WO2004084242A1 - 扁平型コンデンサ用ポリプロピレンフィルム及びそれからなる扁平型コンデンサ - Google Patents
扁平型コンデンサ用ポリプロピレンフィルム及びそれからなる扁平型コンデンサ Download PDFInfo
- Publication number
- WO2004084242A1 WO2004084242A1 PCT/JP2004/003473 JP2004003473W WO2004084242A1 WO 2004084242 A1 WO2004084242 A1 WO 2004084242A1 JP 2004003473 W JP2004003473 W JP 2004003473W WO 2004084242 A1 WO2004084242 A1 WO 2004084242A1
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- WO
- WIPO (PCT)
- Prior art keywords
- film
- flat
- capacitor
- polypropylene film
- type capacitor
- Prior art date
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- 239000003990 capacitor Substances 0.000 title claims abstract description 155
- -1 polypropylene Polymers 0.000 title claims abstract description 109
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 106
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 claims abstract description 62
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 11
- 238000001465 metallisation Methods 0.000 claims description 10
- 229920000306 polymethylpentene Polymers 0.000 claims description 3
- 239000011116 polymethylpentene Substances 0.000 claims description 3
- 239000010408 film Substances 0.000 description 190
- 230000037303 wrinkles Effects 0.000 description 48
- 238000001816 cooling Methods 0.000 description 20
- 238000004804 winding Methods 0.000 description 14
- 238000003851 corona treatment Methods 0.000 description 12
- 238000011084 recovery Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 230000006378 damage Effects 0.000 description 10
- 238000005259 measurement Methods 0.000 description 10
- 229920000642 polymer Polymers 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 230000007423 decrease Effects 0.000 description 5
- 208000028659 discharge Diseases 0.000 description 5
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 4
- 239000002985 plastic film Substances 0.000 description 4
- 229920006255 plastic film Polymers 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000001771 vacuum deposition Methods 0.000 description 4
- 238000007740 vapor deposition Methods 0.000 description 4
- 239000004711 α-olefin Substances 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 229920001519 homopolymer Polymers 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002667 nucleating agent Substances 0.000 description 3
- 238000007738 vacuum evaporation Methods 0.000 description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000011104 metalized film Substances 0.000 description 2
- 229920001083 polybutene Polymers 0.000 description 2
- 229920006267 polyester film Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 239000011135 tin Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 208000037062 Polyps Diseases 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920005606 polypropylene copolymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
- H01G4/18—Organic dielectrics of synthetic material, e.g. derivatives of cellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
Definitions
- the present invention relates to a flat-type capacitor polypropylene film and a flat-type capacitor made of the same, and more particularly to a flat-type capacitor intended for use under a small-sized, large-capacity, high-rated voltage, and a polypropylene film for forming the flat-type capacitor. Is what you do.
- Polypropylene films are widely used in electrical applications because their electrical properties, such as withstand voltage and dielectric loss, are superior to other plastic films. Above all, the demand for dielectric materials for capacitor applications has grown remarkably. Recently, as various types of electrical equipment have been converted to inverters, and as condensers have become smaller and larger in capacity, the demand for thinner polypropylene films has been increasing.
- polypropylene film is a material with poor rigidity among plastic films used for capacitors, as its thickness becomes thinner, there is a growing demand for improved handling and workability. For this reason, various proposals have been made to improve handling and workability.
- the coefficient of static friction at 80 ° C between a non-deposited surface after metal deposition on one surface of a polypropylene film and a metal plate provided with chrome plating is 0.8 or less, and the melting point is 13
- a vapor-deposited polypropylene film for a capacitor in which the content of an additive at 0 ° C or less is 40000 ppm by weight or less has been proposed, and it is known that the vapor-depositing processability is improved (for example, see Japanese Unexamined Patent Publication No. No. 1,704,006).
- a method in which a non-evaporated surface is subjected to a surface treatment with a wet tension of 33 dyne / cm or less to impart high-speed winding property (for example, Japanese Patent Application Laid-Open No. 58-16415). ). Further, F 5 value is one tooth 0 kgf / mm 2 or more, the total particle-containing organic content in the film is 0.2 5 to 0.6 0 Polyester film is a weight% is proposed, winding resistance, scan Li Tsu It is known to improve the stability (for example, Japanese Patent Application Laid-Open No. 2000-204177).
- the difference between the film thickness by the micrometer method and the film thickness by the weight method There is known a method of suppressing a decrease in withstand voltage and insulation defects of a film by setting 3 to 0.01 to 0.5 wm (see, for example, Japanese Patent Application Laid-Open No. H10-1566938). Furthermore, the ratio MMV / WMV of the micrometer thickness (MMV) to the weight average thickness (WMV) is set to 1.2 to 1.6, and the interlaminar flow of the insulating oil at the time of film wrapping is determined. (For example, Japanese Patent Application Laid-Open No. 2001-118430) However, a vapor-deposited polypropylene film for a capacitor described in Japanese Patent Application Laid-Open No. 2-170406.
- the effect of suppressing winding deviation in the winding process of the capacitor element was small and insufficient.
- the effect of suppressing wrinkles in the winding process is unsatisfactory, especially for thin films with a thickness of 4 or less.
- the film described in Japanese Patent Application Laid-Open No. 2000-204177 is a polyester film, and it is difficult to apply it to a polypropylene film due to the difference in the polymer properties and the like. Was.
- an object of the present invention is to overcome the drawbacks of the conventional technology and to generate wrinkles and misalignments even in a thin polypropylene film of, for example, 4 m or less in a winding process of a capacitor element and a subsequent flattening press process.
- it is suitable for making large-capacity and small flat capacitors of 50 O w F or more, while maintaining the withstand voltage characteristics, especially self-healing which is one of the characteristics of flat capacitors.
- Suitable for use with a DC rated voltage of 700 V or more SUMMARY OF THE INVENTION It is an object of the present invention to provide a lum and a flat type capacitor made thereof.
- a difference ⁇ d between the thickness of the film by a micrometer method and the thickness by a mass method is 0.05 to 0.2 m.
- the rate of change of shrinkage dimension in the length direction is 3% or less.
- another flat-type capacitor polypropylene film according to the present invention has a difference d between a thickness of the film measured by a micrometer method and a thickness measured by a mass method of 0.1 to 0.3 wm, and a length direction of the film. F5 value of 50 MPa or more.
- the present invention also provides a metallized polypropylene film for a flat type capacitor, wherein a metal is deposited on one or both sides of the above-mentioned flat type polypropylene film for a capacitor.
- the flat type capacitor according to the present invention comprises at least a part of the flat type capacitor-use polypropylene film as described above. Further, the flat type capacitor according to the present invention is formed by using at least a part of the metallized polypropylene film for a flat type capacitor as described above.
- FIG. 1 is a schematic plan view showing an example of a pattern including a magazine that is not parallel to the length direction of the metallized polypropylene film for a flat capacitor.
- FIG. 2 is a schematic plan view showing another example of a pattern including a margin that is not parallel to the length direction of the metallized polypropylene film for a flat capacitor.
- Ad of the film is not less than 0.05111 and not more than 0.2 wm.
- Ad is the thickness measured by the micrometer method (MMV) minus the thickness measured by the mass method (WMV). If the value is large, it means that the film surface is rough, and the porosity between the film layers when wound on a capacitor element is large, and if it is small, the film surface is smooth. This means that the porosity between the film layers when wound up on the capacitor element is reduced.
- the Ad of the film is less than 0.05 m, the film becomes difficult to slip, which causes a problem in film processing that a wrinkle suppressing effect cannot be obtained.
- the porosity between the film layers in the capacitor decreases, self-recovery in the capacitor prevents gas and scattered metal from leaking out of the system and impairs withstand voltage characteristics. It is unsuitable because it generates.
- ⁇ d is more than 0.2, there will be a problem with the workability of the film such as the film being displaced when the capacitor element is wound up, and the internal discharge will be reduced due to an increase in the porosity between the films in the capacitor.
- the capacitor is charged and a decrease in the withstand voltage of the capacitor.
- it is not less than 0. 07 u m and not more than 0.15 u m.
- Examples of the method for adjusting the ⁇ d of the flat-type capacitor polypropylene film according to the present invention to the above range include a method of controlling the polymer temperature at the time when the polymer extruded from the extruder is cooled and solidified by the cooling roll, Examples include a method of selecting a polymer having excellent crystallinity and a method of including a nucleating agent such as polypropylene.
- the shrinkage dimension change rate in the length direction of the polypropylene film for a flat capacitor according to the present invention needs to be 3% or less. If it exceeds 3%, the film shrinks greatly in the capacitor manufacturing process such as heat treatment of the capacitor element, and the film closes in the capacitor and reduces the film layer, so the gas generated when self-recovery occurs It is not suitable because it causes troubles such as impeding the withstand voltage characteristics without scattered metal coming out of the system.
- the rate of change in shrinkage dimension in the length direction of the flat type polypropylene film for a capacitor according to the present invention is too small, the capacitor element is rolled up on the capacitor element and then subjected to the heat history received during the capacitor manufacturing and use processes. May loosen and the porosity between film layers may change. Therefore, the content is preferably 0.5% or more and 2.8% or less, and more preferably 1.0% or more and 2.5% or less.
- the sum of the shrinkage dimensional change in the length direction and the shrinkage dimensional ratio in the width direction of the polypropylene film for a flat capacitor according to the present invention is preferably 4% or less, more preferably 0.5% or more. . 5 or less is 0/0. Within this range, shrinkage of the film can be suppressed in a process subjected to thermal stress such as a vapor deposition heating press, so that desired dimensional accuracy and capacity accuracy can be obtained. Further, the ten-point average roughness Rz of at least one surface of the flat-type capacitor polypropylene film according to the present invention is preferably 0.6 wm or less.
- Rz of the surface intended for metal deposition exceeds 0.6 wm, it functions as a capacitor electrode.
- the deposited metal surface has coarse irregularities, causing concentration of an electric field and degrading withstand voltage characteristics. Therefore, it is preferable that Rz of the surface for the purpose of metal deposition is 0.6 um or less. More preferably, it is 0.5 m or less.
- the lower limit of Rz is not particularly limited as long as the effects of the present invention are exerted, but is preferably 0.1 m or more in order to properly maintain the slip property of the film.
- the polypropylene film for a flat type capacitor according to the present invention uses polymethylpentene in view of the effect of imparting slipperiness and economy in order to prevent rigidity from decreasing as the thickness becomes thinner and to prevent slippage.
- the content is preferably 0.5 wt% to 5 wt%, and more preferably the content is in the range of 0.7 wt% to 4 wt%.
- the thickness of the polypropylene film in the present invention is not particularly limited, but a thin film having poor rigidity tends to wrinkle easily. The following films are particularly effective and suitable.
- the polymer composing the polypropylene film for a flat type capacitor according to the present invention is not particularly limited.
- a copolymer of propylene and another ⁇ -olefin eg, ethylene, butene, etc.
- a blended product of polypropylene and another ⁇ -olefin polymer eg, polyethylene, polybutene, etc. may be used.
- the flat type capacitor-use polypropylene film according to the present invention may be a tenter.
- the stretching method is not particularly limited. However, since it is required to be thin and small in thickness unevenness, the biaxial stretching by the center method is required. preferable.
- the additives contained in the flat-type capacitor polypropylene film according to the present invention are not particularly limited, and may be appropriately selected and added as long as they do not affect the capacitor characteristics.
- the electrode when the flat type polypropylene film for a capacitor according to the present invention is used for a condenser is not particularly limited.
- the present invention One side or both sides of the polypropylene film may be directly metallized, but it is particularly suitable for directly metallizing the film in capacitor applications where reduction in size and weight is desired.
- the kind of metal used includes, but is not particularly limited to, a simple substance such as zinc, tin, silver, chromium, aluminum, copper, and nickel, or a mixture or alloy of plural kinds. .
- Examples of the method of directly metallizing a film include a vacuum evaporation method and a sputtering method, and are not particularly limited. However, from the viewpoint of productivity and economy, the vacuum evaporation method is more preferable. preferable. In general, a crucible-type wire system or the like is exemplified as the vacuum evaporation method, but is not particularly limited and may be appropriately selected.
- the margin pattern in the case of metallization by vapor deposition is not particularly limited, and may be an ordinary butterfly pattern or a special margin pattern applied for the purpose of improving the security of the capacitor. .
- the metal surface and the film surface alternately come into contact with various rolls, so that the state of friction with the rolls is not constant, which tends to lead to defects such as wrinkles.
- a method including a margin portion 2 that is not parallel to the film length direction with respect to the metallized portion 1 as exemplified in FIG. 1 and FIG. 2 these problems can be reduced, which is preferable.
- the method of forming these margins is not particularly limited. For example, a tape method or an oil method may be used.
- the capacitor made of the polypropylene film according to the present invention is used for a flat type condenser that goes through a flattening press step that is easily wrinkled.
- a method for producing a polypropylene film according to the present invention as described above is shown, but is not particularly limited.
- the min.polypropylene resin is supplied to an extruder at a temperature of 240 to 270 ° C and melted, extruded in a sheet form from a slit T die, and heated to a temperature of 75 to 95 ° C. And cooled and solidified by a cooling roll.
- the higher the cooling roll temperature the greater the surface roughness.Therefore, in order to obtain a desired ⁇ d, the cooling roll temperature may be appropriately selected. preferable.
- the film is stretched 3 to 7 times in the length direction by a stretching roll at 135 to 150 ° C. Also in this case, the size of the surface roughness can be changed by selecting the stretching temperature. Then, it is stretched 7 to 12 times in the width direction at a temperature of 150 to 170 ° C., and further subjected to a heat treatment at 150 to 165 t. In general, the lower the stretching temperature or heat treatment temperature and the higher the stretching ratio, the larger the shrinkage dimensional change ratio. Therefore, these conditions may be appropriately selected. After one side of the thus obtained polypropylene film is subjected to corona discharge treatment, it is wound up with a winder.
- the film has a thickness d of 0.1 to 0.3 wm.
- Ad is the difference between the thickness measured by the micrometer method and the thickness measured by the mass method, as described above.If this value is large, it means that the film surface is rough.
- the porosity between the film layers when wound up on the capacitor element increases, and when it is small, it means that the film surface is smooth, and the porosity between the film layers when wound up on the capacitor element decreases.
- the capacity becomes smaller with the lapse of time when power is applied to the capacitor due to the fact that it becomes easier, causing problems such as lowering the withstand voltage of the capacitor.
- it is in the range of 0.15 to 0.25 ⁇ m.
- a method for setting the d of the flat type capacitor polypropylene film according to the present invention as described above within the above range a method of controlling the polymer temperature when the polymer extruded from the extruder is cooled and solidified by the cooling roll is used. And a method of selecting a polymer having appropriate crystallinity, or a method of including a nucleating agent such as an iS nucleating agent.
- the F5 value in the length direction of the polypropylene film for a flat capacitor according to the present invention needs to be 50 MPa or more. If the pressure is lower than 50 MPa, the film may be broken when processing the film, or may have poor winding properties such as wrinkling when winding the capacitor element, and may be resistant to wrinkling during winding and air entrapment. It is inappropriate because it causes problems such as impairing the voltage characteristics. Preferably it is 55 MPa or more.
- At least one surface of the polypropylene film for a flat capacitor according to the present invention has a ten-point average roughness Rz in the range of 0.7 to 1.4 wm. If Rz is less than 0.7 wm, the gas and scattered metal generated when self-recovery occurs in the capacitor will not be sufficiently released even if the film satisfies ⁇ d, and the withstand voltage characteristics will be poor. Rz is preferably 0.7 m or more, more preferably 0.9 um or more, because it may lower the value.
- Rz of the surface for metal deposition exceeds 1.4 m, the surface of the deposited metal that functions as the capacitor electrode will have coarse concaves and convexes, causing electric field concentration and degrading withstand voltage characteristics. Therefore, it is preferable that Rz of the surface for the purpose of metal deposition be 1.4 or less. Than Preferably it is 1.2 or less.
- the thickness of the flat-type capacitor polypropylene film according to the present invention is not particularly limited. However, a thin film having poor rigidity tends to cause wrinkle film breakage. A film having a meter thickness of 4 ⁇ m or less, preferably 3.5 wm or less has a particularly large effect and is suitable.
- the polymer constituting the above-mentioned flat-type capacitor polypropylene film according to the present invention is not particularly limited. In addition to a homopolymer of polypropylene, propylene and other ⁇ -olefins (eg, ethylene, butene, etc.) may be used.
- the melting point is preferably 167 ° C or lower.
- the polypropylene film for a flat capacitor according to the present invention may be obtained by a tenter method or an inflation method, and the stretching method is not particularly limited, but is thin and has small thickness unevenness. Therefore, the biaxial stretching by the tenter method is preferred.
- the additives contained in the flat type capacitor polypropylene film according to the present invention are not particularly limited, and may be appropriately selected and added within a range that does not affect the capacitor characteristics.
- the electrodes are not particularly limited.
- the kind of metal used includes, but is not particularly limited to, a simple substance such as zinc, tin, silver, chromium, aluminum, and copper-nickel, or a mixture or alloy of plural kinds.
- Methods for directly metallizing films include vacuum evaporation and sputtering. Examples include, but are not limited to, a vacuum deposition method from the viewpoints of productivity and economy.
- a vacuum crucible method such as a crucible method or a one-wire method is exemplified, but is not particularly limited, and may be appropriately selected.
- An EB gun method which has a small defect imparting rate, is more preferable.
- the margin pattern in the case of metallization by vapor deposition is not particularly limited either, and may be a normal pattern or a special margin pattern provided for the purpose of improving the security of the capacitor, etc.
- the metal surface and the film surface alternately come into contact with various rolls, so the frictional state with the rolls is not constant, and it is easy to lead to problems such as wrinkles.
- a method including a margin portion 2 is not parallel to the film length direction with respect to metallization 1, since it is possible to reduce these defects, it is preferable (formation of their margin).
- the system is not particularly limited, and may be, for example, a tape system or an oil system.
- the capacitor made of the polypropylene film for a flat type capacitor according to the present invention is used for a flat type capacitor which goes through a flattening press step which is likely to cause wrinkles.
- the 10 min polypropylene resin is fed to an extruder at a temperature of 230-270 t and melted, extruded in a sheet form from a slit T die, and 75-95 ° It is cooled and solidified by a cooling roll at a temperature of C.
- the higher the temperature of the cooling roll the higher the surface roughness.Therefore, in order to obtain a desired Ad, the temperature of the cooling roll may be appropriately selected, and 80 to 95 t is preferable. No.
- the film is stretched 7 to 12 times in the width direction at a temperature of 150 to 170 ° C, and further subjected to a heat treatment at 150 to 165 ° C. Generally, the lower the stretching temperature or heat treatment temperature and the higher the stretching ratio, the greater the F5 value. Therefore, these conditions may be selected as appropriate.
- One side of the thus obtained flat type polypropylene film for a capacitor is subjected to a corona discharge treatment and then wound up with a winder.
- the measurement was performed under the following conditions using a differential scanning calorimeter DSC-7 manufactured by PerkinElmer Co., Ltd.
- MMV thickness by the micrometer method
- ⁇ d ( ⁇ m) MM V -WM V
- Measurement surface treatment Aluminum was vacuum-deposited on the measurement surface, and a non-contact method was used.
- Width feed rate 0.1 mm / sec
- Measurement direction The width direction of the film.
- Polypropylene film is made of ULVAC Co., Ltd. with a vacuum evaporation machine to make aluminum with a film resistance of 5 ⁇ / port, a normal margin metallized film without T-shaped margin, and a combination of the normal margin product, or a film resistance of 15 ⁇ / mouth, creating a T-shaped margin metallized film of the pattern of FIG. 2, in combination with normal margin products not subjected to T-type margins, performs normal capacitor forming process similar winding, capacitive 1 0 0 w F 100 capacitor elements were prepared, and the occurrence rates of wrinkles and deviations were examined.
- the main winding conditions at this time are as follows.
- the self-recovery number was 7 or less and the destruction number was 3 or less.
- the measurement was performed according to VII.4.5 of JISC-233 (200), and the stress when the sample was stretched by 5% was calculated.
- Melt index 3.5 g / 10 min polypropylene resin containing 0.3 wt% of tetrakis [methylene-13 (3,5—j-hydroxybutyl-14-hydroxyhydroxy) propionate] methane is added. It is fed into an extruder at a temperature of 250 ° C, melted, extruded into a sheet from a slit T die, cooled and solidified with a cooling roll at a temperature of 85 ° C, and then cooled to 140 t. Stretched 5 times in the longitudinal direction at the temperature of The film was stretched 10 times in the width direction at a temperature of 167 ° C, and then heat-treated at a temperature of 165 ° C.
- one side of the film was subjected to corona discharge treatment so that the wetting tension was 42 mN / m and wound up with a winder, and then the width was reduced to 62 mm and the length to 400 m. Cut and rolled up.
- the MMV of the film was 3
- the d was 0.10 wm
- the ten-point average roughness Rz of the surface subjected to the corona discharge treatment was 0.4 m
- the ten-point average roughness Rz of the opposite surface was 0.
- This film was vapor-deposited on one side with a capacitor vacuum evaporator so as to have a film resistance of 5 ⁇ / mouth, and then slit into a width of 100 mm and a length of 480 m, and 8 pieces Of reels were collected.
- a polypropylene film was obtained under the same conditions as in Example 1 except that a polymer to which 2.0 wt% of polymethylpentene was added was used.
- the MMV of the film was 3 m
- ⁇ d was 0.11
- the ten-point average roughness Rz of the surface subjected to the corona discharge treatment was 0.4 m
- the ten-point average roughness of the opposite surface was 0.4 m.
- Rz was 0.7 um ⁇
- the shrinkage dimension change rate in the length direction was 2.6%
- the shrinkage dimension change rate in the width direction was 0.2%.
- This film was vapor-deposited on one side with a capacitor vacuum evaporator so as to have a film resistance of 5 ⁇ / port, and then slit to a width of 100 mm and a length of 480 m. A total of 48 reels were collected.
- the film MMV was 3 wm
- Ad was 0.13 // ⁇
- the ten-point average roughness R 0 of the corona-treated surface was 0.5 m
- the ten-point average roughness of the opposite surface was Rz was 0.8 ⁇ m.
- the shrinkage dimension change rate in the length direction was 2.5%
- the shrinkage dimension change rate in the width direction was 0%.
- This film was deposited on one side of the film with a capacitor vacuum evaporator so as to have a film resistance of 5 ⁇ / port, and then slit to a width of 100 mm and a length of 480 m, A book reel was collected.
- the number of self-healing was 5, and the number of destroyed was 1.
- a polypropylene film was obtained under the same conditions as in Example 1 except that the film was cooled and solidified by a cooling roll at a temperature of C.
- the MMV of the film was 3 m
- Ad was 0.06 wm
- the ten-point average roughness Rz of the corona-treated surface was 0.2 m
- the ten-point average roughness Rz of the opposite surface was Was 0.3 ⁇ m
- the shrinkage dimension change rate in the length direction was 2.9%
- the shrinkage dimension change rate in the width direction was 0.5%.
- Aluminum was deposited on one side of the film with a capacitor vacuum evaporator so as to have a film resistance of 5 ⁇ / mouth, and then slit to a width of 100 mm and a length of 480 m, and Reels of books were collected.
- the number of self-recovery was 2, and the number of destruction was 3.
- a polypropylene film was obtained under the same conditions as in Example 1 except that the sheet extruded from the slit T-die was cooled and solidified by a cooling roll at a temperature of 90 ° C.
- the film MMV is 3 wm
- Ad is 0.18 wm
- corona discharge treatment 10-point average roughness R z of the surface subjected to the treatment is 0.6 m
- the 10-point average roughness R z of the opposite surface is 0.9 m
- the shrinkage dimension change rate in the length direction is 2.7%
- the width direction Had a shrinkage dimensional change of 0.1%.
- This film was deposited on one side of the film with a capacitor vacuum evaporator so as to have a film resistance of 5 ⁇ / port, and then slit to a width of 100 mm and a length of 480 m, A book reel was collected.
- the number of self-healing was four and the number of destruction was two.
- the MMV of the film was 3 m
- Ad was 0.09 ⁇ m
- the ten-point average roughness Rz of the corona-treated surface was 0.4 m
- the ten-point average roughness R of the opposite surface was R z is 0.
- shrinkage dimension change rate in the length direction is 3.0%
- shrinkage dimension change rate in the width direction is 0.
- This film was vapor-deposited on one side with a capacitor vacuum evaporator so as to have a film resistance of 5 ⁇ / port, and then slit to a width of 100 mm and a length of 480 m. A total of 48 reels were collected.
- the number of self-recovery was 3, and the number of destruction was 3.
- a polypropylene film was obtained under the same conditions as in Example 1 except that the sheet extruded from the slit T die was cooled and solidified by a cooling roll having a temperature of 70 t.
- the MMV of the film is 3 wm
- the mm d is 0.03 wm
- the ten-point average roughness Rz of the surface subjected to the corona discharge treatment is 0.2 m
- the ten-point average roughness Rz of the opposite surface is Is 0.3 IX m.
- the shrinkage dimension change rate in the length direction is .8%
- the shrinkage dimension change rate in the width direction is 0.3. 3%.
- This film was vapor-deposited on one side with a capacitor vacuum evaporator so as to have a film resistance of 5 ⁇ / mouth, and then slit to a width of 100 mm and a length of 480 Om. Reels of books were collected.
- the number of self-healing was 7, and the number of destroyed was 8.
- a polypropylene film was obtained under the same conditions as in Example 1 except that the sheet extruded from the slit T-die was cooled and solidified by a cooling roll at a temperature of 96.
- the MMV of the film is 3 m
- the Ad is 0.21 um.
- the ten-point average roughness R z of the surface subjected to the corona discharge treatment is 0.7 wm
- the ten-point average roughness R z of the opposite surface is Was 1.2 wm
- the shrinkage dimension change rate in the length direction was 2.5%
- the shrinkage dimension change rate in the width direction was 0.1%.
- This film was vapor-deposited on one side with a capacitor vacuum evaporator so as to have a film resistance of 5 ⁇ / mouth, and then slit to a width of 100 mm and a length of 480 Om. Eight reels were collected.
- the number of self-recovery was 9, and the number of destruction was 6.
- the MMV of the film was 3 wm
- ⁇ d was 0.09 wm
- the ten-point average roughness R z of the corona-treated surface was 0.4 m
- the ten-point average roughness R z of the opposite surface was Was 0.6 rn
- the shrinkage dimension change rate in the length direction was 3.4%
- the shrinkage dimension change rate in the width direction was 0.8%.
- This film was converted to aluminum with a vacuum evaporation machine for capacitors of 5 ⁇ / film resistance. Then, it was slit to a width of 100 mm and a length of 480 m, and 48 reels were collected.
- the number of self-recovery was 5, and the number of destruction was 6.
- Tetrakis [methylene-1 3 (3,5—dibutyl-butyl-4—hydroxyphenyl) propionate] methane (Ciba Specialty 'Irganoxl Ol O, manufactured by Chemical Co., Ltd.) Melt index added with wt% 3.7 g / 10 min, polypropylene resin with a melting point of 166 ° C was supplied to an extruder at a temperature of 240 t to melt and slit the T-die. After being extruded into a sheet form, cooled and solidified by a cooling roll at a temperature of 90 t, stretched 5 times in the length direction at a temperature of 140 t, and then stretched in a width direction at a temperature of 16 ° C.
- the film was stretched 10 times, and then heat-treated at a temperature of 15 Ot. After that, one side of the film was subjected to a corona discharge treatment so that the wetting tension was 42 mN / m, and a 500 mm wide film was wound with a winder, and then a width of 600 mm was applied. mm. It was cut to a length of 400 m and wound up.
- the MMV of the film was 3.3 m
- ⁇ d was 0.20 wm
- the ten-point average roughness Rz of the corona-discharge treated surface was 1.0 m
- the ten-point average roughness of the opposite surface was The Rz was 1.1
- the F5 value in the length direction was 52 MPa.
- This film was vapor-deposited on one side with a T-shaped pattern shown in Fig. 2 using a vacuum vapor deposition machine for capacitors so as to have a film resistance of 15 ⁇ / port, and then a width of 100 mm and a length of 100 mm. It was slit to 480 m and 480 reels were collected. The width of the margin in the longitudinal direction was 0.7 mm, and a margin of 0.4 mm was provided in the width direction at 16 mm intervals. In addition, normal margin products were collected in the same manner. 100 capacitor elements were prepared by combining the T-type magazine product and the normal magazine product, and the occurrence rates of wrinkles and deviations were examined. The wrinkling rate was 2% and the slip rate was 1%.
- Example 8 Melt index 3.2 g / 10 min, polypropylene resin with a melting point of 166 ° C was supplied to an extruder at a temperature of 250 ° C, melted, and cut through a slit T die.
- a polypropylene film was obtained under the same conditions as in Example 7 except that the film was extruded in the shape of a triangle.
- the MMV of the film was 3.2 m.
- Ad was 0.19 m
- the ten-point average roughness Rz of the corona-discharge treated surface was 1.0 m
- the ten-point average roughness of the opposite surface was Rz was 1.0 m
- F5 value in the length direction was 57 MPa.
- This film was deposited under the same conditions as in Example 7, and then slit to a width of 100 mm and a length of 480 m, and 48 reels were collected.
- a polypropylene film was obtained under the same conditions as in Example 7 except that the sheet extruded from the slit T-die was cooled and solidified by a cooling roll at a temperature of 87 ° C.
- the MMV of the film is 3.2 m.
- ⁇ d is 0.12 .a m.
- the ten-point average roughness R z of the corona-discharge treated surface is 0.8 im, and the ten-point average of the opposite surface is Roughness R z
- This film was deposited under the same conditions as in Example 7 and then 100 mm wide and 4 mm long.
- a polypropylene film was obtained under the same conditions as in Example 7, except that the sheet extruded from the slit T die was cooled and solidified by a cooling roll having a temperature of 93.
- the MMV of the film was 3.3 m
- Ad was 0.27 / m
- the ten-point average roughness Rz of the corona-treated surface was 1.2 m
- the ten-point average of the opposite surface was The roughness Rz was 1.2 wm
- the F5 value in the length direction was 52 MPa.
- This film was deposited under the same conditions as in Example 7, and then slit to a width of 100 mm and a length of 480 m to collect 48 reels.
- 100 capacitor elements were prepared by combining the T-type margin product and the normal margin product, and the occurrence rates of wrinkles and deviations were examined.
- the wrinkling rate was 1%, and the slip rate was 4%.
- Example 7 Same as Example 7 except that the sheet extruded from the slit T die was cooled and solidified by a cooling roll at a temperature of 91, and then stretched 5 times in the length direction at a temperature of 138 ° C. A polypropylene film was obtained under the same conditions.
- the MMV of the film was 3.2 m
- ⁇ d was 0.119 m
- the ten-point average roughness Rz of the surface subjected to corona discharge treatment was 0.7 m
- the ten-point average roughness of the opposite surface was R z
- F5 value in the longitudinal direction was 55 MPa.
- This film was deposited under the same conditions as in Example 7 and then 100 mm in width and 4 mm in length
- the sheet extruded from the slit T-die was cooled and solidified with a cooling roll at a temperature of 89 ° C, and then stretched 5 times in the length direction at a temperature of 1336 ° C.
- a polypropylene film was obtained under the same conditions as in Example 7, except that the film was stretched 10 times in the width direction at a temperature of 5 ° C, and then heat-treated at a temperature of 160 ° C. At this time, the MMV of the film was 3.2 ⁇ m.
- Ad was 0.18 wm
- the ten-point average roughness Rz of the corona-treated surface was 0.8 m
- the ten-point average roughness of the opposite surface was The Rz was 0.8 m
- the F5 value in the length direction was 55 MPa.
- This film was deposited under the same conditions as in Example 7, then slit into a width of 100 mm and a length of 480 m, and collected 48 reels.
- a polypropylene film was obtained under the same conditions as in Example 7, except that the sheet extruded from the slit T die was cooled and solidified with a cooling roll having a temperature of 83 t.
- the MMV of the film was 3.2 m
- ⁇ d was 0.77 m
- the ten-point average roughness Rz of the corona-treated surface was 0.5 m
- the ten-point average roughness of the opposite surface was R z was 0.6 ⁇ m
- F 5 value in the length direction was 52 MPa.
- This film was deposited under the same conditions as in Example 7, then slit into a width of 100 mm and a length of 480 m, and collected 48 reels.
- 100 capacitor elements were prepared by combining the T-type margin product and the normal margin product, and the occurrence rates of wrinkles and deviations were examined.
- the wrinkling rate was 7% and the slip rate was 0%.
- Example 1 Except that the sheet extruded from the slit T die was cooled and solidified in a cooling hole at a temperature of 97 t, and then stretched 5 times in the length direction at a temperature of 142 ° C. A polypropylene film was obtained under the same conditions as in 7.
- the MMV of the film is 3.3 wm, AcH O .35 m, the ten-point average roughness Rz of the surface subjected to corona discharge treatment is 1.5 m, and the ten-point average roughness of the opposite surface is R z
- the F5 value in the longitudinal direction was 1.6 MPa.
- This film was deposited under the same conditions as in Example 7, and then slit into a width of 100 mm and a length of 480 m to collect 48 reels.
- This film was deposited under the same conditions as in Example 7, and then slit into a width of 100 mm and a length of 480 m, and 48 reels were collected.
- 100 capacitor elements were prepared by combining the T-type margin product and the normal margin product, and the occurrence rates of wrinkles and deviations were examined.
- the wrinkle occurrence rate was 11% and the shift occurrence rate was 1%.
- Example 1 ⁇ Example 2 ⁇ Example 3 ⁇ ; Example 4 ⁇ Example 5 ⁇ Example 6 Comparison My meter thickness (/ m 3 3 3 3 3 3 m d (m) 0.1 ⁇ 0 1 1 0 1 3 0. 0 6 0. 1 8 0. 0 9 0. Shrinkage dimension ratio Length direction 2 7 2. 6 2 5 2. 9 2. 7 3. 0 2. (%)
- Width direction 0.3 0. 2 0 0 5 0. 1 0.7.
- Example 7 Example 7 ⁇ Example 8 ⁇ Example 9
- Example 10 Example 11 ⁇ Example 12 Comparative Example 4 Comparative Example 5 Comparative Example 6
- Micrometer thickness m 3.3 3.2 3.2 3. 3 3.2 3.2 .2 3 3 3 .2 m d ( ⁇ m) 0 .2 0 0 .1 9 0 .1 2 0 .2 7 0 .1 9 0 .1 8 0 .0 7 0 . 3 5 0. 2 0
- the flat-type capacitor polypropylene film of the present invention and the flat-type capacitor made of the same are particularly suitable for a flat-type capacitor intended for use at a high rated voltage for the purpose of miniaturization and large capacity.
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Abstract
Description
Claims
Priority Applications (4)
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JP2005503690A JPWO2004084242A1 (ja) | 2003-03-19 | 2004-03-16 | 扁平型コンデンサ用ポリプロピレンフィルム及びそれからなる扁平型コンデンサ |
EP04720977A EP1607990A4 (en) | 2003-03-19 | 2004-03-16 | FLAT CAPACITOR USE POLYPROPYLENE FILM AND FLAT CONDENSER THEREWITH |
US10/548,820 US7405920B2 (en) | 2003-03-19 | 2004-03-16 | Flat type capacitor-use polypropylene film and flat type capacitor using it |
KR1020057017508A KR101117537B1 (ko) | 2003-03-19 | 2005-09-16 | 편평형 콘덴서용 폴리프로필렌 필름 및 그것으로이루어지는 편평형 콘덴서 |
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JP2004356208A (ja) * | 2003-05-27 | 2004-12-16 | Shinetsu Film Kk | オールフィルム製電子レンジ用油浸コンデンサーおよびその製造方法 |
-
2004
- 2004-03-16 US US10/548,820 patent/US7405920B2/en active Active
- 2004-03-16 WO PCT/JP2004/003473 patent/WO2004084242A1/ja active Application Filing
- 2004-03-16 EP EP04720977A patent/EP1607990A4/en not_active Withdrawn
- 2004-03-16 JP JP2005503690A patent/JPWO2004084242A1/ja active Pending
-
2005
- 2005-09-16 KR KR1020057017508A patent/KR101117537B1/ko active IP Right Grant
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1298527C (zh) * | 2004-12-31 | 2007-02-07 | 浙江南洋电子薄膜有限公司 | 适用于大功率电容器的耐高温双向拉伸聚丙烯膜及其制作方法 |
JP2007290380A (ja) * | 2006-03-28 | 2007-11-08 | Toray Ind Inc | 金属化二軸配向ポリプロピレンフィルム及びこれからなるコンデンサ |
WO2015072291A1 (ja) | 2013-11-14 | 2015-05-21 | 東レ株式会社 | 二軸配向ポリプロピレンフィルムおよびその製造方法 |
KR20160086327A (ko) | 2013-11-14 | 2016-07-19 | 도레이 카부시키가이샤 | 2축 배향 폴리프로필렌 필름 및 그의 제조 방법 |
JP2015146374A (ja) * | 2014-02-03 | 2015-08-13 | 王子ホールディングス株式会社 | コンデンサ素子の製造方法 |
KR20160138108A (ko) | 2014-03-28 | 2016-12-02 | 도레이 카부시키가이샤 | 2축 배향 폴리프로필렌 필름 |
JP2018125547A (ja) * | 2018-03-22 | 2018-08-09 | 王子ホールディングス株式会社 | コンデンサ素子の製造方法 |
JP2020124906A (ja) * | 2018-08-29 | 2020-08-20 | 王子ホールディングス株式会社 | 金属層一体型ポリプロピレンフィルム、フィルムコンデンサ、及び、金属層一体型ポリプロピレンフィルムの製造方法 |
JP7256960B2 (ja) | 2018-08-29 | 2023-04-13 | 王子ホールディングス株式会社 | 金属層一体型ポリプロピレンフィルムの製造方法 |
JP2020124905A (ja) * | 2018-09-05 | 2020-08-20 | 王子ホールディングス株式会社 | 金属層一体型ポリプロピレンフィルム、フィルムコンデンサ、及び、金属層一体型ポリプロピレンフィルムの製造方法 |
JP7228132B2 (ja) | 2018-09-05 | 2023-02-24 | 王子ホールディングス株式会社 | 金属層一体型ポリプロピレンフィルム、フィルムコンデンサ、及び、金属層一体型ポリプロピレンフィルムの製造方法 |
Also Published As
Publication number | Publication date |
---|---|
JPWO2004084242A1 (ja) | 2006-06-29 |
KR101117537B1 (ko) | 2012-03-08 |
EP1607990A4 (en) | 2009-11-25 |
EP1607990A1 (en) | 2005-12-21 |
KR20050113655A (ko) | 2005-12-02 |
US20060171100A1 (en) | 2006-08-03 |
US7405920B2 (en) | 2008-07-29 |
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