, a silicone rubber compound in which silica is blended with a silicone polymer can be used. As the silicone rubber compound, "KE-186-U" manufactured by Shin-Etsu Chemical Co., Ltd., "SE-955-U" manufactured by Dow Toray Co., Ltd., and the like can be used as they are. In addition, the silicone rubber compound can also be used as a blend rubber with other rubbers within a range that does not impede the object of the present invention.
[0037] Examples of carbon black include MT carbon. The sealing material composition preferably does not contain a metal-based filler from the viewpoint of filler scattering during use in semiconductor manufacturing equipment. When the sealing material composition contains carbon black, the content of carbon black in the sealing material composition may be, for example, 1 to 30 parts by mass per 100 parts by mass of the fluoroelastomer.
[0038] When the filler contains a fluororesin, it can be contained in the sealing material composition as, for example, fluororesin particles. When the filler contains a fluororesin, the content of the filler containing the fluororesin in the sealing material composition may be, for example, 1 to 30 parts by mass per 100 parts by mass of the fluoroelastomer.
[0039] The fluororesin used in the filler containing a fluororesin is a resin having fluorine atoms in the molecule. For example, 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), polyvinyl fluoride (PVF), vinylidene fluoride-hexafluoropropylene copolymer (VDF-HFP copolymer), vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene copolymer (VDF-HFP-TFE copolymer), etc. can be used. The fluororesin may be used alone or in combination of two or more.
[0040] Among the above, from the viewpoint of preventing the resin from melting and impairing properties such as compression set under a high-temperature environment, it is preferable to use a fluororesin having a relatively high melting point such as PFA and PTFE.
[0041] The fluororesin used in the filler may contain a functional group. The functional group can be introduced, for example, by copolymerizing a monomer having the functional group. When the above-mentioned crosslinking site monomer is copolymerized as the monomer having the functional group, the crosslinking between the fluororesin and the perfluoroelastomer also proceeds by the above crosslinking agent, so that the mechanical strength of the crosslinked product of the sealant composition can be further increased. As an example of the fluororesin containing a functional group, nitrile group-containing polytetrafluoroethylene described in JP-A-2013-177631 can be cited. Further, the fluororesin can also be a modified fluororesin such as "TFM-modified PTFE" (manufactured by Dynion).
[0042] When the sealing material composition contains a silicone polymer and a fluororesin filler, the silicone polymer and the fluororesin can be kneaded together by, for example, 1) kneading the silicone polymer and the fluororesin using a mixing roll, or 2) melt-kneading the silicone polymer and the fluororesin using an apparatus such as a mixer or a twin-screw extruder.
[0043] When the sealing material composition contains a filler, the content of the filler in the sealing material composition (the total content when two or more types are contained) may be, for example, 1 to 160 parts by mass, preferably 1 to 100 parts by mass, and more preferably 1 to 80 parts by mass, per 100 parts by mass of the fluoroelastomer.
[0044] The sealing material composition can be prepared by uniformly kneading the fluorine elastomer, the silicone polymer, the crosslinking agent, and the pigment, silica, etc., which are added as necessary. As the kneading machine, for example, a conventionally known one such as a mixing roll, a pressure kneader, an internal mixer (Banbury mixer), etc. can be used. The components may be mixed and kneaded at once, or may be kneaded in multiple stages, such as by first uniformly kneading the components among the components except for the components that contribute to the crosslinking reaction (crosslinking accelerator, crosslinking retarder, crosslinking agent, etc.), and then kneading the components that contribute to the crosslinking reaction.
[0045] The sealant of the present invention includes a crosslinked product of the above-mentioned sealant composition. The sealant can be produced by crosslinking (vulcanizing) and molding the rubber composition for sealants. The crosslinking and molding methods can be any conventional method such as injection molding, compression molding, and transfer molding.
[0046] The heating temperature (primary crosslinking temperature) during molding may be, for example, 100°C or higher and 220°C or lower, and the heating time (primary crosslinking time) may be, for example, 0.5 minutes or higher and 120 minutes or lower. After vulcanization molding, secondary crosslinking may be performed. The secondary crosslinking temperature may be, for example, 120°C or higher and 280°C or lower, and the secondary crosslinking time may be, for example, 0.5 hours or higher and 24 hours or lower.
[0047] After the primary crosslinking or secondary crosslinking, the sealing material may be irradiated with radiation to further crosslink it. The radiation may be an electron beam or a gamma ray. The radiation dose may be, for example, 20 to 120 KGy, and preferably 40 to 60 KGy.
[0048] The 100% modulus (MPa) of the sealant may be, for example, 1 to 12 MPa, and preferably 2 to 5 MPa. When the hardness of the sealant is within the above range, the sealant is more easily attached to semiconductor manufacturing equipment, and the sealability tends to be improved.
[0049] The hardness (type A durometer hardness) of the sealing material may be, for example, 54 or more, and preferably 60 to 90. When the hardness of the sealing material is within the above range, the ease of mounting on semiconductor manufacturing equipment is improved, and the sealing performance tends to be improved.
[0050] The tensile strength (MPa) of the sealing material may be, for example, 3 to 24 MPa, and is preferably 5 to 19 MPa.
[0051] The elongation (%) of the sealing material may be, for example, 100 to 400% or more, preferably 180 to 280, and more preferably 180 to 250.
[0052] The 100% modulus (MPa), hardness, tensile strength (MPa) and elongation (%) of the sealing material can be measured according to the method described in the Examples section below.
[0053] Another aspect of the present invention is a sealant containing a crosslinked product of the above-mentioned sealant composition. The sealant of the present invention may be a sealant for semiconductor manufacturing equipment, and is suitable as a gate seal for a vacuum chamber in the semiconductor manufacturing equipment, particularly suitable as a gate seal for a vacuum chamber in a semiconductor manufacturing equipment in which plasma processing is performed. Examples of the use form of the sealant include various sealants such as rings, packings, and gaskets.
[0054] Another aspect of the present invention is a semiconductor manufacturing apparatus including the above-mentioned sealant. The semiconductor manufacturing apparatus of the present invention includes, in addition to semiconductor manufacturing apparatus, for example, liquid crystal panel manufacturing apparatus, plasma panel manufacturing apparatus, plasma display panel manufacturing apparatus, plasma addressed liquid crystal panel manufacturing apparatus, organic EL panel manufacturing apparatus, field emission display panel manufacturing apparatus, solar cell substrate manufacturing apparatus, semiconductor conveying apparatus, and the like. EXAMPLES
[0055] The present invention will be described in more detail below with reference to examples. In the examples, "%" and "parts" are by mass % and parts by mass unless otherwise specified.
[0056] <Examples 1 to 24, Comparative Examples 1 to 3, and Reference Examples 1 to 2> A sealing material composition was prepared and then a sealing material was produced according to the following procedure: First, a predetermined amount of each compounding ingredient was kneaded with an open roll according to the compounding compositions shown in Tables 1 to 5 (the units of compounding amounts in the tables are parts by mass). Next, the obtained sealing material composition was press-molded under conditions of 120° C. for 20 minutes, and then subjected to secondary crosslinking by heat under conditions of 200° C. for 4 hours to obtain a sealing material. In Example 11, the sealing material was irradiated with gamma rays at 40 KGy to carry out radiation crosslinking.
[0057] [Table 1]
[0058] Details of the ingredients in Table 1 are as follows: Fluorine elastomer 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, Daikin Industries, Ltd. "Daiel G-912" (Mooney viscosity at 121°C: 56) Fluorine elastomer 2: vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, "Technoflon P459" manufactured by Solvay Japan Co., Ltd. (Mooney viscosity at 121°C: 24) Silicone polymer 1: Fluorovinylmethylsilicone, "FE-251-U" manufactured by Shin-Etsu Chemical Co., Ltd. Silicone polymer 2: Vinyl methyl silicone, "KE-931-U" manufactured by Shin-Etsu Chemical Co., Ltd. Crosslinking agent 1: 2,5-dimethyl-2,5-di(t-butylperoxy)hexane, NOF Corporation "Perhexa 25B" Co-crosslinking agent: Triallyl isocyanurate (TAIC), "TAIC" manufactured by Mitsubishi Chemical Corporation
[0059] [Table 2]
[0060] Details of the ingredients in Table 2 are as follows: Fluorine elastomer 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, Daikin Industries, Ltd. "Daiel G-912" (Mooney viscosity at 121°C: 56) Silicone polymer 3: Phenylvinylmethylsilicone, "KE-186-U" manufactured by Shin-Etsu Chemical Co., Ltd. Crosslinking agent 1: 2,5-dimethyl-2,5-di(t-butylperoxy)hexane, NOF Corporation "Perhexa 25B" Co-crosslinking agent: Triallyl isocyanurate (TAIC), "TAIC" manufactured by Mitsubishi Chemical Corporation
[0061] [Table 3]
[0062] Details of the ingredients in Table 3 are as follows: Fluororubber 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, "Dai-el G-912" manufactured by Daikin Industries, Ltd. (Mooney viscosity at 121°C: 56) Silicone polymer 3: Phenylvinylmethyl silicone, "KE-186-U" manufactured by Shin-Etsu Chemical Co., Ltd. Crosslinking agent 1: 2,5-Dimethyl-2,5-di(t-butylperoxy)hexane, "Perhexa 25B" manufactured by NOF Corporation Co-crosslinking agent: Triallyl isocyanurate (TAIC), "TAC" manufactured by Mitsubishi Chemical Corporation PFPE1: Mirabelle-type perfluoropolyether-based compound, "X71-906" manufactured by Shin-Etsu Chemical Co., Ltd. PFPE2: Perfluoropolyether-based compound, "SIFEL8070A" manufactured by Shin-Etsu Chemical Co., Ltd. PFPE3: Perfluoropolyether-based compound, "SIFEL8070B" manufactured by Shin-Etsu Chemical Co., Ltd. PFPE4: Gel-like perfluoropolyether-based compound (reaction product of "SIFEL8070A" and "SIFEL8070B" manufactured by Shin-Etsu Chemical Co., Ltd.)
[0063]
Table 4
[0064] Details of the compounding ingredients in Table 4 are as follows. Fluororubber 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, "Dai-el G-912" manufactured by Daikin Industries, Ltd. (Mooney viscosity at 121°C: 56) Silicone polymer 3: Phenylvinylmethyl silicone, "KE-186-U" manufactured by Shin-Etsu Chemical Co., Ltd. Crosslinking agent 1: 2,5-Dimethyl-2,5-di(t-butylperoxy)hexane, "Perhexa 25B" manufactured by NOF Corporation Co-crosslinking agent: Triallyl isocyanurate (TAIC), "TAIC" manufactured by Mitsubishi Chemical Corporation PFPE4: Gel-like perfluoropolyether compound (a reaction product of "SIFEL8070A" and "SIFEL8070B" manufactured by Shin-Etsu Chemical Co., Ltd.) Filler 1: Silica (SiO 2 ), "Aerosil RX200" manufactured by Nippon Aerosil Co., Ltd. Filler 2: Fluorine resin particles (PTFE), "Lubron L-5" manufactured by Daikin Industries, Ltd.
[0065] [Table 5]
[0066] Details of the ingredients in Table 5 are as follows: Fluorine elastomer 1: Vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, Daikin Industries, Ltd. "Daiel G-912" (Mooney viscosity at 121°C: 56) Fluorine elastomer 2: vinylidene fluoride (VDF)-hexafluoropropylene (HFP)-tetrafluoroethylene (TFE) copolymer, "Technoflon P459" manufactured by Solvay Japan Co., Ltd. (Mooney viscosity at 121°C: 24) Silicone polymer 2: Vinyl methyl silicone, "KE-931-U" manufactured by Shin-Etsu Chemical Co., Ltd. Silicone polymer 3: Phenylvinylmethylsilicone, "KE-186-U" manufactured by Shin-Etsu Chemical Co., Ltd. Crosslinking agent 1: 2,5-dimethyl-2,5-di(t-butylperoxy)hexane, NOF Corporation "Perhexa 25B" Crosslinker 2: 2,5-dimethyl-2,5-bis(t-butylperoxy)hexane, "C-8" manufactured by Shin-Etsu Chemical Co., Ltd. Crosslinker 3: Paramethylbenzoyl peroxide, "C-23" manufactured by Shin-Etsu Chemical Co., Ltd. Co-crosslinking agent: Triallyl isocyanurate (TAIC), "TAIC" manufactured by Mitsubishi Chemical Corporation PFPE4: Gel-like perfluoropolyether compound (a reaction product of "SIFEL8070A" and "SIFEL8070B" manufactured by Shin-Etsu Chemical Co., Ltd.)
[0067] (Sealing material evaluation) The obtained crosslinked molded articles (sealing materials) were subjected to the following evaluations. The results are shown in Tables 1 to 6.
[0068] [1] Measurement of normal physical properties Hardness (type A durometer hardness) was measured using a type A durometer hardness tester in accordance with JIS K6253: 2012. Tensile tests were performed in accordance with JIS K 6251, with a sample shape of No. 3 dumbbell, and the tensile strength (MPa), elongation (%), and 100% modulus (MPa) were measured using a Shopper-type tensile tester.
[0069] As shown in Tables 1 to 5, it was confirmed that Examples 1 to 24 had a 100% improvement in modulus compared to Comparative Examples 1 to 3.
Claims
1. A sealant composition comprising a fluoroelastomer, a silicone polymer having a vinyl group, and a crosslinking agent.
2. The sealant composition according to claim 1 , wherein the silicone polymer comprises at least one selected from the group consisting of vinyl methyl silicone, fluorovinyl methyl silicone, and phenyl vinyl methyl silicone.
3. The sealing material composition according to claim 1 , wherein the content of the silicone polymer is from 1 part by mass to 500 parts by mass with respect to 100 parts by mass of the fluoroelastomer.
4. The sealing material composition according to claim 1 , wherein the crosslinking agent comprises at least one selected from the group consisting of a peroxide-based compound, a polyol-based compound, and a polyamine-based compound.
5. The sealing material composition according to claim 1, wherein the content of the crosslinking agent is 1 to 6 parts by mass based on 100 parts by mass of the fluoroelastomer.
6. The sealant composition according to claim 1 , further comprising a perfluoropolyether compound.
7. The sealing material composition according to claim 6, wherein the content of the perfluoropolyether compound is 0.5 to 30 parts by mass based on 100 parts by mass of the fluoroelastomer.
8. The sealing material composition according to claim 1, further comprising 1 to 30 parts by mass of a filler based on 100 parts by mass of the fluoroelastomer.
9. The sealant composition of claim 8 , wherein the filler comprises silica.
10. The sealant composition according to claim 8 , wherein the filler comprises a fluororesin, the fluororesin comprising polytetrafluoroethylene.
11. A sealant comprising a crosslinked product of the sealant composition according to claim 1.
12. A gate seal for semiconductor manufacturing equipment, comprising the sealing material according to claim 11.
13. A semiconductor manufacturing device comprising the sealant according to claim 11.
Citation Information
Patent Citations
Fluoroelastomer composition, its crosslinking product, and its use
JP2000119468A