WO2008156210A1 - 絶縁性フィルム - Google Patents
絶縁性フィルム Download PDFInfo
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- WO2008156210A1 WO2008156210A1 PCT/JP2008/061598 JP2008061598W WO2008156210A1 WO 2008156210 A1 WO2008156210 A1 WO 2008156210A1 JP 2008061598 W JP2008061598 W JP 2008061598W WO 2008156210 A1 WO2008156210 A1 WO 2008156210A1
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- C08J2325/00—Characterised by the use 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 an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/259—Silicic material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
Definitions
- the present invention relates to an insulating film. More particularly, the present invention relates to an insulating film having good electrical characteristics and heat resistance and having a particularly high breakdown voltage.
- Stretched films made of syndiotactic polystyrene are excellent in heat resistance, chemical resistance, hot water resistance, dielectric properties, electrical insulation, etc., and are expected to be used in various applications.
- the stretched film is used as an insulator for a capacitor because of its excellent dielectric properties and high electrical insulation and heat resistance.
- Patent Documents 1 to 4 propose a capacitor film using syndiotactic polystyrene.
- Patent Document 1 Japanese Patent Application Laid-Open No. Hei 3 1 2 4 7 50
- Patent Document 2 Japanese Patent Laid-Open No. 6-8 0 7 9 3
- Patent Document 3 Japanese Patent Laid-Open No. 7-1 5 6 2 6 3
- Patent Document 4 Japanese Patent Laid-Open No. 8-2 8 3 4 9 6 Disclosure of Invention
- an object of the present invention is to provide an insulating film having a high dielectric breakdown voltage and excellent heat resistance and handleability.
- a biaxially stretched film containing a syndiotactic polystyrene and particles and having a specific orientation structure has a high dielectric breakdown voltage.
- the present invention was completed by discovering excellent heat resistance and handleability.
- the present invention provides (i) a styrenic polymer having a syndiotactic structure and (i i) particles,
- the present invention comprises (1) a styrenic polymer having a syndiotactic structure, and
- An average particle size of 0.01 mass% or more and 1.5 mass% or less is 0. 3 or more 3.
- Spherical cross-linked polymer particles A having a particle size ratio of 1.0 to 1.
- a biaxially stretched insulating film (hereinafter sometimes referred to as film (1)) having a refractive index in the thickness direction of 1.6050 or more and 1.6505 or less.
- the present invention also provides (1) a styrenic polymer having a syndiotactic structure,
- (ii-2) Inactive fine particles having an average particle size of 0.05 m or more and 2.0 mass% or less, an average particle size of 0.01 m or more and 0.5 m or less, and a relative standard deviation of the particle size of 0.5 or less.
- a biaxially stretched insulating film (hereinafter sometimes referred to as film (2)) containing B 2 and having a refractive index in the thickness direction of 1.6050 or more and 1.6505 or less.
- the present invention also provides a U) syndiotactic styrenic polymer
- Resin X having a dielectric constant different by 0.2 or more from styrene polymer of 3% by mass to 48% by mass, And a biaxially stretched insulating film (hereinafter sometimes referred to as film (3)) having a refractive index in the thickness direction of 1.6050 or more and 1.6505 or less.
- the present invention also provides (i) a styrenic polymer having a syndiotactic structure,
- Inactive fine particles A 4 having an average particle size of not less than 0.01 mass% and not more than 1.5 mass%, an average particle diameter of not less than 0.3 and not more than 3.0 m, and a relative standard deviation of the particle diameter of not more than 0.5, and ( iii) 0. 1% by weight to 8% by weight antioxidant,
- a biaxially stretched insulating film (hereinafter sometimes referred to as film (4)) having a refractive index in the thickness direction of 1.6050 or more and 1.6505 or less.
- the present invention has the modes of the films (1) to (4). First, common matters will be described.
- the styrene polymer in the present invention is a styrene polymer having a syndiotactic structure. That is, it has a three-dimensional structure in which the phenyl group or substituted phenyl group, which is a side chain, is alternately located in the opposite direction with respect to the main chain formed from a carbon-carbon bond.
- tacticity is quantified by nuclear magnetic resonance ( 13 C-NMR) with isotope carbon.
- 13 C-NMR nuclear magnetic resonance
- the existence ratio of a plurality of consecutive structural units for example, two is a diat, and three is a triad. In the case of five, it can be indicated by a pentad or the like.
- a syndiotactic styrenic polymer means a syndiotacticity ratio of 75% or more, preferably 85% or more, or 30% or more, preferably 50% or more, racemic pentad (rrrr).
- Styrene polymers are polystyrene, poly (alkylstyrene), poly (halogenated styrene), poly (alkoxystyrene), poly (halogenated alkylstyrene), poly (vinyl benzoate), poly (vinyl naphthalene).
- poly (alkylstyrene) include poly (methylstyrene), poly (ethylstyrene), poly (propylstyrene), poly (butylstyrene), and poly (phenylstyrene).
- poly (halogenated styrene) include poly (chlorostyrene), poly (promostyrene), and poly (polystyrene styrene).
- poly (alkoxystyrene) examples include poly (methoxystyrene) and poly (ethoxystyrene).
- particularly preferred styrenic polymers include polystyrene, poly (P-methylstyrene), poly
- the styrenic polymer in the present invention may be used as a copolymer containing a copolymer component.
- preferred comonomers include styrene polymer monomers as described above, olefin monomers such as ethylene, propylene, butene, hexene, and octene, gen monomers such as butadiene and isoprene, and cyclic gen. Examples include monomers and polar vinyl monomers such as methyl methacrylate, maleic anhydride, and acrylonitrile.
- the weight average molecular weight of the styrenic polymer is preferably 1.0 X 1 0 4 or more and 3.0 X 1 0 6 or less, more preferably 5. 0 1 0 4 or more and 1.5 X 1 0 6 or less, more preferably It is preferably 1. 1 X 1 0 5 or more and 8.0 0 X 1 0 5 or less.
- the weight average molecular weight is 3.0 ⁇ 10 6 or less, the stretching tension is in a suitable range, and breakage or the like hardly occurs during film formation.
- a method for producing such a styrene polymer having a syndiotactic structure is disclosed in, for example, JP-A-62-187708. That is, in the presence of an inert hydrocarbon solvent or in the absence of a solvent, a styrene monomer (the above styrene heavy monomer) is produced using a titanium compound and a condensation product of water and an organoaluminum compound, particularly trialkylaluminum, as a catalyst. It can be produced by polymerizing a monomer corresponding to the coalescence.
- Japanese Patent Application Laid-Open No. 1 1 4 6 9 12 discloses hydrogenated polymers in Japanese Patent Application Laid-Open No. 1 1 7 8 500 5, respectively.
- the styrenic polymer having a syndiotactic structure in the present invention may contain an appropriate amount of an additive such as a known antistatic agent, if necessary.
- the blending amount of these is preferably 10 parts by mass or less with respect to 100 parts by mass of the styrene polymer. If it exceeds 10 parts by mass, it tends to break during stretching, and the production stability becomes poor.
- Such a styrene polymer having a syndiotactic structure is much more excellent in heat resistance than a conventional styrene polymer having an atactic structure.
- the film of the present invention contains particles.
- the average particle diameter of the particles is preferably not less than 0.01 / zm and not more than 3.Oxm. When the average particle size of the particles is within this range, good handleability such as winding property and workability can be obtained while maintaining good electrical characteristics. If the average grain size is too small, the handleability tends to be poor. On the other hand, if the size is too large, the size of the voids in the film increases, so that the electrical characteristics tend to be inferior.
- the film of the present invention contains particles in an amount of 0.01 to 5.0% by mass in 100% by mass of the film. When the content of the particles is within this range, it is possible to improve the winding property and workability while maintaining a good dielectric breakdown voltage of the film.
- the particles may be organic particles or inorganic particles.
- polymer resin particles are preferable.
- crosslinked polystyrene resin particles crosslinked silicone resin particles, crosslinked acrylic resin particles, crosslinked styrene-acrylic resin particles, crosslinked divinylbenzene-acrylic resin particles, crosslinked polyester resin.
- silicone resin particles and cross-linked polystyrene resin particles are particularly preferred from the viewpoint of excellent slipperiness and abrasion resistance.
- Inorganic particles include: (1) silicon dioxide (including hydrates, key sands, quartz, etc.); (2) various crystal forms of alumina; (3) 30% by mass or more of Si 0 2 component Including (4) Mg, containing silicates (eg amorphous or crystalline clay minerals, aluminosilicates (including calcined and hydrated), warm asbestos, zircon, fly ash, etc.)
- silicates eg amorphous or crystalline clay minerals, aluminosilicates (including calcined and hydrated), warm asbestos, zircon, fly ash, etc.
- Ba, and Ca phosphates (including monohydrogen and dihydrogen salts); (7) Li, Na, and K benzoates; (8) Ca, Ba, Zn, and Mn. (9) Mg, Ca, Ba, Zn, Cd, Pb, Sr, Mn, Fe, Co, and Ni titanates; (10) Ba and Pb chromates; (1) Carbon (for example, carbon black, graphite, etc.); (12) Glass (for example, glass powder, glass beads, etc.); (13) Carbonate of Ca and Mg; (14) Foalite; (1 5) Examples include spinel oxides. Of these, calcium carbonate particles and silica particles are preferred, and silica particles are particularly preferred from the viewpoint of excellent slipperiness and abrasion resistance.
- an embodiment containing one type of particle may be used, but an embodiment containing two or more types of particles from the viewpoint that the effect of improving the handleability can be enhanced without lowering the dielectric breakdown voltage. preferable.
- an embodiment containing two or more types of particles having different compositions, an embodiment containing two or more types of particles having different average particle diameters, an embodiment containing two or more types of particles having different shapes, or these A combined mode may be used, but a mode including at least two types of particles having different average particle sizes is particularly preferable.
- the film of the present invention has a refractive index in the thickness direction of 1.6050 or more and 1.6505 or less.
- the dielectric breakdown voltage can be increased.
- the frequency of film breaks in the film manufacturing process is reduced, and productivity can be improved. If the refractive index in the thickness direction is too high, the frequency of film breakage in the film manufacturing process tends to increase, and the productivity of the film decreases. On the other hand, if it is too low, the dielectric breakdown voltage tends to be low and the electrical characteristics are poor.
- the frequency of film breaks in the capacitor manufacturing process increases, and capacitor productivity decreases. Furthermore, the film thickness Spots tend to get worse, making it difficult to obtain capacitors with stable quality.
- the preferred refractive index in the thickness direction in the present invention is such that the stretching ratio of the film is in a specific range, and in the stretching step, the stretching in the direction perpendicular to the uniaxial direction is performed after the stretching in the uniaxial direction. This is achieved by dividing the temperature into multiple stages and creating a specific temperature difference between the first stage temperature and the final stage temperature.
- the film of the present invention may contain other resin components in order to improve moldability, mechanical properties, surface properties, and the like.
- Examples of other resin components that can be contained include a styrene polymer having an atactic structure, a styrene polymer having an isotactic structure, a polyphenylene ether, and a styrene monomaleic anhydride copolymer. It is done. These are easily compatible with styrene polymers having a syndiotactic structure, and are effective in controlling crystallization when preparing a preform for drawing. Therefore, the subsequent stretchability is improved, the stretching conditions can be easily controlled, and a film having excellent mechanical properties can be obtained.
- a styrenic polymer having an atactic structure and a Z or isotactic structure those composed of the same monomers as the syndiotactic styrene polymer are preferable.
- the content of these compatible resin components is preferably 40 parts by mass or less, more preferably 20 parts by mass or less, particularly preferably 10 parts by mass or less with respect to 100 parts by mass of the styrene polymer having a syndiotactic structure. May be 10 parts by mass or less.
- the content ratio of the compatible resin component exceeds 40 parts by mass, the effect of improving the heat resistance, which is an advantage of the syndiotactic styrene polymer, becomes low.
- examples of the resin that is incompatible with the styrene polymer having a syndiotactic structure include polyolefin resins such as polyethylene, polypropylene, polybutene, and polypentene. Polyesters such as polyethylene terephthalate, polybutylene terephthalate, and polyethylene naphthate are listed. I can get lost. Also, polyamides such as nylon 6, nylon 6, 6 and the like can be mentioned.
- Polyphenylene ethers such as polyphenylene sulfide, polycarbonates, polyacrylates, polysulfones, polyether ether ketones, polyether sulfones, polyimides, vinyl halide polymers such as Teflon (registered trademark), polymethyl methacrylate, etc.
- Resins other than the said compatible resin such as an acrylic polymer and polyvinyl alcohol, are mentioned.
- the crosslinked resin containing the said compatible resin is mentioned. Since these resins are incompatible with the syndiotactic styrene polymer, when contained in a small amount, they can be dispersed in an island shape in the syndiotactic styrene polymer and stretched.
- the content ratio of the incompatible resin component is preferably 30 parts by mass or less, more preferably 20 parts by mass or less, and particularly preferably 10 parts by mass or less, with respect to 100 parts by mass of the syndiotactic styrene polymer. .
- additives such as antistatic agents, colorants, weathering agents and the like can be added to the film of the present invention as long as the physical properties thereof are not impaired.
- Films (1) to (4) which are preferred embodiments of the insulating film of the present invention, have the following characteristics in addition to the above common items.
- the film (1) of embodiment 1 of the present invention is
- the refractive index in the thickness direction is 1. 6050 or more and 1. 6550 or less.
- Film (1) is further U i) 0.05 mass% or more and 2.0 mass% or less, the average particle size is 0.01 // m or more and 2.6 m or less, and the average particle size is high in spherical cross-linking It is preferable to contain inert fine particles B 1 smaller than the average particle size of the molecular particles A 1 by 0.4 / xm or more.
- the spherical cross-linked polymer particles A 1 are surface treated with a silane coupling agent. It is preferable.
- the spherical crosslinked polymer particles A 1 are preferably silicone resin particles.
- the inert fine particles B 1 are preferably spherical silica particles having a particle size ratio of 1.0 or more and 1.3 or less.
- the thickness of the film is preferably 0.4 m or more and less than 6.5 m.
- the present invention includes a capacitor using the film (1).
- the styrenic polymer in film (1) is as described in the section on common matters.
- the film (1) of the present invention comprises 0.01 mass of spherical crosslinked polymer particles A 1 having an average particle size of 0.5 m or more and 3.0 zm or less and a particle size ratio of 1.0 or more and 1.3 or less. % To 1.5% by mass.
- the average particle diameter of the spherical cross-linked polymer particles A 1 is not less than 0 and not more than 3.0 / m, preferably not less than 0.6 / zm and not more than 2.0 m, more preferably not less than 0.8 / zm and 1.6. It is as follows. When the average particle size is less than 0.5 xm, the slipping property and the winding property are inferior. On the other hand, if it exceeds 3.0 m, the dielectric breakdown voltage decreases. Especially in the case of a capacitor, it is not preferable because space factor increases and insulation defects increase.
- the spherical crosslinked polymer particles A 1 preferably have a sharp particle size distribution, and specifically, the relative standard deviation representing the steepness of the distribution is preferably 0.5 or less.
- the relative standard deviation representing the particle size distribution of the spherical crosslinked polymer particle A 1 is more preferably 0.4 or less, still more preferably 0.3 or less, and particularly preferably 0.2 or less.
- the shape of the spherical crosslinked polymer particle A 1 is substantially spherical or true spherical.
- the particle size ratio representing the degree of sphericity in the particles must be 1.0 or more and 1.3 or less. There is a point.
- the particle size ratio is preferably 1.0 or more and 1.2 or less, more preferably 1.0 or more and 1.1 or less.
- the apparent Young's modulus of the spherical crosslinked polymer particles A 1 is preferably 1 O kgZmm 2 or more 100 k gZmm 2 or less, more preferably 10 k gZmm 2 or 50 k gZ mm 2 or less.
- the apparent Young's modulus is 10 kgZm 2 or more, the particles are not easily deformed when the film is stretched, and the shape is maintained, so that the slipping property and the winding property can be further improved.
- the apparent Young's modulus is 100 kgZm 2 or less, the particles are less likely to fall off the film, and the breakdown voltage can be further improved.
- the content of the spherical cross-linked polymer particles A 1 in the film (1) is 0.01% by mass or more and 1.5% by mass or less, preferably 0.11% by mass or more and 1.5% by mass or less, more preferably 0. 26 mass% or more and 0.9 mass% or less.
- the content is less than 0.01% by mass, the winding property deteriorates.
- the content exceeds 1.5% by mass, the film surface becomes rough, the abrasion resistance deteriorates, and the dielectric breakdown voltage decreases.
- a capacitor is not preferable because it causes an increase in space factor and a decrease in dielectric breakdown voltage.
- Examples of the spherical cross-linked polymer particles A 1 include cross-linked polyacrylic resin particles, cross-linked polystyrene resin particles, cross-linked acrylic-styrene copolymer resin particles, and silicone resin particles.
- Silicone resin particles have the following formula (1)
- R is at least one selected from alkyl groups having 1 to 6 carbon atoms and phenyl groups.
- the above unit means the following structural formula (2).
- R is the same as described above, and is at least one selected from an alkyl group having 1 to 6 carbon atoms and a phenyl group.
- R in the formula (1) and the structural formula (2) is at least one selected from an alkyl group having 1 to 6 carbon atoms and a phenyl group.
- the alkyl group include a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, and a hexyl group. Two or more of these may be used.
- R is plural kinds, for example, when R is a methyl group and an ethyl group, it can be produced by using a mixture of methyltrimethoxysilane and ethyltrimethoxysilane as a starting material.
- silicone resin polymethylsilsesquioxane particles in which R is a methyl group are particularly preferred.
- Such silicone resin particles are produced by a conventionally known production method, for example, a method of hydrolyzing and condensing organo trialkoxysilane (for example, Japanese Examined Patent Publication No. 40 0 1 1 4 9 1 7 or Japanese Patent Publication No. 2-2). 2 7 6 7 etc.) and production method of polymethylsilsesquioxane particles using methyltrichlorosilane as a starting material (eg Belgian Patent 5 7 2 4 1 2) Can do.
- a conventionally known production method for example, a method of hydrolyzing and condensing organo trialkoxysilane (for example, Japanese Examined Patent Publication No. 40 0 1 1 4 9 1 7 or Japanese Patent Publication No. 2-2). 2 7 6 7 etc.) and production method of polymethylsilsesquioxane particles using methyltrichlorosilane as a starting material (eg Belgian Patent 5 7 2 4 1 2) Can do.
- the silicone resin particles are preferably polymerized in the presence of a surfactant.
- a surfactant include polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene sorbate alkyl ester, and alkylbenzene sulfonate.
- polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, and alkylbenzene sulfonate are preferably used.
- polyoxyethylene alkyl ether polyoxyethylene laur Ryl ether is mentioned.
- the polyoxyethylene alkylphenyl ether include an ethylene oxide adduct of nonylphenol.
- alkylbenzene sulfonates include sodium dodecylbenzenesulfonate. (surface treatment)
- the insulation breakdown voltage is further improved.
- the silane coupling agent used for the surface treatment include vinyltriethoxysilane, vinyltrichlorosilane, vinyltris () 8-methoxyethoxy) silane having an unsaturated bond, and the like.
- Amino-based silanes (j8-aminoethyl) monoaminopropylmethyldimethyloxysilane, N- (jS-aminoethyl) monoaminopropyl trimethoxysilane, Examples include aminopropyltriethoxysilane, N-phenylaminopropyltrimethoxysilane, and the like.
- Epoxy silanes such as jS- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, ⁇ -dalicidoxypropyltrimethoxysilane, glycidoxypropylmethyljetoxysilane, and glycidoxy Propyltriethoxysilane isotropic S.
- methacrylic acid silanes such as acryloxypropylmethyldimethyoxysilane, armethacryloxypropyl trimethoxysilane, armethacryloxypropylmethyljetoxysilane, and armethacryloxypropyl ligatoxysilane. It is done.
- silane pulling agent composed of an epoxy-based silane is preferable from the viewpoints of ease of handling, difficulty in coloring when added, and the like.
- the surface treatment with a silane coupling agent is preferably performed by the following method.
- First, the spherical crosslinked polymer particle A 1 is separated by filtering the slurry (water slurry or organic solvent slurry) of the spherical crosslinked polymer particle A 1 immediately after synthesis, or treating it with a centrifuge or the like. Thereafter, the slurry is again slurried with water or an organic solvent in which a silane coupling agent is dispersed before or after drying, and then heat-treated. Then separate the particles again, then dry the separated particles, depending on the type of silane coupling agent Further, heat treatment can be performed.
- the mechanism by which the dielectric breakdown voltage is further improved by using spherical crosslinked polymer particles A 1 surface-treated with a silane coupling agent, particularly silicone resin particles surface-treated with a silane coupling agent, is The first is that the silane coupling agent adsorbs to the particles, thereby improving the affinity between the syndiotactic polystyrene and the particles and suppressing the generation of voids during stretching. A mechanism for improving the dielectric breakdown voltage is estimated.
- the film (1) of the present invention preferably contains inert fine particles B 1 in addition to the spherical cross-linked polymer particles A 1.
- the dielectric breakdown voltage can be further increased while maintaining the properties.
- the average particle diameter of the inert fine particles B 1 is preferably smaller than the average particle diameter of the spherical crosslinked polymer particles A 1.
- the difference between the average particle diameter of the inert fine particles B 1 and the average particle diameter of the spherical crosslinked polymer particles A 1 is preferably 0.4; um or more, more preferably 0.5 ⁇ m or more, and still more preferably 0. 7 tm or more.
- the average particle diameter of the inert fine particles B 1 is preferably 0.01 111 to 2.6 ⁇ m, more preferably 0 to 0.8 / m, and still more preferably 0.2 zm to 0.6. m or less. If the average particle size is less than 0.01 m, the effect of improving the slipperiness will be reduced. In addition, when the average particle size is 2.6 m or less, the abrasion resistance can be improved.
- the inert fine particles B 1 preferably have a sharp particle size distribution from the same viewpoint as the spherical crosslinked polymer particles A 1 described above.
- the relative standard deviation representing the steepness of the distribution is preferably 0.5 or less, more preferably 0.4 or less, further preferably 0.3 or less, and particularly preferably 0.2 or less.
- the inert fine particles B 1 have a substantially spherical or true spherical shape.
- a particle size ratio that represents the degree of sphericity in the particles is preferred. It is preferably 1.0 or more and 1.3 or less, more preferably 1.0 or more and 1.2 or less, and even more preferably 1.0 or more and 1.1 or less.
- the content of the inert fine particle B 1 is preferably 0.05% by mass or more and 2.0% by mass or less, and the slipperiness is deteriorated when the content is decreased. Therefore, if it is less than 0.05% by mass, the effect of improving slipperiness is low. On the other hand, when the content is 2.0% by mass or less, the insulation breakdown voltage can be further increased. From such a viewpoint, the content of the inert fine particle B 1 is more preferably 0.1% by mass or more and 0.6% by mass or less, and further preferably 0.2% by mass or more and 0.4% by mass or less. .
- the same kind as the spherical crosslinked polymer particle A1 can be used, but from the viewpoint that a function different from the spherical crosslinked polymer particle A1 can be imparted, It is preferable that the particles be different from the crosslinked polymer particles A1.
- silicon dioxide hydrate, Kei sand, comprising quartz, etc.
- the seed crystal form of alumina e.g., the seed crystal form of alumina
- S I_ ⁇ 2 Kei salt containing component at least 30 wt% e.g.
- carbonic acid calcite particles and spherical silica particles are preferred, and spherical silica particles are particularly preferred.
- spherical silica particles are particularly preferred.
- the method of incorporating the various particles as long as they are finally contained in the film (1).
- a method of adding or depositing in an arbitrary process during polymerization of a styrene monomer and a method of adding in an arbitrary process of melt extrusion. Again this In order to disperse these particles effectively, a dispersant, a surfactant or the like can be used.
- the film (1) of the present invention has a refractive index in the thickness direction of 1.6050 or more and 1.6550 or less.
- the refractive index in the thickness direction is preferably 1. 6100 or more and 1. 6450 or less, more preferably 1. 6150 or more and 1. 6350 or less, and particularly preferably 1. 6200 or more and 1. 6250 or less.
- the refractive index in the thickness direction is less than 1.6050, the dielectric breakdown voltage is lowered.
- the film breaks in the capacitor manufacturing process.
- the thickness unevenness of the film deteriorates, and a capacitor with stable quality cannot be obtained.
- film breakage frequently occurs in the film production process and it is very difficult to obtain a film.
- the refractive index in the thickness direction in the present invention is determined by dividing the stretching temperature into a plurality of stages in the stretching in the direction perpendicular to the axial direction, which is performed after stretching in the uniaxial direction. This is achieved by adding a temperature difference, which will be described later, to the stage temperature.
- the thickness of the film (1) is preferably 0.4 / m or more and less than 6. More preferably, it is 0.5; m or more but less than 5. More preferably, it is 0.6 m or more.
- the film thickness In the case of a film used as an insulator for a capacitor, generally the film thickness The thinner the thickness, the higher the capacitance of the capacitor, which is preferable. However, if the film thickness is reduced, wrinkles are easily formed on the film, and the film is easily broken, so that the handleability is lowered. Also, as the film thickness is reduced, the added particles are more likely to fall off. Moreover, problems such as a decrease in the absolute value of the dielectric breakdown voltage occur as the film thickness decreases. It is therefore essential to balance them.
- the present invention provides a highly insulating film having a novel structure having specific particles and an oriented structure by a special manufacturing method described later so that the above-mentioned problem does not occur even when the film thickness is reduced. It is.
- the center line average surface roughness (Ra) of the film (1) is preferably l nm or more and 89 nm or less.
- the center line average surface roughness (Ra) is l l nm or more, the slipperiness becomes better and the workability is further improved. Furthermore, when winding into a roll shape, blocking is suppressed and it becomes easy to obtain a roll having a good winding shape. Further, when the average surface roughness (Ra) of the center line is 89 nm or less, it is difficult to cause a cracking deviation and an end face deviation.
- the lower limit of the centerline average surface roughness (Ra) is preferably 21 nm or more, and more preferably 31 nm or more.
- the upper limit of the center line average surface roughness (Ra) is preferably 79 nm or less, more preferably 69 ⁇ m or less, and particularly preferably 59 nm or less.
- the film (1) preferably has a 10-point average roughness (Rz) of 900 nm or more and 3,000 nm or less.
- Rz 10-point average roughness
- the lower limit of the 10-point average roughness (Rz) is preferably 950 nm, more preferably 1,050 nm, and particularly preferably 1,250 nm.
- the upper limit of R z) is preferably 2,600 nm, more preferably 2,250 nm, particularly preferably 1,950 nm. Especially when the film is thin, Since the film is not as thin as the case, the winding property tends to be worse. for that reason
- the film (1) can be produced by a method that has been conventionally known or accumulated in the industry except for some special production conditions. Hereinafter, the production method of the film (1) will be described in detail.
- a resin composition mainly composed of a styrene polymer having a syndiotactic structure is heated and melted to prepare an unstretched sheet. Specifically, it is heated and melted at a temperature not lower than the melting point (Tm, unit) and not higher than (Tm + 70), extruded into a sheet, cooled and solidified to obtain an unstretched sheet.
- this unstretched sheet is stretched in the biaxial direction. Stretching may be performed simultaneously in the machine direction (machine axis direction) and the transverse direction (direction perpendicular to the machine axis direction), or may be sequentially performed in an arbitrary order. For example, in the case of sequential stretching, first, in a uniaxial direction, a temperature of (glass transition temperature (Tg, unit) -1 O) or more and (Tg + 70t :) or less, preferably 2.3 times or more 6.0 It is stretched at a magnification of not more than 2 times, more preferably not less than 2.5 times and not more than 5.0 times, more preferably not less than 2.times.
- Tg, unit glass transition temperature
- the film is stretched at a magnification of 2.9 to 4.7.
- the temperature difference is preferably 4 or more times higher than the temperature in the first step, more preferably 7 or more, more preferably 11 or more, and particularly preferably 21 or more.
- the upper limit of the temperature difference is preferably 49 or less, more preferably 39 or less, and particularly preferably 29 or less.
- the zone refers to the 1 area delimited by the shutter etc.
- the value obtained by dividing the film width immediately after leaving the final stage by the film width immediately before entering the first stage may be the target draw ratio. It is preferable to increase the film width in an inclined manner, and it is particularly preferable to increase it linearly. Even when stretching in the machine and transverse directions at the same time, the stretching temperature is divided into a plurality of stages, and the temperature difference between the first stage and the final stage is made.
- the film (1) is then heat set at a temperature (at Tg + 70) to Tm.
- the heat setting temperature is preferably 2 0 0 to 2 6 0, more preferably 2 2 0 to 2 5 0, and further preferably 2 3 0 to 2 4 0. heat If the fixing temperature is too high, breakage is liable to occur, especially when a film having a thin film thickness is produced, and the thickness unevenness deteriorates. It is preferable to perform relaxation treatment at a temperature 20: to 9 Ot: lower than the heat setting temperature as necessary after heat setting because the dimensional stability is improved.
- the film (2) of embodiment 2 of the present invention is
- silica particles A2 having an average particle size of 0.6 m or more and 3. or less and a relative standard deviation of the particle size of 0.5 or less.
- Inactive fine particles having an average particle size of 0.05 to 0.5% by mass and a relative standard deviation of particle size of 0.5 or less, 0.05% to 2.0% by mass B 2, and the refractive index in the thickness direction is 1.6050 or more and 1.6505 or less.
- the average particle diameter of the silica particles A 2 is preferably 0.3 / zm or more larger than the average particle diameter of the inert fine particles B 2.
- the inert fine particles B 2 are preferably inorganic fine particles.
- the inert fine particles B 2 are preferably spherical silica particles having a particle size ratio of 1.0 or more and 1.3 or less.
- Silica particles A2 are preferably spherical silica particles having a particle size ratio of 1.0 or more and 1.3 or less.
- the thickness of the film is preferably 0.4 m or more and less than 6.5.
- the present invention includes a capacitor using the film (2).
- the styrenic polymer in film (2) is as described in the section on common matters.
- Film (2) contains 0.01% by mass or more of silica particles A2 having an average particle size of 0.6 // m or more and 3.0 m or less and a relative standard deviation of particle size of 0.5 or less. Contain less than mass%.
- the average particle size of the silica particles A 2 is from 0 to 3.0, preferably 0. 7 // m or more and 2. O m or less, more preferably 0.8 zm or more and 1.6 wm or less, and particularly preferably 0.9 ⁇ 1! 1 or more and 1.3 m or less. If the average particle size is less than 0.6 m, the air-removing ability is lowered and the winding property is deteriorated. On the other hand, when the average particle size exceeds 3.0 m, the dielectric breakdown voltage decreases, and particularly in capacitor applications, the space factor and insulation defects increase.
- the average particle diameter of the silica particles A 2 is preferably 0.3 / zm or more larger than the average particle diameter of the inert fine particles B 2 described later.
- the difference is more preferably 0.5; m or more, particularly preferably 0.7 jm or more.
- the silica particle A2 in the present invention preferably has a sharp particle size distribution.
- the relative standard deviation representing the steepness of the distribution is 0.5 or less.
- the relative standard deviation is small and the particle size distribution is steep, the height of the projection on the film surface becomes uniform.
- the winding property is improved and the number of coarse particles and coarse protrusions is reduced, so that defects are reduced and the breakdown voltage can be improved.
- an increase in the relative standard deviation is not preferable because coarse particles and coarse protrusions increase, defects increase, and the dielectric breakdown voltage decreases.
- the relative standard deviation representing the particle size distribution of the silica particles A2 is preferably 0.4 or less, more preferably 0.3 or less, and particularly preferably 0.2 or less.
- the content of the silica particles A 2 in the film (2) is 0.01% by mass or more and 1.5% by mass or less, preferably 0.05% by mass or more and 1.0% by mass or less, more preferably 0.1% by mass.
- the content is 0.5% by mass or less, more preferably 0.2% by mass or more and 0.4% by mass or less.
- the content is less than 0.01% by mass, the air release property is lowered and the winding property is deteriorated.
- the content exceeds 1.5% by mass Surface becomes too rough, wear resistance deteriorates, and breakdown voltage decreases. In particular, it is not preferable for a capacitor application because the space factor increases.
- the silica particles A2 spherical silica particles having a shape that is substantially spherical or true spherical are preferred.
- the winding effect is improved and the dielectric breakdown voltage is improved.
- the particle size ratio representing the degree of sphericalness in the particles is preferably 1.0 or more and 1.3 or less.
- the particle size ratio is more preferably 1.0 or more and 1.2 or less, and particularly preferably 1.0 or more and 1.1 or less.
- spherical silica particles that are a preferred embodiment of the silica particles A2 and spherical silica particles that are a preferred embodiment of the inert fine particles B2 to be described later are, for example, hydrolyzed orthoketic acid [S i (OC 2 H 5 ) J From the decomposition, hydrous silica [S i (OH) 4 ] monodisperse spheres are formed (Equation 1 below), and the hydrous silica monodisperse spheres are dehydrated to form silica bonds [ ⁇ S i— ⁇ —S i 3] can be produced by three-dimensional growth. (Formula below) (The Chemical Society of Japan '81, No. 9, P. 1503).
- the film (2) of the present invention further contains inert fine particles B 2 in addition to the silica particles A 2 described above.
- inert fine particles B2 By containing the inert fine particles B2, the slipping property is improved, thereby the winding property is improved and the dielectric breakdown voltage is increased.
- the average particle diameter of the inert fine particles B 2 is not less than 0. Ol ⁇ m and not more than 0. Preferably, it is not less than 0.05 mm and not more than 0. More preferably, not less than 0.1 l / m and not more than 0.5 xm. Is 0.2 / m or more and 0.4; m or less. If the average particle size is less than 0.01 m, sufficient slipping property cannot be obtained, that is, sufficient winding property cannot be obtained. On the other hand, if the average particle size exceeds 0.5 im, the height of the low protrusion on the film surface becomes too high, and the slipperiness becomes too high. It becomes easy to wake up. Also, it is not preferable because the abrasion resistance deteriorates and the dielectric breakdown voltage decreases. As described above, the average particle size of the inert fine particles B 2 is silica particles.
- It is preferably smaller than the average particle diameter of A2, and the difference is preferably 0.3 m or more.
- the inert fine particle B 2 in the present invention needs to have a sharp particle size distribution, and a relative standard deviation representing a steepness of the distribution is 0.5.
- the following is preferable.
- the relative standard deviation of the particle diameter of the inert fine particles B 2 is preferably 0.4 or less, more preferably 0.3 or less, and particularly preferably 0.2 or less.
- the content of the inert fine particles B 2 is preferably 0.05% by mass or more and 2.0% by mass or less in the film (2). If the content is small, the slipping property is deteriorated, and if it is less than 0.05% by mass, sufficient slipping property cannot be obtained. On the other hand, an increase in the content is not preferable because the frequency of voids due to particles increases or the breakdown voltage tends to decrease. In addition, the slipping property tends to be too high, and the end face is liable to be displaced during winding. From such a viewpoint, the content of the inert fine particles B 2 is preferably 0.1% by mass or more and 1.0% by mass or less, more preferably 0.1% by mass or more and 0.6% by mass or less. Particularly preferred is 0.1% by mass or more and 0.3% by mass or less.
- inert fine particles B 2 can be used.
- organic fine particles examples include crosslinked polystyrene resin particles, crosslinked silicone resin particles, crosslinked acrylic resin particles, crosslinked styrene-acrylic resin particles, crosslinked divinylbenzene-acrylic resin particles, crosslinked polyester resin particles, polyimide resin particles, and melamine resin particles. Can be mentioned.
- the inorganic fine particles (1) silicon dioxide (hydrate, including Kei sand, quartz, etc.); (2) alumina various crystal forms; (3) the S I_ ⁇ 2 component 3 0 wt% or more free (4) Mg, Zn, Z, silicates (eg, amorphous or crystalline clay minerals, aluminosilicates (including calcined and hydrated), warm asbestos, zircon, fly ash, etc.) oxides of r and T i; (5) sulfates of C a and B a; (6) Li, Ba, and Ca phosphates (including monohydrogen and dihydrogen salts); (7) Li, Na, and K benzoates; (8) Ca, Ba, Zn, and Mn.
- silicates eg, amorphous or crystalline clay minerals, aluminosilicates (including calcined and hydrated), warm asbestos, zircon, fly ash, etc.
- oxides of r and T i oxides of r and T i
- the inert fine particles B 2 are preferably substantially spherical or spherical.
- the particle size ratio representing the degree of sphericity in the particles is preferably 1.0 or more and 1.3 or less, more preferably 1.0 or more and 1.2 or less, and even more preferably 1.0 or more and 1.1. It is as follows. By making the shape more spherical, the breakdown voltage can be further increased. Accordingly, in combination with the above-mentioned particularly preferable types of the inert fine particles B 2, spherical silica particles are particularly preferable as the inert fine particles B 2.
- the spherical silica particles can be obtained, for example, by the production method described above.
- the silica particles A 2 and the inert fine particles B 2 that are indispensable for achieving the object of the present invention other types or other particle sizes may be used as long as the object of the present invention is not inhibited.
- Inactive particles such as fine particles or inorganic fillers may be included.
- the content is preferably 4.0% by mass or less, more preferably 2.5% by mass or less, still more preferably 1.0% by mass or less, and particularly preferably 0. Less than 5% by mass. If the content of other inert particles is increased, the abrasion resistance of the film surface is deteriorated, so that the force dielectric breakdown voltage may be lowered undesirably.
- the various particles used in the present invention as described above are not limited in the method of inclusion as long as they are contained in the final film.
- a method of adding or precipitating in an arbitrary process during polymerization of a styrenic monomer, and a method of adding in an arbitrary process of melt extrusion are included.
- dispersants, surface activity An agent or the like can be used.
- the silica particles A 2 and the inert fine particles B 2 an embodiment using spherical silli force particles can be exemplified.
- the average particle size of each particle is in a specific range that does not overlap, and the relative standard deviation of the particle size of each particle is in a specific range. Therefore, in the particle size distribution curve, the two types of particles show two particle size peaks that can be clearly distinguished. That is, the silica particles A 2 and the inert fine particles B 2 can be clearly distinguished.
- the two particle size peaks overlap each other at the base portion to form a valley portion, it is decomposed into two particle size peaks at the point where the minimum value is shown in the valley portion.
- the film (2) of the present invention has a refractive index in the thickness direction of 1. 6050 or more and 1.655 0 or less, preferably 1. 6100 or more and 1. 6450 or less, more preferably 1. 6 150 or more and 1. 6350 or less. Preferably it is 1. 6200 or more and 1. 6250 or less.
- the refractive index in the thickness direction is less than 1.6050, the dielectric breakdown voltage becomes low.
- the film is easily broken in the manufacturing process of the capacitor, and the handleability is poor.
- the thickness unevenness of the film is poor, and it is not preferable because a capacitor with stable quality cannot be obtained.
- film breakage frequently occurs in the film production process making it very difficult to obtain a film.
- the refractive index in the thickness direction in the present invention is determined by dividing the stretching temperature into a plurality of stages in the stretching in the direction perpendicular to the axial direction, which is performed after stretching in the uniaxial direction. This is achieved by adding a temperature difference to be described later.
- the thickness of the film (2) is preferably 0.4 zm or more and less than 6.5 m, more preferably 0. or more and less than 5.5 // m, and even more preferably 0.6 xm or more 4.
- the present invention provides a highly insulating film having a novel structure having specific particles and an oriented structure by a special manufacturing method described later so that the above-mentioned problem does not occur even when the film thickness is reduced. is there. (Center line average surface roughness: Ra)
- the film (2) preferably has a center line average surface roughness (Ra) of from l nm to 89 nm.
- the center line average surface roughness (Ra) is l l nm or more, the slipperiness is good and the workability is improved. Furthermore, when winding into a roll shape, blocking is suppressed, and it becomes easy to obtain a roll having a good winding shape. Also, if the center line average surface roughness (Ra) is 89 nm or less, winding deviation and end face deviation are less likely to occur.
- the lower limit of the center line average surface roughness (Ra) is preferably 21 nm, more preferably 31 nm.
- the upper limit of the center line average surface roughness (R a) is preferably 79 nm, more preferably 69 nm, and particularly preferably 59 nm.
- the film (2) preferably has a 10-point average roughness (Rz) of 900 nm or more and 3,000 nm or less.
- 10-point average roughness (Rz) is 900 nm or more.
- the lower limit of the 10-point average roughness (R z) is preferably 950 nm, more preferably 1, 0 5 O nm, and further preferably 1, 250 nm.
- the upper limit of the 10-point average roughness (R z) is preferably 2,600 nm, more preferably 2,250 nm, and further preferably 1,950 nm.
- the winding property tends to be worse because the film is less stiff than when it is thick. Therefore, it is particularly effective to set the 10-point average roughness (Rz) within the above range.
- the film (2) of the present invention can be obtained by a method conventionally known or accumulated in the industry, except for some special conditions. Hereinafter, the production method of the film (2) will be described in detail.
- a resin composition mainly composed of a styrene polymer having a syndiotactic structure is heated and melted to prepare an unstretched sheet. Specifically, it is heated and melted at a temperature not lower than the melting point (Tm, in units) and not higher than (Tm + 70V.), Extruded into a sheet, cooled and solidified to obtain an unstretched sheet.
- the obtained unstretched sheet has an intrinsic viscosity of 0.35 to 0.9 d.
- a range of 1 is preferred.
- this unstretched sheet is stretched in the biaxial direction. Stretching may be performed simultaneously in the machine direction (machine axis direction) and in the horizontal direction (direction perpendicular to the machine axis direction), or may be sequentially performed in any order. For example, in the case of sequential stretching, first, in the uniaxial direction, at a temperature of (glass transition temperature (Tg, unit)-1 OX) or more (Tg + 70t :) or less, 2.7 times or more and 4. 9 times or less, preferably 2 8 times or more 4. 6 times or less, more preferably 2. 9 times or more 4. 1 time or less, particularly preferably 3.3 times or more and 3. 8 times or less.
- Tg, unit glass transition temperature
- the temperature difference is preferably 4 or higher than the temperature of the first stage, more preferably 7 or higher, more preferably 11 or higher, and more preferably 20 or higher. .
- too large temperature difference is not preferable because stretchability is low and thickness unevenness of the film after stretching is unfavorable.
- the upper limit of the temperature difference is preferably 49 T: or less, and 39 or less is the following.
- the zone refers to the area of 1 divided by the shirt evening etc. in the ten evening etc.
- the film width immediately after leaving the final stage divided by the film width immediately before entering the first stage should be the target draw ratio, and it is preferable to increase the film width in an inclined manner. It should be increased linearly. Even when stretching in the machine and transverse directions at the same time, the stretching temperature is divided into a plurality of stages, and the temperature difference between the first stage and the final stage is made.
- the film (2) is then heat-set at a temperature (at Tg + 70) to Tm.
- the heat setting temperature is preferably 200 or more and 260 or less, more preferably 220 to 25 Ot: or less, and further preferably 230 or more and 240 or less.
- the heat setting temperature is too high, particularly when a film having a thin film thickness is produced, a breaking force is likely to occur, and thickness unevenness is deteriorated. It is preferable to perform relaxation treatment at a temperature 20 to 90 lower than the heat setting temperature as necessary after heat setting because the dimensional stability is improved.
- the film (3) of embodiment 3 of the present invention is
- the refractive index in the thickness direction is 1. 6050 or more and 1. 6550 or less.
- the melting point of the resin X is preferably (Tms -30) or more and (Tms +30) or less in the following range with respect to the melting point (Tms, unit: 1 ) of the styrene polymer.
- the resin X is preferably at least one selected from the group consisting of a polyethylene terephthalate resin and a polyethylene naphtharate resin.
- Fine particles (ii-1) 0.01 mass% or more and 1.5 mass% or less, average particle size of 0.6 ⁇ or more and 3.0_im or less, relative standard deviation of particle size of 0.5 or less (Ii 1 2) 0.05 mass% or more and 2.0 mass% or less, average particle size of 0.01 // 111 or more and 0.5 / zm or less, relative particle size Standard deviation is 0.5 or less
- the average particle size of the inert fine particles A 3 is 0.3 zzm or more larger than the average particle size of the inert fine particles B 3.
- the inert fine particles A 3 are preferably spherical particles having a particle size ratio of 1.0 or more and 1.3 or less.
- the inert fine particles A 3 are preferably spherical polymer particles.
- the inert fine particles A3 are preferably spherical silica particles.
- the inert fine particles B 3 are preferably spherical silica particles having a particle size ratio of 10 or more and 1.3 or less.
- Aspect 3 includes a condenser using film (3).
- the styrenic polymer in film (3) is as described in the section on common matters.
- the film (3) of the present invention contains fine particles having an average particle diameter of not less than 0. Ol ⁇ m and not more than 3. O / zm.
- the average particle size of the contained fine particles is in the above range, good handleability such as winding property and workability can be obtained while maintaining good electrical characteristics. If the average particle size of the fine particles is too small, the handleability tends to be poor. On the other hand, if the average particle size of the fine particles is too large, the size of voids in the film increases, so that the electrical characteristics tend to be inferior.
- the average particle size of the fine particles is preferably from 0. 2 to ⁇ ⁇ , more preferably from 0.1 m to 1.6 / m, and particularly preferably from 0.2 / m to 1.
- the film (3) contains 0.01% by mass to 5.0% by mass of fine particles in 100% by mass of the film (3).
- the content of the fine particles is preferably 0.1% by mass or more and 3.5% by mass or less, more preferably 0.2% by mass or more and 2.0% by mass or less, and still more preferably 0.8% by mass. 3 mass% or more and 0.7 mass% or less.
- the fine particles as described above may be organic fine particles or inorganic fine particles.
- polymer resin particles are preferable, for example, crosslinked polystyrene.
- silicone resin particles and cross-linked polystyrene resin particles are particularly preferred from the viewpoint of excellent sliding properties and abrasion resistance.
- silicon dioxide hydrate, including Kei sand, quartz, etc.
- alumina various crystal forms
- S I_ ⁇ 2 components or more 30 wt% content (4) Mg, Zn, Zr. (4) Mg, Zn, Zr, etc.
- an embodiment containing one kind of fine particles is preferred, and an aspect containing two or more kinds of fine particles is preferred from the viewpoint that the effect of improving the handleability can be enhanced without reducing the dielectric breakdown voltage.
- an embodiment containing two or more types of fine particles having different compositions, an embodiment containing two or more types of fine particles having different average particle diameters, an embodiment containing two or more types of fine particles having different shapes, or this An embodiment in which these are combined may be used, but an embodiment power S containing at least two types of fine particles having different average particle sizes is particularly preferable.
- U i 1) Average particle diameter is 0.6 m or more and 3.0 // m or less, and the relative standard deviation of particle diameter is 0.
- the average particle size is 3 m or more larger than the average particle size of 3 can be exemplified.
- it is possible to suppress a decrease in electrical characteristics due to the addition of fine particles to a minimum, and it is possible to further enhance the effect of improving handling properties such as winding property and workability. .
- the average particle diameter of the inert fine particles A3 is preferably 0.6 zm or more and 3. or less, more preferably 0. or more and 2. or less, and still more preferably 0.8 / m or more.
- the average particle diameter of the inert fine particles A 3 is in the above range, the air release property can be improved, and the effect of improving the winding property can be enhanced. If the average particle size of the inert fine particles A 3 is too small, sufficient air repellency tends not to be obtained, that is, the effect of improving the winding property is lowered. On the other hand, if it is too large, the size of the voids in the film tends to increase, that is, the effect of improving the electrical characteristics becomes low.
- the relative standard deviation of the particle diameter of the inert fine particles A 3 is preferably 0.5 or less, more preferably 0.4 or less, further preferably 0.3 or less, and particularly preferably 0.2 or less. If the relative standard deviation of the particle size is in the above range, it means that the particle size distribution of the inert fine particles A 3 is a sharp shape, and the projection height on the film surface becomes uniform, thereby improving the winding property. Can be high. In addition, coarse particles and coarse protrusions are reduced, thereby reducing defects and increasing the dielectric breakdown voltage improvement effect.
- the content of inert fine particles A3 is preferably 0.01% by mass or more and 1.5% by mass or less, more preferably 0.05% by mass or more and 1.0% by mass or less in 100% by mass of the film (3). More preferably, the content is 0.1% by mass or more and 0.5% by mass or less, and particularly preferably 0.2% by mass or more and 0.4% by mass or less. Inactive fine particles A3 in the above range By containing this amount, it is possible to increase the effect of improving the handleability while keeping the dielectric breakdown voltage of the film (3) good. If the content of the inert fine particles A3 is too small, the air release property tends to be inferior, and the effect of improving the winding property is lowered.
- the film surface tends to become too rough, which tends to deteriorate the abrasion resistance of the film surface, and the effect of improving the dielectric breakdown voltage is reduced. Also, especially in capacitor applications, the space factor tends to increase.
- the inert fine particles A 3 are preferably spherical particles having a particle size ratio of 1.0 or more and 1.3 or less.
- the particle size ratio is more preferably 1.0 or more and 1.2 or less, and particularly preferably 1.0 or more and 1.1 or less.
- the particle size ratio is in the above range, the effect of improving the scraping property and the effect of improving the dielectric breakdown voltage can be further increased.
- inert fine particles A organic fine particles and inorganic fine particles similar to the fine particles described above can be used.
- polymer resin particles are preferable, and silicone resin particles and cross-linked polystyrene resin particles are particularly preferable from the viewpoint of excellent slipperiness and abrasion resistance.
- polymer resin particles are preferably spherical as described above, that is, spherical polymer resin particles are preferred.
- spherical silicone resin particles and spherical cross-linked polystyrene resin particles are particularly preferred from the viewpoint of superior slipperiness and abrasion resistance.
- inorganic fine particles calcium carbonate particles and silica particles are preferable, and silica particles are particularly preferable from the viewpoint of excellent slipperiness and abrasion resistance.
- Such inorganic fine particles are preferably spherical as described above, and spherical silica particles are particularly preferred from the viewpoint of superior slipperiness and abrasion resistance.
- the average particle size of the inert fine particles B3 is preferably from 0.1 1 zm to 0.5 m, more preferably from 0.05 m to 0.5 m, and even more preferably from 0.1 im to 0.5 m. Hereinafter, it is particularly preferably 0.2 m or more and 0.4 / zm or less.
- the average particle size of the inert fine particles B 3 is in the above range, moderate slipperiness can be obtained, The effect of improving the winding property can be increased. If the average particle size of the inert fine particles B 3 is too small, sufficient slipping property tends to be not obtained, that is, the effect of improving the winding property is lowered.
- the inert fine particle B 3 preferably has a sharp particle size distribution from the same viewpoint as the inert fine particle A 3 described above, and the relative standard deviation of the particle size of the inert fine particle B 3 is preferably 0. .5 or less, more preferably 0.4 or less, still more preferably 0.3 or less, and particularly preferably 0.2 or less.
- the content of the inert fine particles B 3 is preferably from 0.05% by mass to 2.0% by mass, more preferably from 0.1% by mass to 1.0% by mass in the film (3) 100% by mass. % By mass or less, more preferably 0.1% by mass or more and 0.6% by mass or less, and particularly preferably 0.1% by mass or more and 0.3% by mass or less.
- Inert fine particles B 3 are preferably spherical particles having a particle size ratio of 1.0 or more and 1.3 or less, and more preferably 1.0 or more, from the same viewpoint as the aforementioned inert fine particles A 3. .2 or less, particularly preferably 1.0 or more and 1.1 or less.
- inert fine particles B 3 organic fine particles and inorganic fine particles similar to the fine particles described above can be used.
- inorganic fine particles are preferable, and calcium carbonate particles and silica particles are preferable, and silica particles are particularly preferable from the viewpoint of excellent slipperiness and abrasion resistance.
- such inorganic fine particles are preferably spherical, and may be superior in terms of slipperiness and abrasion resistance. Particularly preferred are spherical force particles.
- the inert fine particles A3 and the inert fine particles B3 preferably have an average particle size of the inert fine particles A3 of 0.3 / zm or more larger than the average particle size of the inert fine particles B3.
- the difference is more preferably 0.5 m or more, particularly preferably 0.7 m or more.
- the fine particles used in the present invention are not limited in the method of inclusion as long as they are contained in the final film.
- a method of adding or precipitating in an arbitrary process during polymerization of a styrene monomer there are a method of adding in an arbitrary process of melt extrusion.
- a dispersant, a surfactant or the like can be used.
- Film (3) contains resin X.
- the resin X is a resin having a dielectric constant different from the dielectric constant of the styrene polymer by 0.2 or more.
- the difference between the dielectric constant of the styrenic polymer and the dielectric constant of the resin X is preferably 0.4 or more, and more preferably 0.5 or more.
- the resin X in the present invention has a melting point in the range of (Tms ⁇ 30) or more and (Tms + 30) or less with respect to the melting point of the styrene polymer (Tms, unit: 1 C). It is preferable to have.
- the melting point of the resin X is in the above range, when the styrenic polymer and the resin X are mixed, the mixed state becomes good, that is, the resin The dispersion state of X becomes good, and the effect of improving the breakdown voltage is enhanced.
- the melting point of the resin X is preferably (Tms—20) and above (Tms +20), and in the following range: (Tms—15): above (Tms +15): below Is more preferably in the range of (Tms ⁇ 5) and above (Tms + 5) X: It is particularly preferably in the following range.
- the difference between the melting point of the resin X and the melting point of the styrene polymer is 1 or more, the dispersion state of the resin X may be better, or the effect of improving the breakdown voltage may be further enhanced. Is preferable. From such a viewpoint, the difference between the melting point of the resin X and the melting point of the styrene polymer is more preferably 2 or more, and particularly preferably 3 or more.
- Examples of the resin X described above include polyethylene terephthalate (PET) resin, polyethylene naphthenate (PEN) resin, polyester such as polybutylene terephthalate (PBT) resin, polyolefin such as polypropylene, and nylon 6 Polyamides such as polyamide such as nylon 6 and nylon 6, polyphenylene sulfide, etc., polycarbonate, polyacrylate, polysulfone, polyether ether ketone, polyethersulfone, polyimide, vinyl halide polymer, acrylic polymer such as methyl methacrylate Preferable examples include a polymer and polyvinyl alcohol.
- polyester is preferable, and polyethylene terephthalate (PET) resin and polyethylene naphtharate (PEN) resin are more preferable.
- PET polyethylene terephthalate
- PEN polyethylene naphtharate
- PET polyethylene terephthalate
- the film (3) of the present invention is a biaxially stretched film made of a resin composition containing 3% by mass or more and 48% by mass or less of the resin X.
- the resin X By blending the resin X in an amount in the above range, the electrical characteristics of the resulting film can be improved. Specifically, the breakdown voltage can be increased.
- the amount of the resin X is preferably 4% by mass or more and 40% by mass or less, more preferably 6% by mass or more and 3 ⁇ % by mass or less, and particularly preferably 9% in 100% by mass of the resin composition.
- the mass is 24% by mass or more. (Other additives)
- the film (3) of the present invention has a refractive index in the thickness direction of 1.6050 or more and 1.6550 or less.
- the refractive index in the thickness direction is preferably 1. 6100 or more and 1. 6400 or less, more preferably 1. 6130 or more and 1. 6380 or less, and particularly preferably 1. 6150 or more and 1. 6360 or less.
- the dielectric breakdown voltage can be improved.
- the frequency of film breaks in the film manufacturing process decreases, and the productivity can be improved. If the refractive index in the thickness direction is too high, the frequency of film breakage in the film production process tends to increase, and the productivity of the film decreases.
- the dielectric breakdown voltage tends to be low, and the electrical characteristics are poor.
- the frequency of film breaks in the capacitor manufacturing process increases.
- the thickness unevenness of the film tends to deteriorate, and a capacitor with stable quality cannot be obtained.
- the refractive index in the thickness direction in the present invention is determined by dividing the stretching temperature into a plurality of stages in stretching in the direction perpendicular to the -axial direction, which is performed simultaneously with stretching in the uniaxial direction after stretching in the uniaxial direction. This is achieved by making a specific temperature difference between the first stage temperature and the final stage temperature.
- the thickness of the film (3) of the present invention is preferably 0.3 im or more and less than 12 m, more preferably 0.4 m or more and less than 6. O m, more preferably 0.5 m or more and less than 3.5 zm. It is. By setting the film thickness within the above range, a capacitor having a high electrostatic capacity can be produced.
- a film used as an insulator for a capacitor is generally preferred to have a thinner film thickness because the capacitance of the capacitor is higher.
- wrinkles tend to occur in the film and the film breaks and becomes thin.
- the added particles are likely to fall off, resulting in a low breakdown voltage.
- problems such as a decrease in the absolute value of the dielectric breakdown voltage occur as the film thickness decreases. Therefore, it is essential to balance them.
- the present invention obtains a film (3) having a novel structure having specific fine particles and an oriented structure by adopting a production method described later so that the above-mentioned problem does not occur even when the film thickness is reduced. Is.
- the film (3) of the present invention preferably has a center line average surface roughness (Ra) of at least one surface of 11 nm or more and 89 nm or less.
- Ra center line average surface roughness
- the film (3) of the present invention preferably has a center line average surface roughness (Ra) of at least one surface of 11 nm or more and 89 nm or less.
- the lower limit of the surface roughness (Ra) is preferably 21 nm, and more preferably 31 nm.
- the upper limit of the surface roughness (Ra) is preferably 79 nm, more preferably 69 nm, and particularly preferably 59 nm.
- the film (3) of the present invention preferably has a 10-point average roughness (Rz) of at least one surface of 900 nm or more and 3,000 nm or less.
- Rz 10-point average roughness
- 10-point average roughness (Rz) is more preferably 950 nm, still more preferably 1,050 nm, particularly preferably 1,250 nm.
- the upper limit of the 10-point average roughness (Rz) is more preferably 2,600 nm, still more preferably 2,250 nm, and particularly preferably 1,950 nm.
- the film (3) of the present invention can be obtained by a method conventionally known or accumulated in the industry, except for some special conditions. Hereinafter, the production method of the film (3) of the present invention will be described in detail.
- an unstretched sheet is prepared by heating and melting a resin composition in which a predetermined amount of resin X is blended with a syndiotactic styrene polymer. Specifically, the melting point of the resin composition (Tm, unit: in) above (at Tm + 70) is heated and melted at the following temperature, extruded into a sheet, cooled and solidified to obtain an unstretched sheet.
- this unstretched sheet is stretched in the biaxial direction. Stretching may be performed simultaneously in the machine direction (machine axis direction) and the transverse direction (direction perpendicular to the machine axis direction), or may be sequentially performed in any order. For example, in the case of sequential stretching, first, in the uniaxial direction (glass transition temperature of the resin composition (Tg, unit: in) 1 l Ot) above (at Ding + 70) below 2.7 times 4. Stretch at a magnification of 8 times or less, preferably 2.9 times or more, 4. 4 times or less, more preferably 3.1 times or more and 4.0 times or less.
- Tg or more (Tg + 80 :) or less in the direction perpendicular to the axial direction it is 2.8 times or more and 4. 9 times or less, preferably 3.0 times or more and 4.5 times or less, more preferably 3. More than 2 times 4. Stretch at a magnification of 1 times or less.
- the stretching speed is preferably 500% or more, more preferably 1,000% or more, more preferably 2,000% or more, and particularly preferably 4, 0 0 0% Z min or more.
- the stretching speed is preferably 3 0, 0 0 0% Z min or less, more preferably 1 5 0 0 0 0% / min or less, further preferably 9 0 0 0%% or less, particularly preferably 6, 0 0 0% / min or less.
- the temperature difference is preferably such that the final stage temperature is 4 or more higher than the first stage temperature, more preferably 7 or more, even more preferably 1 It: or more, and particularly preferably 15 or more.
- the temperature difference is 49 or less, preferably 39 or less, more preferably 29 T: or less, and particularly preferably 20 or less. If the temperature difference is too large, film breakage tends to occur or the thickness unevenness of the film after stretching tends to deteriorate.
- the zone is the shutter at Tenyu etc. Indicates one area separated by etc. In either case, it is preferable to further divide between the first stage and the final stage, and to increase the temperature gradually from the first stage to the final stage. For example, when two or more continuous stretching zones having different temperatures are used, it is preferable to further provide one or more stretching zones between the first stretching zone and the last stretching zone.
- the value obtained by dividing the film width immediately after leaving the final stage by the film width immediately before entering the first stage may be the target draw ratio. It is preferable to increase the film width in an inclined manner, and it is particularly preferable to increase it linearly. Even when stretching in the machine and transverse directions at the same time, the stretching temperature is divided into a plurality of stages, and the temperature difference between the first stage and the final stage is made.
- the stretching speed and the stretching temperature described above are employed, but it is more preferable to employ both embodiments, the stretching process is stabilized, It becomes easy to achieve the refractive index and preferred film thickness in the present invention.
- the heat setting temperature is 2 0 0 or more and 2 60 or less, preferably 2 2 0 or more and 2 5 0 or less, and more preferably 2 3 0 or more and 2 40 or less.
- the heat setting temperature is too high, film breakage is likely to occur especially when a thin film is produced, and the thickness unevenness deteriorates. 2o from heat setting temperature if necessary after heat setting
- Inactive fine particles A 4 having an average particle size of not less than 0.1 and not more than 1.5% by mass, an average particle size of not less than 0.3 and not more than 3, and a relative standard deviation of the particle size of not more than 0.5, iii) 0.1 to 8% by weight of antioxidant,
- the refractive index in the thickness direction is 1. 6050 or more and 1. 6550 or less.
- Film (4) has an average particle size of 0.05 to 2.0 mass%, an average particle size of 0.01 to 0.5 m, and an average particle size of inert fine particles A4. It is preferable to contain inert fine particles B4 smaller than 0.2 // m and having a relative standard deviation of particle size of 0.5 or less.
- the inert fine particles A 4 are preferably spherical particles having a particle size ratio of 1.0 or more and 1.3 or less.
- the inert fine particles A4 are preferably spherical polymer particles.
- the inert fine particles A4 are preferably spherical silica particles.
- the inert fine particles B 4 are preferably spherical silica particles having a particle size ratio of 1.0 or more and 1.3 or less.
- the thermal decomposition temperature of the antioxidant is preferably 250 or more.
- the film (4) preferably has a thickness of 0.4 / m or more and less than 6.5 m.
- the present invention includes a capacitor using the film (4).
- the styrenic polymer in film (4) is as described in the section on common matters.
- the dielectric breakdown voltage can be increased.
- Such an antioxidant may be either a primary antioxidant that captures the generated radicals to prevent oxidation or a secondary antioxidant that decomposes the generated peroxides to prevent oxidation.
- primary antioxidants include phenolic antioxidants and amine antioxidants.
- Secondary antioxidants include phosphorus-based antioxidants and sulfur-based antioxidants.
- phenolic antioxidants 2,6-di-tert-butyl-4-methylphenol, 2,6-di-tert-butyl-4-ethyl phenol, 2-t-butyl-4-1 methoxyphenol, 3-t-butyl-4 -Methoxyphenol, 2,6-di-t-butyl-4 (4,6-bis (octylthio) -1,3,5-triazine-2-ylamino) phenol, n-octyldecyl 3- (3, 5—Di-t-Buchi (Lu 4-hydroxyphenyl) Monophenolic antioxidants such as propionate. '
- amine-based antioxidant examples include alkyl-substituted diphenylamine.
- Phosphorous antioxidants include triphenyl phosphite, diphenyl isodecyl phosphite, phenyl diisodecyl phosphite, 4,4'-butylidene bis (3-methyl-6_t-butylphenyl ditridecyl) phosphite, Decylphosphite, tris (nonylphenyl) phosphite, diisodecyl pen Erisri!
- Sulfur-based antioxidants include dilauryl 1,3,3 'monodipropionate, dimyristyl-3,3' monothiodipropionate, distearyl-3,3'-didipropionate, Penyu Erisli! ⁇ One-tetrakis (3-laurylthiopropionate), 2-mercaptobenzimidazole, etc.
- the antioxidant is particularly preferable from the viewpoint that it is more excellent in corrosion resistance and can further enhance the effect of improving the dielectric breakdown voltage, and a phenolic antioxidant is particularly preferable.
- the antioxidant preferably has a thermal decomposition temperature of 2500 or higher. If the thermal decomposition temperature is too low, the antioxidant itself is thermally decomposed during melt extrusion, which tends to cause problems such as contamination of the process and yellowing of the polymer. From such a viewpoint, the thermal decomposition temperature of the antioxidant is more preferably 28 8 Ot: or more, further preferably 30 ° C .: or more, particularly preferably 3 20 or more.
- the antioxidant in the present invention is preferably more resistant to thermal decomposition, but preferably has a higher thermal decomposition temperature. However, in reality, the upper limit is about 500 and below.
- the melting point of the antioxidant is preferably 90 or more. If the melting point is too low, the antioxidant melts faster than the polymer during melt extrusion, and the polymer tends to slip at the screw feed portion of the extruder. As a result, the supply of polymer becomes unstable and problems such as poor film thickness unevenness occur. From such a viewpoint, the lower limit of the melting point of the antioxidant is more preferably 1 2 O t :, more preferably 15 O: and particularly preferably 20 0. On the other hand, when the melting point of the antioxidant is too high, the antioxidant becomes difficult to melt during melt extrusion, and the dispersion in the polymer tends to be poor. As a result, problems such as the effect of adding the antioxidant appear only locally. From such a viewpoint, the upper limit of the melting point of the antioxidant is preferably 30, more preferably 25, and further preferably 2 2 O :, particularly preferably 1700.
- the film (4) of the present invention contains the above antioxidant in an amount of 0.1% by mass or more and 8% by mass or less based on the mass of the film (4).
- the dielectric breakdown voltage is excellent.
- the lower limit of the content of the antioxidant is preferably 0.2% by mass, more preferably 0.5% by mass, and even more preferably 1% by mass.
- the upper limit of the content of the antioxidant is preferably 7% by mass, more preferably 5% by mass, and further preferably 3% by mass.
- One type of antioxidant may be used alone, or two or more types may be used in combination. When two or more types are used in combination, an embodiment using two or more types of primary antioxidants may be used. Alternatively, two or more types of secondary antioxidants may be used, or one or more types of primary antioxidants and one or more types of secondary antioxidants may be used in combination. For example, it is expected that both primary and secondary oxidations can be prevented by using two types of antioxidants, a primary antioxidant and a secondary antioxidant. In the present invention, among them, an embodiment in which a primary antioxidant is used alone or an embodiment in which two or more kinds of primary antioxidants are used is preferable from the viewpoint that the effect of improving the dielectric breakdown voltage can be further increased. An embodiment in which a phenolic antioxidant is used alone or an embodiment in which two or more phenolic antioxidants are used is preferred.
- the film (4) of the present invention contains inert fine particles A4.
- the average particle diameter of the inert fine particles A4 is not less than 0 and not more than 3.0. By setting the average particle size of the inert fine particles A 4 within the above range, the film can have good air evacuation performance while maintaining a high dielectric breakdown voltage, and has excellent winding properties.
- the average particle diameter of the inert fine particles A 4 is preferably 0.2 or more and 2. O m or less, more preferably 0.4 mm or more and 1.6 m or less, and particularly preferably 1.0 ⁇ It is 111 or more and 1.2 m or less.
- the relative standard deviation of the particle diameter of the inert fine particles A 4 is 0.5 or less.
- the relative standard deviation of the particle size is preferably 0.4 or less, more preferably 0.3 or less, and particularly preferably 0.2 or less.
- the inert fine particles A 4 are preferably spherical particles having a particle size ratio of 1.0 or more and 1.3 or less.
- the particle size ratio is more preferably 1.0 or more and 1.2 or less, particularly preferably It is preferably 1.0 or more and 1.1 or less.
- the content of the inert fine particles A 4 is not less than 0.01% by mass and not more than 1.5% by mass with respect to 100% by mass of the film (4).
- the film can be handled easily while maintaining a high dielectric breakdown voltage.
- the content of the inert fine particles A 4 is too small, the air release property tends to be inferior and the winding property is inferior.
- the amount is too large, the film surface tends to be too rough, which tends to deteriorate the abrasion resistance of the film surface, resulting in poor dielectric breakdown voltage. Also, especially in capacitor applications, the space factor tends to increase.
- the content of the inert fine particles A 4 is preferably 0.05% by mass or more and 1.0% by mass or less, more preferably 0.1% by mass or more and 0.5% by mass or less, and particularly preferably. In other words, it is 0.2% by mass or more and 0.4% by mass or less.
- the inert fine particles A 4 as described above may be organic fine particles or inorganic fine particles.
- organic fine particles examples include polymer resin particles such as polystyrene resin particles, silicone resin particles, acrylic resin particles, styrene-acrylic resin particles, divinylbenzene-acrylic resin particles, polyester resin particles, polyimide resin particles, and melamine resin particles.
- polymer resin particles such as polystyrene resin particles, silicone resin particles, acrylic resin particles, styrene-acrylic resin particles, divinylbenzene-acrylic resin particles, polyester resin particles, polyimide resin particles, and melamine resin particles.
- silicone resin particles and polystyrene resin particle strength are particularly preferred from the viewpoint of excellent slipperiness and abrasion resistance.
- Such polymer resin particles are preferably spherical as described above, that is, spherical polymer resin particles are preferred.
- spherical silicone resin particles and spherical polystyrene resin particles are particularly preferable from the viewpoint of superior slipperiness and abrasion resistance.
- silicon dioxide hydrate, including Kei sand, quartz, etc.
- alumina various crystal forms
- the S I_ ⁇ 2 component 3 0 wt% or more Containing silicates (eg amorphous or crystalline clay minerals, aluminosilicates (including calcined and hydrated), warm asbestos, zircon, fly ash, etc.);
- Mg, Zn, Oxides of Zr and Ti (5) sulfates of Ca and Ba; (6) L i, B a and C a phosphates (including monohydrogen and dihydrogen salts); (7) L i, Na and K benzoates; (8) C a, Ba, Zn, (9) Mg, Ca, Ba, Zn, Cd, Pb, Sr, Mn, Fe, Co, and Ni titanates; (10) Ba, and Pb chromium (1 1) Carbon (eg, carbon black, graphite, etc.); (12) Glass (eg, glass powder,
- calcium carbonate particles and silica particles are preferred, and silica particles are particularly preferred from the viewpoint of excellent slipperiness and abrasion resistance.
- silica particles are particularly preferred from the viewpoint of excellent slipperiness and abrasion resistance.
- inorganic fine particles are preferably spherical as described above, and spherical silica particles are particularly preferred from the viewpoint of being superior in terms of slipperiness and abrasion resistance.
- the film (4) preferably contains, in addition to the inert fine particles A 4, inert fine particles B 4 whose average particle diameter and relative standard deviation of the particle diameter are in a specific range.
- the average particle diameter of the inert fine particles B 4 is not less than 0. Oljum and not more than 0.5 // m. By setting the average particle diameter of the inert fine particles B 4 within the above range, it is possible to obtain an appropriate slip property and to enhance the winding effect. If the average particle size of the inert fine particles B4 is too small, the slipping property tends to be low, and the effect of improving the winding property is low. On the other hand, if it is too large, the height of the low protrusions on the film surface tends to be too high, thereby making the slipping property too high and causing the end face to be misaligned during winding. Become. In addition, the wear resistance tends to deteriorate, and the effect of improving the breakdown voltage is reduced.
- the average particle size of the inert fine particles B 4 is preferably 0.05 / 111 or more and 0 or less, more preferably 0.08 mm or more and 0 or less, and further preferably 0.1 zm or more and 0. . 3 m or less.
- the average particle diameter of the inert fine particles B 4 is preferably smaller than the average particle diameter of the inert fine particles A 4 by 0.2 m or more.
- the average particle diameter of the inert fine particles B4 is more preferably 0.4 / m or more smaller than the average particle diameter of the inert fine particles A4, and the aspect smaller than 0.6 m is further preferred.
- An embodiment having a size of 0.8 zm or more is particularly preferable.
- the inert fine particle B 4 has a relative standard deviation of the particle size of 0.5 or less from the same viewpoint as the inert fine particle A 4 described above.
- the relative standard deviation of the particle diameter of the inert fine particles B 4 is preferably 0.4 or less, more preferably 0.3 or less, and particularly preferably 0.2 or less.
- the inert fine particles B 4 in the present invention are preferably spherical particles having a particle size ratio of 1.0 or more and 1.3 or less, more preferably 1 from the same viewpoint as the inert fine particles A 4 described above. 0 or more and 1.2 or less, particularly preferably 1.0 or more and 1.1 or less.
- the film (4) of the present invention preferably contains 0.05% by mass or more and 2.0% by mass or less of the inert fine particles B 4 in 100% by mass of the film (4).
- the content of the inactive fine particles B 4 in the above range, the effect of improving the handleability of the film can be enhanced while maintaining a high dielectric breakdown voltage.
- the content of the inert fine particles B 4 is too small, the slipping property tends to be low, and the effect of improving the winding property is low.
- the amount is too large, the frequency of voids in the film tends to increase, and the effect of improving the dielectric breakdown voltage decreases.
- the slipping property tends to be too high, and the effect of improving the winding property, such as end face misalignment during winding, is reduced.
- the content of the inert fine particles B 4 is more preferably 0.1% by mass or more and 1.0% by mass or less, and further preferably 0.1% by mass or more and 0.5% by mass or less. Particularly preferably, the content is 0.1% by mass or more and 0.3% by mass or less.
- the inert fine particles B 4 the same organic fine particles and inorganic fine particles as the aforementioned inert fine particles A 4 can be used.
- inorganic fine particles are preferable, and calcium carbonate particles and silica particles are preferable, and silica particles are particularly preferable from the viewpoint of excellent slipperiness and abrasion resistance.
- Such inorganic fine particles are preferably spherical as described above, and spherical silica particles are particularly preferred from the viewpoint of being superior in terms of slipperiness and abrasion resistance.
- the inert fine particles A 4 and the inert fine particles B 4 are not limited in the method of inclusion as long as they are contained in the final film.
- a method of adding or precipitating in an arbitrary process during polymerization of a styrenic monomer, and a method of adding in an arbitrary process of melt extrusion are included.
- a dispersant, a surfactant and the like can be used.
- the inert fine particles A 4 and the inert fine particles B 4 there can be exemplified an embodiment using spherical silli force particles, but even in such a case, each particle In the particle size distribution curve, the above two types of particles can be clearly distinguished because the average particle size in each is in a specific range that does not overlap, and the relative standard deviation of the particle size in each particle is small. Two particle size peaks are shown, that is, the inactive fine particles A 4 and the inactive fine particles B 4 can be clearly distinguished. In addition, when the two particle size peaks overlap each other at the base portion to form a valley portion, it is decomposed into two particle size peaks at the point where the minimum value is shown in the valley portion.
- the film (4) of the present invention has a refractive index in the thickness direction of 1.6050 or more and 1.6550 or less.
- the refractive index in the thickness direction is preferably 1. 6100 or more and 1. 6400 or less, more preferably 1. 6130 or more and 1. 6380 or less, and further preferably 1. 6150 or more and 1. 6360 or less.
- Set the refractive index in the thickness direction within the above range. Can increase the dielectric breakdown voltage.
- the frequency of film breaks in the film manufacturing process decreases, and productivity can be improved.
- the refractive index in the thickness direction is too high, the frequency of film breakage in the film manufacturing process tends to increase, and the productivity of the film decreases.
- the breakdown voltage tends to be low and the electrical characteristics are poor.
- the frequency of film breaks in the manufacturing process of a capacitor increases and the productivity of the capacitor decreases.
- uneven thickness of the film tends to deteriorate, making it difficult to obtain a capacitor with stable quality.
- the preferred refractive index in the thickness direction in the present invention is such that the stretching ratio of the film is in a specific range to be described later, and in the stretching step, the film is stretched in the direction perpendicular to the -axis direction, which is performed after the uniaxial stretching.
- the stretching temperature is divided into multiple stages, and this is achieved by making a specific temperature difference between the first stage temperature and the final stage temperature.
- the film (4) of the present invention preferably has a film thickness of 0.4 Aim or more and less than 6.5 / zm. More preferably, it is 0.4 / m or more and less than 6. Especially preferably, it is 0.5 m or more and less than 3.5 m.
- a film used as an insulator for a capacitor is preferable to have a thinner film because the capacitance of the capacitor is higher.
- wrinkles tend to occur in the film, and the film becomes broken and squeezed, resulting in poor handling.
- the added particles easily fall off, resulting in a low breakdown voltage.
- problems such as a decrease in the absolute value of the dielectric breakdown voltage occur as the film thickness decreases. Therefore, it is essential to balance them.
- the present invention provides a film (4) having a novel structure comprising an antioxidant and specific particles so that the above-mentioned problems do not occur even when the film thickness is reduced. It is obtained by the manufacturing method.
- the film (4) of the present invention preferably has a center line average surface roughness (Ra) of at least one surface of 7 nm or more and 89 nm or less.
- Ra center line average surface roughness
- the lower limit of the center line average surface roughness (Ra) is preferably l nm, more preferably 21 nm, and even more preferably 31 nm.
- the upper limit of the center line average surface roughness (Ra) is preferably 79 nm, more preferably 69 nm, and still more preferably 59 nm.
- the film (4) of the present invention preferably has a 10-point average roughness (R z) of at least one surface of 200 nm or more and 3,000 nm or less.
- R z 10-point average roughness
- the film (4) of the present invention preferably has a 10-point average roughness (R z) of at least one surface of 200 nm or more and 3,000 nm or less.
- the 10-point average roughness (Rz) is more preferably 600 nm or more, still more preferably 1,000 nm or more, and particularly preferably 1,250 nm or more.
- the upper limit of the 10-point average roughness (Rz) is more preferably 2,600 nm or less, further preferably 2,250 nm or less, and particularly preferably 1,950 nm or less.
- the film (4) of the present invention can be obtained by a method that has been conventionally known or accumulated in the industry, except for some special production methods. Hereinafter, the production method of the film (4) of the present invention will be described in detail.
- a resin composition in which a predetermined amount of an antioxidant is blended with a syndiotactic styrene polymer is heated and melted to prepare an unstretched sheet.
- the resin composition is heated and melted at a temperature not lower than the melting point (Tm, unit :) and not higher than (Tm + 70 t :), extruded in a single bowl shape, cooled and solidified to obtain an unstretched sheet.
- this unstretched sheet is stretched biaxially.
- the stretching may be performed simultaneously in the machine direction (machine axis direction) and the transverse direction (direction perpendicular to the machine axis direction), or may be sequentially performed in an arbitrary order.
- sequential stretching first, in the uniaxial direction (the glass transition temperature of the resin composition (T g, unit:)-1 O t :) 2.7 times at a temperature below (T g + 70) 4.8 times or less, preferably 2.9 times or more, 4.4 times or less, more preferably 3.1 times or more and 4.0 times or less, and then stretched in the direction perpendicular to the axial direction.
- the lower limit of the stretching speed is preferably 500% / min or more, more preferably 1, 0 0 0% min or more, more preferably 2,00% min min or more, particularly preferably 4,00% min min or more.
- the upper limit of the stretching speed is preferably 30, 0 00% / min or less, more preferably 15 5, 0 0% min or less, further preferably 9, 0 0 0% Z min or less, particularly preferably Less than 6, 0 0 0% min.
- the stretching temperature is not made constant, but is divided into a plurality of stages, and the temperature of the first stage and the temperature of the final stage are It was proved effective to add a temperature difference.
- the lower limit of the temperature difference is preferably 4 or more higher than the temperature in the first stage, more preferably 7 or higher, more preferably 12 or higher, and 15 or higher. Is particularly preferred.
- the upper limit of the temperature difference is preferably 49 or less, more preferably 39 or less, even more preferably 29 or less, and particularly preferably 2 O t: or less. If the temperature difference is too large, film breakage tends to occur. In addition, the uneven thickness of the film after stretching tends to deteriorate.
- the zone inlet (first stage) and outlet (final stage) in one stretching zone It is possible to create a temperature difference between the first and second stretching zones (first stage) and the last stretching zone (final stage) by providing two or more continuous stretching zones with different temperatures.
- the zone refers to the area of 1 divided by the shirt evening etc. in the ten evening etc. In either case, it is preferable to further divide between the first stage and the final stage, and to increase the temperature gradually from the first stage to the final stage, and in particular, increase linearly. .
- the stretching zone when two or more continuous stretching zones having different temperatures are used, it is preferable to further provide one or more stretching zones between the first stretching zone and the last stretching zone. More preferably, a zone is provided. It is disadvantageous from the viewpoint of equipment costs to set the total of the drawing zones to 13 or more.
- the film width immediately after leaving the final stage divided by the film width immediately before entering the first stage should be the target draw ratio, and it is preferable to increase the film width in an inclined manner. It should be increased linearly. Even when stretching in the machine and transverse directions at the same time, the stretching temperature is divided into a plurality of stages, and the temperature difference between the first stage and the final stage is made.
- these means can be preferably exemplified as means for achieving the preferred refractive index in the thickness direction in the present invention. Furthermore, according to these means, breakage is unlikely to occur even if the film thickness is reduced. Therefore, these means can be preferably exemplified as means for achieving a preferable film thickness in the present invention.
- heat fix at a temperature of ⁇ Tm at Ding ⁇ + 70).
- the temperature for heat setting is 2 0 0 X: not less than 2 6 0, preferably 2 2 0 or more and not more than 2 5 0, and more preferably 2 3 0 or more and 2 4 0 or less.
- the heat setting temperature is too high, film breakage is likely to occur, and unevenness in thickness is worsened, particularly when a film having a thin film thickness is produced. If heat treatment is followed by relaxation treatment at a temperature 2 Ot: ⁇ 90 ° below the heat setting temperature as necessary, the dimensional stability will be improved.
- the powder is dispersed so that individual particles do not overlap as much as possible, and a gold thin film deposited layer is formed on this surface with a thickness of 200 to 30 OA by a gold sputtering device, Observation with a scanning electron microscope at 10,000 to 30,000 times, and at least 100 particles with a Luzex 500 manufactured by Nihon Regiureter Co., Ltd., the equivalent area diameter (D i), major axis (D 1 i) and the minor axis (D si) were determined.
- a small piece of sample film is fixed on a sample stage for a scanning electron microscope, and the surface of the film is measured using a sputtering device (JIS-1100 type ion sputtering device) manufactured by JEOL Ltd. under a vacuum of 0.13 Pa. Ion etching treatment was performed for 10 minutes under the conditions of 25 kV and 1.25 mA.
- a gold spatter was applied using the same device, and observed at 10,000 to 30,000 times using a scanning electron microscope, and the area of at least 100 particles was measured with the Luzex 500 manufactured by Nihon Regiyureta Corporation.
- the equivalent particle diameter (D i), major axis (D 1 i) and minor axis (D si) were determined.
- the values obtained from the above item (1-1) and for the average particle size and particle size ratio of the particles in the film are as follows:
- the number n of particles was used, and the number average value of the area equivalent particle diameter (D i) was defined as the average particle diameter (D).
- the particle diameter ratio was calculated as D 1 ZDs from the average value of the major axis (D 1) and the average value of the minor axis obtained from the following formula (Ds).
- Measurement length (Lx) lmm, sampling pitch 2 using a non-contact type 3D roughness meter (Kosaka Laboratories, ET-30HK) with a semiconductor laser with a wavelength of 780 nm and an optical stylus with a beam diameter of 1.6 / zm / m, cut-off 0.25 mm, thickness direction magnification 10,000 times, horizontal direction magnification 200 times, number of scanning lines 100 (thus, measurement length Ly 0.2 mm in Y direction) Measure the protrusion profile.
- the shrinkage rate (unit:%) of the film in 30 minutes in an atmosphere at 150 with no tension was determined.
- the measurement was performed according to the method shown in JISC 2 1 5 1. 23 and relative humidity 5 In a 0% atmosphere, using a DC withstanding voltage tester, the upper electrode uses a brass cylinder with a diameter of 25 mm, the lower electrode uses an aluminum cylinder with a diameter of 75 mm, and the pressure is increased at a pressure increase rate of 100 VZ seconds. The voltage when the film was broken and short-circuited was read. The measurement was performed 41 times, and the median value of 21 samples was taken as the breakdown voltage (BDV) measurement value, except for the 10 larger and 10 smaller ones.
- BDV breakdown voltage
- Measurements at 10 o and 12 ot were performed by setting electrodes and samples in a hot-air oven, connecting to a power source using a heat-resistant cord, and starting pressurization 1 minute after the oven was turned on.
- Judgment was made as follows according to the number of breaks that occurred during the production of a biaxially stretched film of 1 million m.
- Stretchability ⁇ Less than 1 break per film formation of 100,000 111
- Stretchability ⁇ Breaking 2 to less than 4 times per 100,000 m film
- Stretchability X 4 to less than 8 breaks per 100,000 m film formation
- Stretchability X X Break more than 8 times per 100,000 111 film formation
- the film was rolled up into a roll of 6,000 m in a 550 mm width at a speed of 10 OmZ, and was rated as follows according to the winding condition and appearance of the roll.
- aqueous solution containing 0.06% by mass of sodium hydroxide 7, OO Og is placed in a 10 liter glass container with a stirring blade, and polyoxyethylene lauryl ether is added to the upper layer.
- polyoxyethylene lauryl ether is added to the upper layer.
- 1,000 g of methyltrimethoxysilane containing 0.01% by mass is added to form two layers, and then react for 2 hours while rotating slightly at 10 to 15 to produce spherical particles. I let you. Thereafter, the temperature in the system was set at 70, and the mixture was aged for about 1 hour, cooled, and filtered through a vacuum filter to obtain a cake-like product of silicone resin particles having a water content of about 40%.
- a cake having a water content of about 40% was obtained. Finally, the cake was subjected to reduced pressure treatment at 100 to 15 torr for 10 hours to obtain about 400 g of powder of silicone resin particles having a small amount of aggregated particles and surface-treated with a silane coupling agent.
- the obtained silicone resin particle powder had an average particle size of 1.3; m, a relative standard deviation of 0.14, and a particle size ratio of 1.1.
- Weight average molecular weight 3.0 x 10 5 polystyrene observed to have almost perfect syndiotactic structure by 13 C-NMR measurement, average particle size 1.3 g as spherical cross-linked polymer particle A1, relative 0.3 mass% of silicone resin particles with a standard deviation of 0.14 and a particle size ratio of 1.1, an average particle size of 0.3 im as an inert fine particle B1, a relative standard deviation of 0.17, a particle size ratio 1.
- Spherical silica particles (1) manufactured by Nippon Shokubai Co., Ltd. (trade name: Seafos Yuichi KE) were added in an amount of 0.2% by mass to obtain a styrene polymer.
- silicone resin particles surface-treated with the silane coupling agent obtained above were used.
- This polymer is dried at 12 Ot: for 4 hours, fed to an extruder, melted at 29, extruded from a die slit, cooled and solidified on a casting drum, and unstretched sheet It was created.
- This unstretched sheet was stretched 2.9 times in the longitudinal direction (machine axis direction) at 1 4 and then led to the ten evening direction, and then 3.0 times in the lateral direction (direction perpendicular to the machine axis direction).
- the film was stretched twice.
- the stretching in the transverse direction is carried out by a stretching process composed of two stretching zones having the same length, and is stretched 2.0 times at a temperature of 100 in the first stretching zone (first stage).
- the film width was linearly increased so that the final stretching ratio was 3.0 times by further stretching 1.5 times at a temperature of 11 1.
- the film was heat-fixed at 2 3 5 for 9 seconds, and further cooled to 1 80 and subjected to 5% relaxation treatment to obtain a biaxially stretched film having a thickness of 3.0 // m and wound into a roll.
- Table 1 shows the properties of the film.
- Example 1 The film obtained from Example 1 had good stretchability and winding property, had a high dielectric breakdown voltage, and was suitable as an insulator for a capacitor. Examples 2-7, Comparative Example 1
- a biaxially stretched film was obtained in the same manner as in Example 1 except that the spherical crosslinked polymer particles A 1, the inert fine particles B 1, the film forming conditions and the film thickness were as shown in Table 1.
- Table 1 shows the properties of the film.
- the films obtained from Examples 2 and 3 were excellent in stretchability and winding property, had high dielectric breakdown voltage, and were suitable as an insulator for a capacitor.
- the films obtained from Examples 4 to 6 had good winding properties, high dielectric breakdown voltage, and were suitable as an insulator for a capacitor. The stretchability was able to withstand practical use.
- Example 7 Although the film obtained from Example 7 was inferior in stretchability, it had a high dielectric breakdown voltage and was suitable as an insulator for a capacitor.
- Comparative Example 2 In order to obtain a film having a refractive index in the thickness direction of approximately 1.6600, film forming conditions such as the stretching ratio in the machine direction and the transverse direction were set as shown in Table 1, and film rupture occurred frequently. However, a biaxially stretched film could not be obtained. Comparative Example 3
- the film obtained from Comparative Example 3 had low heat resistance, and the dielectric breakdown voltage significantly decreased at high temperatures. Moreover, the heat shrinkage rate was high, and it was not suitable as a highly insulating film.
- condenser one was created as follows using the obtained film.
- aluminum was vacuum-deposited on one side of the film to a thickness of 50 OA.
- deposition was performed in the form of vertical stripes consisting of a repetition of an 8 mm wide deposited portion and an lmm wide non-deposited portion.
- the obtained vapor-deposited film is slit at the center in the width direction of the vapor-deposited part and the non-vapor-deposited part, and consists of a 4-mm wide vapor-deposited part and a 0.5-mm wide non-deposited part. Into a take-up reel.
- the two reels were overlapped and wound so that the non-deposited portions became the opposite end faces, respectively, to obtain a wound body, and then pressed at 150 and IMP a for 5 minutes.
- Metallicon was sprayed on both end faces of the wound body after pressing to form external electrodes, and lead wires were welded to the metallicon to create a wound film capacitor.
- the film capacitors obtained from Examples 1 to 7 were excellent in heat resistance and withstand voltage characteristics and exhibited excellent performance as a capacitor.
- the Luzex 500 made by Nihon Regiyure Ichiyu Co., Ltd. at least 1,000 particles, the area equivalent particle size (D i), major axis (D 1 i ) And minor axis (D si) were determined.
- a small piece of sample film is fixed to a sample stage for a scanning electron microscope, and the surface of the film is subjected to a vacuum of 0.13 Pa using a sputtering apparatus (JIS-1100 type ion sputtering apparatus) manufactured by JEOL Ltd. Then, ion etching was performed for 10 minutes under the conditions of 0.25 kV and 1.25 mA. Furthermore, a gold spatter was applied with the same device, and observed at a magnification of 10,000 to 30,000 using a scanning electron microscope. In Luzex 500, the area equivalent particle diameter (D i), major axis (DI i) and minor axis (D si) of at least 1,000 particles were determined.
- D i area equivalent particle diameter
- DI i major axis
- D si minor axis
- the values obtained from the above (1 1 1), and for the average particle size and particle size ratio of the particles in the film The number n of particles was used, and the number average value of the area equivalent particle diameters (D i) was taken as the average particle diameter (D).
- the particle size ratio was calculated as D 1 ZDs from the average value of the major axis (D 1) and the average value of the minor axis (Ds) obtained from the following formula.
- a weight-average molecular weight 3. 0X 10 5 the polystyrene to be an almost perfect syndiotactic structure observed in 13 C-NMR measurement, the silica particles A2 Spherical silica particles with an average particle size of 1., a relative standard deviation of 0.15, and a particle size ratio of 1.08 (made by Nippon Shokubai Co., Ltd .: trade name Seifos Yuichi (registered trademark) KE-P100) Spherical silica particles with an average particle size of 0.3 // m, relative standard deviation of 0.16, and a particle size ratio of 1.08 as 3% by mass and inert fine particles B2 (made by Nippon Shokubai Co., Ltd .: trade name Sea Hoster) (Registered trademark) KE-P30) was added in an amount of 0.2% by mass to obtain a styrenic polymer. This polymer was dried at 120 for 4 hours, supplied to an extruder, melted at 290, extruded from
- This unstretched sheet was stretched 3.0 times in the longitudinal direction (machine axis direction) at 1 14 and then led to Tenyu, and then stretched 3.1 times in the transverse direction (direction perpendicular to the machine axis direction). did.
- the stretching in the transverse direction is performed by a stretching process composed of two stretching zones having the same length, and the first stretching zone (first stage) is stretched 2.05 times at a temperature of 100, and the second stretching zone.
- the film width was linearly increased so that the final draw ratio was 3.1 times by further stretching 1.51 times at a temperature of 112.
- the film obtained from Example 8 had good stretchability and winding property, high dielectric breakdown voltage, and was suitable as a capacitor insulator.
- Example 15 A biaxially stretched film was obtained in the same manner as in Example 8, except that the silica particles A2, the inert fine particles B2, the film forming conditions, and the film thickness were as shown in Table 2. Table 2 shows the characteristics of the film obtained.
- Example 15 A biaxially stretched film was obtained in the same manner as in Example 8, except that the silica particles A2, the inert fine particles B2, the film forming conditions, and the film thickness were as shown in Table 2. Table 2 shows the characteristics of the film obtained.
- Example 15 shows the characteristics of the film obtained.
- silica particles A 2 and A biaxially stretched film was obtained in the same manner as in Example 8 except that the content of the inert fine particles B2, the film forming conditions, and the film thickness were as shown in Table 2. Table 2 shows the properties of the film.
- Spherical silica particles with an average particle size of 1.6 m, a relative standard deviation of 0.13, and a particle size ratio of 1.10 as silica particles A2 (Nippon Shokubai Co., Ltd .: trade name )
- Spherical silica particles with an average particle size of 0.1 m, a relative standard deviation of 0.17, and a particle size ratio of 1.07 as inert fine particles B2 (Nippon Catalyst Co., Ltd.)
- Shihosyuichi registered trademark
- the films obtained from Examples 9 and 10 had good stretchability and winding property, high insulation breakdown voltage, and were suitable as an insulator for a capacitor.
- the films obtained from Examples 1 to 13 had good tearability, high dielectric breakdown voltage, and were suitable as an insulator for a capacitor. The stretchability could withstand practical use.
- Example 14 Although the film obtained from Example 14 was inferior in stretchability, it had a high dielectric breakdown voltage and was suitable as an insulator for a capacitor.
- the films obtained from Examples 15 and 16 were excellent in stretchability and winding property, had high dielectric breakdown voltage, and were suitable as an insulator for a capacitor. Comparative Example 4
- a biaxially stretched film was obtained in the same manner as in Example 8, except that the silica particles A2, the inert fine particles B2, the film forming conditions, and the film thickness were as shown in Table 2.
- Table 2 shows the characteristics of the film obtained.
- the film obtained from Comparative Example 4 has a low refractive index in the thickness direction and thus has a low dielectric breakdown voltage, and is not suitable as an insulator for a capacitor. I got it. Comparative Example 5
- Polypropylene having an isotactic degree of 97% obtained from 13 C_NMR was melted at 250, and after extrusion through a die slit, it was cooled and solidified on an 8 Ot: roll to obtain an unstretched sheet. Next, the film was stretched 4.5 times in the longitudinal direction at 135, 9 times in the transverse direction at 163, heat-fixed at 163 for 9 seconds, and relaxed by 2% at 160 to a film thickness of 3.0. m biaxially oriented polypropylene film was obtained. Table 2 shows the properties of the film.
- the film obtained from Comparative Example 6 had low heat resistance, and the dielectric breakdown voltage significantly decreased at high temperatures. Moreover, the heat shrinkage rate was high, and it was not suitable as a highly insulating film.
- the capacitor was created as follows using the obtained film.
- aluminum was vacuum-deposited on one side of the film to a thickness of 50 OA.
- deposition was performed in the form of vertical stripes consisting of repetition of an 8 mm wide vapor deposition part and an lmm wide non-deposition part.
- the obtained vapor-deposited film is slit at the center in the width direction of the vapor-deposited part and the non-vapor-deposited part, and consists of a 4-mm wide vapor-deposited part and a 0.5-mm wide non-deposited part. Into a take-up reel.
- a wound type film capacitor was created by spraying a methicon on both end faces of the wound body after pressing to form an external electrode and welding a lead wire to the metallicon.
- the film capacitors obtained from Examples 8 to 14 were excellent in heat resistance and withstand voltage characteristics and exhibited excellent performance as a capacitor. Examples 17-29, Comparative Examples 7-8
- Dimethyl terephthalate and ethylene glycol are used as monomers, manganese acetate is used as an ester exchange catalyst, antimony trioxide is used as a polymerization catalyst, and phosphorous acid is used as a stabilizer.
- polyethylene terephthalate resin melting point: 258, dielectric constant: 3.2).
- the resulting mixture is pelletized, and the pellet is dried at 130 for 7 hours, then supplied to an extruder, melted at 290, extruded from a die slit, and cooled and solidified on a casting drum to produce an unstretched sheet did.
- the weight average molecular weight is 3.0 X 10 5 , and 95 parts by weight of polystyrene, which is observed to have a nearly perfect syndiotactic structure by 13 C—NM R measurement,
- a biaxially stretched film was obtained in the same manner as in Example 17 except that 5 parts by mass of the polyethylene terephthalate resin obtained above was blended as the resin composition, and was wound up in a mouth shape.
- the properties of the obtained film are shown in Table 3.
- Example 18 The film obtained in Example 18 was excellent in stretchability and winding property, had a high dielectric breakdown voltage, and was suitable as a highly insulating film. Therefore, it was a suitable capacitor as an insulator.
- Example 1 9-2 2 The film obtained in Example 18 was excellent in stretchability and winding property, had a high dielectric breakdown voltage, and was suitable as a highly insulating film. Therefore, it was a suitable capacitor as an insulator.
- a biaxially stretched film was obtained in the same manner as in Example 18 except that a resin composition in which the blending ratio of the styrenic polymer and the resin X was as shown in Table 3 was used and wound into a roll. The properties of the obtained film are shown in Table 3.
- Example 19 to 21 were excellent in stretchability and winding property, particularly high in dielectric breakdown voltage, and were suitable as highly insulating films. Therefore, it is suitable as an insulator for capacitors, and particularly suitable as an insulator for capacitors used in hybrid vehicles. Comparative Example 7, Example 2 3
- a biaxially stretched film was obtained and wound into a roll in the same manner as in Example 19 except that the film forming conditions such as the stretching ratio in the machine direction and the transverse direction, and the stretching temperature were as shown in Table 3.
- the properties of the obtained film are shown in Table 3.
- Comparative Example 7 Since the film obtained in Comparative Example 7 had a low refractive index in the thickness direction, the dielectric breakdown voltage was low, and it was unsuitable as a highly insulating film.
- the film obtained in Example 23 was excellent in stretchability and winding property, particularly high in dielectric breakdown voltage, and was suitable as a highly insulating film. Therefore, it is suitable as an insulator of a capacitor, and particularly suitable as an insulator of a capacitor used in a hybrid vehicle. Comparative Example 8
- a biaxially stretched film was obtained and wound into a roll in the same manner as in Example 19 except that the film forming conditions such as the stretching speed and stretching temperature in the transverse direction were as shown in Table 3.
- the properties of the obtained film are shown in Table 3.
- Example 24 and 25 were inferior in stretchability because the stretching speed condition in the transverse stretching was not in the preferred range.
- dielectric breakdown voltage was relatively low, the roll-up property was good and it could withstand practical use as a highly insulating film.
- Example 1 9 except that a mixture obtained by adding 0.6 parts by mass (namely 0.6% by mass in the obtained film) is used. A biaxially stretched film was obtained. The properties of the obtained film are shown in Table 3.
- Example 27 The film obtained in Example 26 had a relatively low winding property and dielectric breakdown voltage, but could withstand practical use as a highly insulating film.
- Example 27
- a biaxially stretched film was obtained in the same manner as in Example 19 except that fine particles composed of 0.2 parts by mass (0.2% by mass in the obtained film) were used. The properties of the obtained film are shown in Table 3.
- Example 27 The film obtained in Example 27 had good stretchability and winding property, and particularly had a high dielectric breakdown voltage, and was suitable as a highly insulating film. Therefore, it is suitable as an insulator of a capacitor, and particularly suitable as an insulator of a capacitor used in a hybrid vehicle.
- Example 28
- Example 29 A biaxially stretched film was obtained in the same manner as in Example 19 except that a polyethylene naphtharate resin (melting point: 269, dielectric constant: 3.1) was used as the resin X. Table 3 shows the properties of the film.
- the film obtained in Example 28 had a relatively low dielectric breakdown voltage, but was excellent in stretchability and winding property and could withstand practical use as a highly insulating film.
- Example 29
- a biaxially stretched film was obtained in the same manner as in Example 19 except that a polypropylene resin (melting point: 170, dielectric constant: 2.1) was used as the resin X. Table 3 shows the properties of the film.
- the film obtained in Example 29 had a relatively low dielectric breakdown voltage at high temperatures because of the low heat resistance of the polypropylene used as Resin X, but could withstand practical use as a highly insulating film. It was hot.
- Example 30 A biaxially stretched film was obtained in the same manner as in Example 19 except that polycarbonate resin (melting point: 24 3:, dielectric constant: 2.8) was used as the resin X. Table 3 shows the characteristics of the obtained film.
- PET Polyethylene terephthalate
- PEN Polyethylene naphthalate resin
- PET Polyethylene terephthalate resin
- PEN Polyethylene naphthalate resin
- PET Polyethylene terephthalate resin
- PEN Polyethylene naphthale
- PET Polyethylene terephthalate resin
- PEN Polyethylene naphthalate resin
- the capacitor was created as follows using the obtained film.
- aluminum was vacuum-deposited on one side of the film to a thickness of 50 OA.
- deposition was performed in the form of vertical stripes consisting of repetition of an 8 mm wide vapor deposition part and an lmm wide non-deposition part.
- the obtained vapor-deposited film is slit at the center in the width direction of the vapor-deposited part and the non-vapor-deposited part, and consists of a 4-mm wide vapor-deposited part and a 0.5-mm wide non-deposited part. Into a take-up reel.
- the two reels were overlapped and wound so that the non-deposited portions became the opposite end faces, respectively, to obtain a wound body, and then pressed at 150 and IMP a for 5 minutes.
- Metallicon was sprayed on both end faces of the wound body after pressing to form external electrodes, and lead wires were welded to the metallicon to create a wound film capacitor.
- the film capacitor using the films obtained in Examples 18 to 29 was excellent in heat resistance and withstand voltage characteristics and exhibited excellent performance as a capacitor. In addition, it was excellent in workability when making one capacitor.
- the film capacitors using the films obtained in Examples 19 to 23 and 27 were excellent in heat resistance, particularly excellent in withstand voltage characteristics, and exhibited superior performance as a capacitor.
- the film was wound up into a roll of 500 mm width and 9000 m at a speed of 14 OmZ, and the roll shape of the obtained roll and the end face deviation at the end face of the roll were rated as follows.
- the end face deviation at the end face of the roll is less than 0.5 mm, which is good.
- ⁇ The end face deviation at the end face of the roll is 0.5 mm or more and less than lmm, which is almost good.
- the end face deviation at the end face of the roll is 1 mm or more and less than 2 mm, which is slightly inferior, but can be used as a product.
- the end face deviation at the end face of the roll is 2 mm or more, which is inferior and cannot be used as a product.
- the weight average molecular weight is 3.0X 10 5 and is observed to have an almost complete syndiotactic structure by 13 C-NMR measurement.
- spherical silica particles (Nippon Shokubai Co., Ltd. product name: Seafos Yuichi KE) (0.3% by mass based on the mass of the film obtained) and inert fine particles B4, Spherical shape with average particle size 0.3 / xm, relative standard deviation 0.16, particle size ratio 1.08 Guatemala particles (made by Nippon Shokubai Co., Ltd .: trade name Seafos Yuichi KE) were mixed with 0.2 part by mass (0.2% by mass based on the mass of the film obtained) to obtain a resin mixture. It was.
- the resulting resin mixture was dried at 130 for 7 hours, then fed to the extruder, melted at 290, solidified by cooling on a casting drum cooled at 20 after extrusion from a die sledge, unstretched Created a sheet.
- a biaxially stretched film having a thickness of 3.0 m was obtained in the same manner as in Example 32 except that the content of the antioxidant was as shown in Table 4, and wound into a roll. Table 4 shows the characteristics of the film obtained. The amount of polystyrene was adjusted so that the whole would be 100 parts by mass.
- Example 37
- N N 'bis [3- (3, 5-- tert-butyl 4-phenyloxyl) propionyl] hydrazine (Ciba Specialty' Chemicals: Trade name I RGANOX 1024) (melting point 210
- a biaxially stretched film having a thickness of 3. O ⁇ m was obtained and wound into a roll.
- the properties of the obtained film are shown in Table 4.
- the films obtained in Examples 32 to 35 had good stretchability and tearability, had high insulation breakdown voltage, and were suitable as an insulator for a capacitor.
- Example 38 the film obtained in Example 37 using an antioxidant different from Examples 32 to 35 described above also has good stretchability and winding property, high dielectric breakdown voltage, and a capacitor-like insulator. It was suitable as.
- Example 38
- a biaxially stretched film was obtained and wound into a roll.
- Table 4 shows the properties of the film. The amount of polystyrene was adjusted so that the whole would be 100 parts by mass.
- Spherical silica particles with an average particle size of 0.5 rn, a relative standard deviation of 0.15, and a particle size ratio of 1.08 with 98.4 parts by mass of polystyrene and inert fine particles A4 (Nippon Catalysts: product name) Seafos Yuichi KE) 0.1 parts by mass (0.1% by mass based on the mass of the resulting film) and inert fine particles B 4 with an average particle size of 0.1 m and a relative standard deviation of 0. 17.
- inert fine particles A4 0.3 parts by mass of spherical silicone resin particles having an average particle size of 1.3 mm, a relative standard deviation of 0.14, and a particle size ratio of 1.10 (based on the mass of the resulting film)
- the biaxially stretched film having a thickness of 3.0 m was obtained in the same manner as in Example 33 except that 0.3 wt. Table 4 shows the properties of the film.
- Example 3 3 and Examples 3 8 to 4 5 knowledge regarding the aspect of the inert fine particle A 4 and the aspect of the inert fine particle B 4 can be obtained.
- a biaxially stretched film having a thickness of 3.0 m was obtained in the same manner as in Example 33 except that the film forming conditions were as shown in Table 4. Table 4 shows the properties of the obtained film. Comparative Example 1 0
- Example 3 in order to obtain a film having a refractive index in the thickness direction of approximately 1 ⁇ 65 5 80 except that the film forming conditions such as the stretching ratio in the longitudinal direction and the transverse direction were as shown in Table 4.
- the film forming conditions such as the stretching ratio in the longitudinal direction and the transverse direction were as shown in Table 4.
- the films obtained in Examples 3 3 and 4 6 have an appropriate refractive index in the thickness direction, the stretchability and the winding property are good, the dielectric breakdown voltage is high, and the capacitor insulator Therefore, it was suitable.
- Comparative Example 9 the film obtained in Comparative Example 9 was inferior in winding property and dielectric breakdown voltage because the draw ratio was low and the refractive index in the thickness direction of the film was too low.
- Comparative Example 10 the intended refractive index in the thickness direction was too high, and a film could not be obtained.
- Antioxidant C 2 N, N '—bis [3— (3,5-di-tert-butyl-4-hydroxyphenyl) propionyl] hydrazine (I RGANOX 1024)
- Antioxidant C1 Pentaerythritol tetrakis [3— (3,5-Di-tert-butyl-4-hydroxyphenyl) propionate] (I RG ANOX 1010)
- Antioxidant C2 N, N '— Bis [3— (3, 5_di-t-petituyl 4-hydroxyphenyl) propionyl] hydrazine (I RGANOX 1024)
- Antioxidant C I Penn erythritol tetrakis [3— (3,5-Di-tert-butyl-4-hydroxyphenyl) propionate]
- Antioxidant C 2 N, N '— Bis [3— (3, 5-Di-t-butyl-4-hydroxyphenyl) propionyl] hydrazine (I RGA NOX 1024)
- Antioxidant C 1 Penyu Erythritol Tetrakis [3— (3, 5—G t
- Antioxidant C 2 N, N '—Bis [3— (3, 5—Di-t 1-Petiru 4-Hydroxyphenyl) Propionyl] Hydrazine (I RGANOX 1024) Using the obtained film, a capacitor was prepared as follows.
- Example 3 A film capacitor using the film obtained in 2 to 46 was excellent in heat resistance and withstand voltage characteristics and exhibited excellent performance as a capacitor. In addition, it was excellent in processability when making capacitors.
- the film capacitors using the films obtained in Examples 3 3, 3 4, 3 8, 40 to 4 2, 4 5, 4 6 are particularly excellent in withstand voltage characteristics and more excellent performance as a capacitor. It was to show.
- the invention's effect is particularly excellent in withstand voltage characteristics and more excellent performance as a capacitor. It was to show. The invention's effect
- the insulating film of the present invention has a high dielectric breakdown voltage and excellent electrical characteristics.
- the insulating film of the present invention has a low heat shrinkage rate, a high dielectric breakdown voltage at a high temperature, and excellent heat resistance.
- the insulating film of the present invention is excellent in winding property, has a good roll winding shape, and is good with little end face displacement.
- the insulating film of the present invention can be suitably used as an insulator for a capacitor.
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Abstract
Description
Claims
Priority Applications (5)
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US12/665,618 US8859087B2 (en) | 2007-06-21 | 2008-06-19 | Insulating film |
EP20080765839 EP2163573B1 (en) | 2007-06-21 | 2008-06-19 | Insulating film |
CN2008800210271A CN101679653B (zh) | 2007-06-21 | 2008-06-19 | 绝缘性膜 |
AT08765839T ATE551705T1 (de) | 2007-06-21 | 2008-06-19 | Isolierfolie |
KR1020097024779A KR101484797B1 (ko) | 2007-06-21 | 2008-06-19 | 절연성 필름 |
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JP2007163566A JP5249531B2 (ja) | 2007-06-21 | 2007-06-21 | 高絶縁性フィルム |
JP2007231687A JP5378667B2 (ja) | 2007-09-06 | 2007-09-06 | 高絶縁性フィルム |
JP2007-231687 | 2007-09-06 | ||
JP2007-271356 | 2007-10-18 | ||
JP2007271356A JP5587534B2 (ja) | 2007-10-18 | 2007-10-18 | 高絶縁性フィルム |
JP2008-086358 | 2008-03-28 | ||
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WO2011065585A1 (ja) * | 2009-11-30 | 2011-06-03 | 帝人株式会社 | 高絶縁性フィルム |
WO2012147777A1 (ja) * | 2011-04-26 | 2012-11-01 | 帝人株式会社 | 高絶縁性フィルム |
JP2012229340A (ja) * | 2011-04-26 | 2012-11-22 | Teijin Ltd | 高絶縁性フィルム |
JP2012246372A (ja) * | 2011-05-26 | 2012-12-13 | Teijin Ltd | 高絶縁性フィルム |
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JP2015021017A (ja) * | 2013-07-16 | 2015-02-02 | 倉敷紡績株式会社 | ポリスチレン系フィルムおよびその製造方法 |
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US9754721B2 (en) | 2009-10-28 | 2017-09-05 | Teijin Dupont Films Japan Limited | Biaxially oriented film for electrical insulation and film capacitor made using biaxially oriented film for electrical insulation |
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CN102985153B (zh) * | 2010-06-16 | 2015-02-11 | 日东电工株式会社 | 防水透气过滤器及其用途 |
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KR102302155B1 (ko) | 2017-01-25 | 2021-09-14 | 가부시끼가이샤 구레하 | 불화 비닐리덴계 수지 필름 |
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KR20220002595A (ko) | 2019-04-30 | 2022-01-06 | 사빅 글로벌 테크놀러지스 비.브이. | 열가소성 다층 물품, 제조 방법, 및 이의 용도 |
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KR101781662B1 (ko) * | 2009-10-28 | 2017-09-25 | 데이진 필름 솔루션스 가부시키가이샤 | 전기 절연용 2 축 배향 필름 및 전기 절연용 2 축 배향 필름을 사용하여 이루어지는 필름 콘덴서 |
US9754721B2 (en) | 2009-10-28 | 2017-09-05 | Teijin Dupont Films Japan Limited | Biaxially oriented film for electrical insulation and film capacitor made using biaxially oriented film for electrical insulation |
JP2011093984A (ja) * | 2009-10-28 | 2011-05-12 | Teijin Dupont Films Japan Ltd | 電気絶縁用二軸配向フィルム |
CN102712770B (zh) * | 2009-11-30 | 2016-03-02 | 帝人株式会社 | 高绝缘性膜 |
WO2011065585A1 (ja) * | 2009-11-30 | 2011-06-03 | 帝人株式会社 | 高絶縁性フィルム |
JP2011111592A (ja) * | 2009-11-30 | 2011-06-09 | Teijin Ltd | 高絶縁性フィルム |
CN102712770A (zh) * | 2009-11-30 | 2012-10-03 | 帝人株式会社 | 高绝缘性膜 |
US10438746B2 (en) | 2009-11-30 | 2019-10-08 | Teijin Limited | Insulating film |
EP2508553A4 (en) * | 2009-11-30 | 2016-06-29 | Teijin Ltd | HIGH-INSULATING LAYER |
US9617407B2 (en) | 2011-04-26 | 2017-04-11 | Teijin Limited | Highly insulating film |
JP2012229340A (ja) * | 2011-04-26 | 2012-11-22 | Teijin Ltd | 高絶縁性フィルム |
WO2012147777A1 (ja) * | 2011-04-26 | 2012-11-01 | 帝人株式会社 | 高絶縁性フィルム |
JP2012246372A (ja) * | 2011-05-26 | 2012-12-13 | Teijin Ltd | 高絶縁性フィルム |
JP2015021017A (ja) * | 2013-07-16 | 2015-02-02 | 倉敷紡績株式会社 | ポリスチレン系フィルムおよびその製造方法 |
JP2013241626A (ja) * | 2013-08-30 | 2013-12-05 | Teijin Ltd | 高絶縁性フィルム |
WO2016080356A1 (ja) * | 2014-11-18 | 2016-05-26 | 帝人株式会社 | 配向フィルム |
JPWO2016080356A1 (ja) * | 2014-11-18 | 2017-07-27 | 帝人株式会社 | 配向フィルム |
Also Published As
Publication number | Publication date |
---|---|
KR101484797B1 (ko) | 2015-01-20 |
CN101679653B (zh) | 2012-07-04 |
EP2163573B1 (en) | 2012-03-28 |
KR20100023831A (ko) | 2010-03-04 |
EP2163573A4 (en) | 2010-07-14 |
EP2434505A1 (en) | 2012-03-28 |
US20100178483A1 (en) | 2010-07-15 |
US8859087B2 (en) | 2014-10-14 |
EP2434505B1 (en) | 2013-08-21 |
CN101679653A (zh) | 2010-03-24 |
ATE551705T1 (de) | 2012-04-15 |
TW200916485A (en) | 2009-04-16 |
EP2163573A1 (en) | 2010-03-17 |
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