JP5299863B2 - Metal vapor deposited film and method for producing the same - Google Patents
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
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Images
Abstract
Description
本発明は、金属蒸着高分子フィルムの密着性を向上するものであり、特にコンデンサ用金属蒸着フィルム及びそれを用いてなるコンデンサに関するものである。 The present invention improves the adhesion of a metal-deposited polymer film, and particularly relates to a metal-deposited film for a capacitor and a capacitor using the same.
コンデンサ用金属蒸着フィルムは、蒸着時にマージン形成の為、テープを用いたり、或いはマージン形成部にオイルを塗布し、この部分に金属を付着させないようにしたりしている。 The metal-deposited film for a capacitor uses a tape to form a margin at the time of vapor deposition, or applies oil to the margin forming portion so that the metal does not adhere to this portion.
このうちオイルを塗布して形成したマージンをもつ金属蒸着フィルムは、テープを利用したマージンで生じるマージン際への蒸着金属粉の付着、あるいは金属蒸着層のマージン際の端面が不均一となることによる絶縁耐電圧の低下がなく、高い耐電圧、高いコロナ開始電圧を有する優れた金属蒸着フィルムである。一方このマスキングオイルの残存のためコンデンサ素子作成時にフィルムの密着性が悪化、かつばらつきが発生するため、コンデンサ容量の安定性に欠け、高精度な容量を求められるコンデンサにおいては、歩留まりが悪いという問題がある。 Of these, metal-deposited film with a margin formed by applying oil is due to adhesion of vapor-deposited metal powder at the margin generated by the margin using tape, or non-uniform end face at the margin of the metal-deposited layer It is an excellent metal vapor-deposited film having no high withstand voltage and high corona onset voltage without lowering the withstand voltage. On the other hand, because of the remaining masking oil, the adhesion of the film deteriorates when the capacitor element is created, and variations occur. Therefore, the capacitor capacity is not stable and the yield is poor for capacitors that require high precision capacity. There is.
また、特許文献１や特許文献２などに記載されるような電極となる金属蒸着層の表層に、電極金属腐食防止のオイルを蒸着したコンデンサ用金属蒸着フィルムにおいては、特にコンデンサ素子のプレス性の悪化が大きく、容量バラツキが大きくなる傾向にある。
Moreover, in the metal vapor deposition film for a capacitor in which oil for preventing electrode metal corrosion is vapor-deposited on the surface layer of the metal vapor deposition layer to be an electrode as described in Patent Document 1 or
この問題を防ぐため、特許文献３では、フィルムに接着性の良い材質をコーティングしたフィルムを金属蒸着フィルムと抱き合わせる方法が提案されているが、これらの方法は材料および加工工程が増し、高コスト、およびコンデンサのサイズが大きくなる問題を抱えている。 In order to prevent this problem, Patent Document 3 proposes a method of tying a film obtained by coating a film having a good adhesive property with a metal vapor-deposited film. However, these methods increase the materials and processing steps, and increase the cost. , And have the problem of increasing the size of the capacitor.
コンデンサ用途以外にも密着性が必要とされる用途は多く、マスキングオイルで印刷を施す構成では該オイルが密着性を阻害することが問題となる。 In addition to the capacitor application, there are many applications that require adhesion, and in the configuration in which printing is performed with a masking oil, the oil impedes adhesion.
本発明は、金属蒸着高分子フィルムの密着性を向上するものであり、特にコンデンサ素子作成時のフィルム層間の接着性を向上させ、密着性を改善し容量ばらつきの少ない金属蒸着フィルムを提供するものである。 The present invention improves the adhesion of a metal vapor-deposited polymer film, and in particular, improves the adhesion between film layers at the time of making a capacitor element, thereby improving the adhesion and providing a metal vapor-deposited film with little variation in capacity. It is.
かかる課題を解決するための本発明は、次の（１）〜（６）のいずれかの構成を特徴とするものである。
（１）高分子フィルムからなる基材の片面に金属蒸着層を有する金属蒸着フィルムにおいて、該高分子フィルムの金属蒸着層を有する面の反対面に鉄またはクロムの金属が付着しており、５００μｍ□の範囲内における該反対面に付着した金属の飛行時間型２次イオン質量分析による測定強度が３００〜８０００ｃｏｕｎｔｓの範囲にあることを特徴とする金属蒸着フィルム。
（２）（１）に記載の金属蒸着フィルムを製造する方法であって、前記高分子フィルムの金属蒸着層を設ける面の反対面に放電処理することにより鉄またはクロムの金属を付着させることを特徴とする金属蒸着フィルムの製造方法。
（３）前記放電処理がプラズマ放電処理であることを特徴とする（２）に記載の金属蒸着フィルムの製造方法。
（４）前記高分子フィルムの金属蒸着層を有する面に、オイルを用いたマスキング法によりマージン部を形成することを特徴とする（２）または（３）に記載の金属蒸着フィルムの製造方法。
（５）（１）に記載の金属蒸着フィルム、または（２）〜（４）のいずれかに記載の方法で得られた金属蒸着フィルムであって、コンデンサ用であることを特徴とする金属蒸着フィルム。
（６）（５）に記載の金属蒸着フィルムを用いたコンデンサ。
The present invention for solving this problem is characterized by any one of the following configurations (1) to (6).
(1) In a metal vapor-deposited film having a metal vapor-deposited layer on one side of a substrate made of a polymer film, an iron or chromium metal is attached to the opposite side of the surface of the polymer film having the metal vapor-deposited layer, 500 μm metallized film which measured intensity by time-of-flight secondary ion mass spectrometry of metal adhering to the reflected face in the range of □ is being in the range of 300 to 8000 counts the.
(2) A method for producing a metal vapor-deposited film as described in (1), wherein an iron or chromium metal is adhered to the surface opposite to the surface on which the metal vapor-deposited layer of the polymer film is provided. A method for producing a metal-deposited film.
(3) The method for producing a metal-deposited film according to (2), wherein the discharge treatment is a plasma discharge treatment.
(4) The method for producing a metal vapor-deposited film according to (2) or (3), wherein a margin portion is formed on the surface of the polymer film having the metal vapor-deposited layer by a masking method using oil.
(5) A metal vapor deposition film according to (1) or a metal vapor deposition film obtained by the method according to any one of (2) to (4), wherein the metal vapor deposition film is used for a capacitor. the film.
(6) A capacitor using the metal vapor deposited film according to (5).
本発明は、高分子フィルムの金属蒸着層を有する面の反対面に、金属を散点状に付着させることにより金属蒸着高分子フィルム層間の密着性を向上するものであり、特にコンデンサ用途において、コンデンサを形成する複数の蒸着フィルムを巻回、または積層し、加熱成型する際の各フィルム層間の密着を安定させることで、コンデンサの容量のばらつきを小さくするもので、高いコンデンサ容量精度を得ることが可能となる。 The present invention is to improve the adhesion between metal vapor deposited polymer film layers by attaching a metal to the surface opposite to the surface having the metal vapor deposited layer of the polymer film, particularly in capacitor applications, Capable of obtaining high capacitor capacity accuracy by reducing the variation in capacitor capacity by stabilizing the adhesion between each film layer when winding or laminating a plurality of vapor-deposited films that form a capacitor and then heat-molding. Is possible.
以下、本発明の金属蒸着フィルムと該金属蒸着フィルムの製造方法、及び該金属蒸着フィルムを用いてなるコンデンサについて、更に詳しく説明をする。 Hereinafter, the metal vapor deposition film of this invention, the manufacturing method of this metal vapor deposition film, and the capacitor | condenser using this metal vapor deposition film are demonstrated in more detail.
本発明の一実施態様である金属蒸着フィルムの概略図を図１に示す。なお、本発明は本実施態様に限定されるものではない。 The schematic of the metal vapor deposition film which is one embodiment of this invention is shown in FIG. The present invention is not limited to this embodiment.
本発明のフィルムは、高分子フィルムからなる基材の片面に金属蒸着層を有する金属蒸着フィルムにおいて、該高分子フィルムの金属蒸着層を有する面の反対面に金属が付着しており、５００μｍ□範囲内における該反対面に付着した金属の飛行時間型２次イオン質量分析による測定強度が３００〜１００００ｃｏｕｎｔｓの範囲にあることを特徴とする金属蒸着フィルムである。図１は本発明の金属蒸着フィルムであり、１は高分子フィルムからなる基材、２は金属蒸着層、３は金属蒸着層が形成されていないか、或いは金属酸化物等から形成された絶縁部でコンデンサにした時の対極との絶縁を保持するための絶縁部（以下マージン部と呼ぶ）である。 The film of the present invention is a metal vapor-deposited film having a metal vapor-deposited layer on one side of a substrate made of a polymer film, wherein the metal is attached to the opposite side of the surface of the polymer film having the metal vapor-deposited layer. It is a metal vapor deposition film characterized by the measurement intensity | strength by the time-of-flight secondary ion mass spectrometry of the metal adhering to this opposite surface in the range being in the range of 300-10000counts. FIG. 1 shows a metal vapor deposition film according to the present invention, wherein 1 is a base material made of a polymer film, 2 is a metal vapor deposition layer, 3 is an insulating layer formed from a metal oxide layer or the like. This is an insulating part (hereinafter referred to as a margin part) for maintaining insulation from the counter electrode when the part is used as a capacitor.
４はマージン部を形成する際に使用したマスキングオイルの残存物である。 Reference numeral 4 denotes a residue of the masking oil used when forming the margin portion.
５は、金属蒸着層を施す側の反対面のフィルム基材１の表面であるが、本発明の金属蒸着フィルムは表面５に、５００μｍ□範囲内の飛行時間型２次イオン質量分析による測定強度が３００〜１００００ｃｏｕｎｔｓの範囲にある金属が付着している。 5 is the surface of the film substrate 1 on the side opposite to the side on which the metal vapor deposition layer is applied, but the metal vapor deposition film of the present invention has a surface 5 having a measured intensity by time-of-flight secondary ion mass spectrometry within the range of 500 μm □. Is in the range of 300-10000 counts.
本発明において、高分子フィルムの金属蒸着層を有する面の反対面に付着している金属の材質は特に限定されないが、例えば、アルミニウム、亜鉛、インジウム、スズ、ニッケル、クロム、鉄、銅、チタン、あるいはこれらの中から複数の物質、およびその化合物が挙げられ、好ましくは亜鉛、スズ、インジウム、ニッケル、クロム、鉄、銅であり、より好ましくはスズ、インジウム、ニッケル、クロム、鉄、銅である。 In the present invention, the material of the metal adhering to the surface opposite to the surface having the metal vapor deposition layer of the polymer film is not particularly limited. For example, aluminum, zinc, indium, tin, nickel, chromium, iron, copper, titanium Or a plurality of these substances and compounds thereof, preferably zinc, tin, indium, nickel, chromium, iron, copper, more preferably tin, indium, nickel, chromium, iron, copper is there.
本発明における高分子フィルムの金属蒸着層を有する面の反対面に付着している金属は、５００μｍ□範囲内における飛行時間型２次イオン質量分析による測定強度が３００〜１００００ｃｏｕｎｔｓの範囲となるようにごく微量、散点状に付着される。ここで散点状とは、例えば塗液で形成した連続的な付着ではなく、非連続的かつ島状に分散した付着である。各島状構造は電気的に浮遊した状態となっており、本発明の金属蒸着フィルムをコンデンサ用途にした場合にコンデンサの絶縁抵抗が良好に確保される。あるいは該金属は付着した後に空気にさらされ、一部または全てが酸化され、本発明の金属蒸着フィルムをコンデンサ用途にした場合にコンデンサの絶縁抵抗は良好に確保される。複数の金属を付着させた場合は、各金属における測定強度の和がこの範囲となることが必要である。 In the present invention, the metal adhering to the surface opposite to the surface having the metal vapor deposition layer of the polymer film has a measurement intensity by time-of-flight secondary ion mass spectrometry in the range of 500 μm □ within the range of 300 to 10000 counts. A very small amount is attached in the form of dots. Here, the scattered dot shape is not continuous adhesion formed with, for example, a coating liquid but discontinuous adhesion dispersed in islands. Each island-like structure is in an electrically floating state, and when the metal-deposited film of the present invention is used for a capacitor, a good insulation resistance of the capacitor is ensured. Alternatively, the metal is exposed to air after being deposited, and a part or all of the metal is oxidized. When the metal-deposited film of the present invention is used as a capacitor, the insulation resistance of the capacitor is ensured satisfactorily. When a plurality of metals are attached, it is necessary that the sum of the measured intensities of each metal falls within this range.
測定強度が３００ｃｏｕｎｔｓより小さいと複数枚の金属蒸着フィルムを重ねて定加重をかけたときの層間密着力、あるいは金属蒸着フィルムに他の高分子フィルムを接着剤で貼り合わせる場合の密着力が十分保てない。１００００ｃｏｕｎｔｓより大きいと金属量が多くなって電気的に浮遊した状態が保てなくなり、絶縁抵抗（ＩＲ）に影響を及ぼし不適である。測定強度は好ましくは５００〜８０００ｃｏｕｎｔｓ、より好ましくは８００〜８０００ｃｏｕｎｔｓである。 If the measured strength is less than 300 counts, the adhesion strength between layers when multiple metal vapor deposition films are stacked and applied with a constant load, or the adhesion strength when another polymer film is bonded to the metal vapor deposition film with an adhesive is sufficiently maintained. Not. If it is greater than 10,000 counts, the amount of metal increases and the electrically floating state cannot be maintained, which affects the insulation resistance (IR) and is not suitable. The measured intensity is preferably 500 to 8000 counts, more preferably 800 to 8000 counts.
本発明における高分子フィルムの金属蒸着層を有する面の反対面に付着している金属は、放電処理によって付着させることができ、放電処理の方法としては、たとえば、誘導加熱法、電子ビーム法、スパッタリング法等の真空蒸着法や、常圧で行う大気圧プラズマ処理法やコロナ処理法などが挙げられる。 The metal adhering to the surface opposite to the surface having the metal vapor deposition layer of the polymer film in the present invention can be attached by electric discharge treatment. Examples of electric discharge treatment methods include induction heating, electron beam, Examples include a vacuum deposition method such as a sputtering method, an atmospheric pressure plasma treatment method and a corona treatment method performed at normal pressure.
特に本発明における高分子フィルムの金属蒸着層を有する面の反対面に付着している金属を、飛行時間型２次イオン質量分析による測定強度３００〜１００００ｃｏｕｎｔｓと極めて微量になるように形成するためには、プラズマ放電処理が効果的であり、真空蒸着法では比較的蒸着レートの低いスパッタリング法のうちグロー処理法が、常圧では大気圧プラズマ処理やコロナ処理などの放電処理法により、放電処理装置の電極をスパッタして付着させることが好ましい。金属蒸着層を真空蒸着法で形成する場合には、真空グロー処理法を用いると、真空蒸着工程で効率的に処理ができるため好ましい。 In particular, in order to form the metal adhering to the surface opposite to the surface having the metal vapor deposition layer of the polymer film according to the present invention so as to have a very small amount of measurement intensity of 300 to 10000 counts by time-of-flight secondary ion mass spectrometry. The plasma treatment is effective, and the vacuum deposition method uses a relatively low deposition rate sputtering method, the glow treatment method is a normal pressure, and the atmospheric pressure plasma treatment or corona treatment discharge treatment method. It is preferable to deposit the electrode by sputtering. In the case where the metal vapor deposition layer is formed by a vacuum vapor deposition method, it is preferable to use a vacuum glow treatment method because it can be efficiently processed in a vacuum vapor deposition process.
真空グロー処理法による場合は、放電処理装置の電極には高分子フィルムの金属蒸着層を設ける面の反対面に付着させたい金属を使用し、高分子フィルムの金属蒸着層を設ける面と反対面に真空グロー処理を行うことによって、そのスパッタ効果で反対面に金属が付着する。グロー処理電力が大きいほど付着する金属量は多くなり、またライン速度が低い（遅い）ほど、付着する金属は多くなる。これらにより好適な範囲に金属量を調整する。
真空グロー処理については、設定条件は特に限定されないが、速度100〜800m/min、2〜120W/min・ｍ２、周波数10〜500kHzであることが好ましい。
When using the vacuum glow processing method, use the metal that you want to adhere to the surface opposite to the surface on which the metal vapor deposition layer of the polymer film is provided for the electrode of the discharge treatment device, and the surface opposite to the surface on which the metal vapor deposition layer of the polymer film is provided By performing a vacuum glow process, the metal adheres to the opposite surface due to the sputtering effect. The larger the glow processing power is, the more metal is deposited, and the lower the line speed (slower), the more metal is deposited. The amount of metal is adjusted to a suitable range by these.
Regarding the vacuum glow treatment, the setting conditions are not particularly limited, but it is preferable that the speed is 100 to 800 m / min, 2 to 120 W / min · m 2 , and the frequency is 10 to 500 kHz.
本発明における高分子フィルムとは、例えば、ポリエチレンテレフタレート、ポリエチレンナフタレートなどのポリエステル、ポリプロピレン、などのポリオレフィン、ポリスチレン、ポリフェニレンスルフィド、ポリカーボネート、ポリアミド、ポリフッ化ビニリデン、ポリパラキシレンなどあるいはこれらの共重合樹脂等の高分子樹脂をフィルム状に成型したものをさす。 The polymer film in the present invention is, for example, a polyester such as polyethylene terephthalate or polyethylene naphthalate, a polyolefin such as polypropylene, polystyrene, polyphenylene sulfide, polycarbonate, polyamide, polyvinylidene fluoride, polyparaxylene, or a copolymer resin thereof. It refers to a polymer resin such as that formed into a film.
また、その他の有機重合体との混合体、積層体であっても良い。これらの高分子化合物に、公知の添加剤、例えば、滑剤や可塑剤などが含まれても良い。本発明で用いられる高分子フィルムの主成分としては、ポリエステル、ポリオレフィンおよびポリフェニレンスルフィドから選ばれた１種であることが、耐湿性及びコンデンサ電気特性の観点から好ましい。ここで、主成分とは高分子フィルム全体に対して５０質量％以上であることを言う。より好ましくは６０質量％以上が、ポリエステル、ポリオレフィンおよびポリフェニレンスルフィドから選ばれた１種であることを言う。特に好ましくは、ポリエチレンテレフタレート、ポリエチレンナフタレート、ポリプロピレン、ポリフェニレンスルフィド及びこれらの共重合体から選ばれた１種であることがコンデンサの電気特性上好ましい。 Moreover, the mixture and laminated body with another organic polymer may be sufficient. These polymer compounds may contain known additives such as lubricants and plasticizers. The main component of the polymer film used in the present invention is preferably one selected from polyester, polyolefin and polyphenylene sulfide from the viewpoint of moisture resistance and capacitor electrical characteristics. Here, the main component means 50% by mass or more based on the entire polymer film. More preferably 60% by mass or more is one selected from polyester, polyolefin and polyphenylene sulfide. Particularly preferably, it is one kind selected from polyethylene terephthalate, polyethylene naphthalate, polypropylene, polyphenylene sulfide, and copolymers thereof from the viewpoint of electrical characteristics of the capacitor.
本発明で用いられる高分子フィルムの厚みは、特に限定されないが、０．５μｍ〜１００μｍの範囲が好ましい。厚みをこの範囲とすることで、本発明の効果をより高く発揮することができる。より好ましくは高分子フィルムの厚みは０．７μｍ〜１３μｍの範囲であり、さらに好ましくは１．０μｍ〜６μｍの範囲である。 Although the thickness of the polymer film used by this invention is not specifically limited, The range of 0.5 micrometer-100 micrometers is preferable. By making thickness into this range, the effect of this invention can be exhibited more highly. More preferably, the thickness of the polymer film is in the range of 0.7 μm to 13 μm, and more preferably in the range of 1.0 μm to 6 μm.
本発明の金属蒸着フィルムは、高分子フィルムの片面に金属蒸着層を有する。その金属蒸着層の形成方法は特に限定されない。例えば、蒸着、スパッタリング、イオンプレーティングあるいはメッキなどの方法を用いて形成することができる。好ましくは真空蒸着法を用いて形成された金属蒸着層である。真空蒸着法を用いると、効率的に本発明のフィルムを製造することができる。 The metal vapor deposition film of this invention has a metal vapor deposition layer on the single side | surface of a polymer film. The formation method of the metal vapor deposition layer is not specifically limited. For example, it can be formed using a method such as vapor deposition, sputtering, ion plating, or plating. Preferably, it is a metal vapor deposition layer formed using a vacuum vapor deposition method. When the vacuum deposition method is used, the film of the present invention can be produced efficiently.
本発明における金属蒸着層の材質としては、例えば、アルミニウム、亜鉛、スズ、ニッケル、クロム、鉄、銅、チタン、あるいはこれらを含有する合金等が挙げられる。生産性の面からは、亜鉛、アルミニウム、またはそれらを含む合金が好ましく用いられる。より好ましくは、金属蒸着層がアルミニウムを９０質量％以上含むことである。具体的には、アルミニウム単体またはアルミニウムを９０質量％以上含むアルミニウム合金を用いることが耐湿性の観点から好ましい。 Examples of the material for the metal vapor deposition layer in the present invention include aluminum, zinc, tin, nickel, chromium, iron, copper, titanium, and alloys containing these. From the viewpoint of productivity, zinc, aluminum, or an alloy containing them is preferably used. More preferably, the metal vapor deposition layer contains 90% by mass or more of aluminum. Specifically, it is preferable from the viewpoint of moisture resistance to use aluminum alone or an aluminum alloy containing 90% by mass or more of aluminum.
コンデンサ用途においては、金属蒸着層の厚みは１〜１００ｎｍであることが、電気特性上好ましい。また金属蒸着層の膜抵抗は、好ましくは０．５〜３０Ω／□、より好ましくは１．５〜２５Ω／□、さらに好ましくは３〜２０Ω／□の範囲であることが好ましい。膜抵抗が０．５Ω／□未満では、セルフヒーリング不良を発生し絶縁抵抗が悪化するなど本来のコンデンサ特性が得られないことがある。また、３０Ω／□を越えると直列等価抵抗が増大し、誘電正接（ｔａｎδ）が悪化することがある。より好ましくは１．５〜２５Ω／□、さらに好ましくは３〜２０Ω／□である。膜抵抗を上記範囲にするには、金属蒸着層の厚みの制御および金属種の選定をすることで可能である。 In the capacitor application, the thickness of the metal deposition layer is preferably 1 to 100 nm in terms of electrical characteristics. The film resistance of the metal vapor deposition layer is preferably in the range of 0.5 to 30Ω / □, more preferably 1.5 to 25Ω / □, and further preferably 3 to 20Ω / □. If the film resistance is less than 0.5Ω / □, the original capacitor characteristics may not be obtained, for example, a self-healing failure occurs and the insulation resistance deteriorates. On the other hand, if it exceeds 30Ω / □, the series equivalent resistance may increase and the dielectric loss tangent (tan δ) may deteriorate. More preferably, it is 1.5-25 ohm / square, More preferably, it is 3-20 ohm / square. In order to make film resistance into the said range, it is possible by controlling the thickness of a metal vapor deposition layer, and selecting a metal seed | species.
本発明の金属蒸着フィルムにおいて、前記金属蒸着層の表層に、電極金属腐食防止層を形成することが好ましい。特に、耐候性に劣る亜鉛などを金属蒸着層に用いて電極金属とする場合、金属蒸着層の上に電極金属腐食防止層を形成させることで耐侯性が高まる。電極金属防止層はオイルで形成され、たとえば特公昭６３−１５７３７号公報に開示された公知のものを用いることができる。具体的には、フッ素系オイルやシリコーン系オイルが挙げられ、シリコーン系オイルがより好ましい。電極金属腐食防止層の形成方法としては、金属蒸着層を設ける工程において、金属蒸着層を形成後に、その金属蒸着層の上にフッ素系オイルやシリコーン系オイルを真空中で加熱・蒸散させて付着させることにより電極金属腐食防止層を形成することができる。 In the metal vapor deposition film of the present invention, an electrode metal corrosion prevention layer is preferably formed on the surface layer of the metal vapor deposition layer. In particular, when zinc or the like, which is inferior in weather resistance, is used for the metal vapor deposition layer to form an electrode metal, weather resistance is enhanced by forming an electrode metal corrosion prevention layer on the metal vapor deposition layer. The electrode metal prevention layer is made of oil, and for example, a known layer disclosed in Japanese Patent Publication No. 63-15737 can be used. Specific examples include fluorine oil and silicone oil, and silicone oil is more preferable. As a method of forming an electrode metal corrosion prevention layer, in the step of providing a metal vapor deposition layer, after forming the metal vapor deposition layer, the fluorine vapor or silicone oil is heated and evaporated in vacuum on the metal vapor deposition layer. By doing so, an electrode metal corrosion prevention layer can be formed.
本発明の金属蒸着フィルムは、例えば、コンデンサにした時に対電極との絶縁をとるため、マージン部を設けることができる。マージン部を設ける方法は特に限定されるものではないが、マスキング方式がオイルを用いたマスキング法を用いることがコンデンサの電気特性上好ましく、本発明の効果を顕著に発現させることが出来る。オイルを用いたマスキング法においては、金属蒸着層を設ける工程において、金属蒸着層を形成する前に、マスキングオイルとしてフッ素系オイル、シリコーン系オイル、あるいは鉱物系オイルを高分子フィルム上に付着させることにより、金属の付着を妨げてマージン部を設ける。マスキングオイルを付着させる方法は、マスキングオイルを真空中で加熱・蒸散させ、所定の間隔で穴あるいはスリットを設けたマスクを通してフィルムに付着させる方法などが例示できる。 The metal vapor deposition film of the present invention can be provided with a margin portion, for example, in order to insulate from the counter electrode when a capacitor is formed. The method of providing the margin portion is not particularly limited, but the masking method using an oil-based masking method is preferable in terms of the electrical characteristics of the capacitor, and the effects of the present invention can be remarkably exhibited. In the masking method using oil, in the step of forming a metal vapor deposition layer, before forming the metal vapor deposition layer, fluorine oil, silicone oil, or mineral oil is deposited on the polymer film as masking oil. Thus, the margin is provided by preventing the adhesion of the metal. Examples of the method for attaching the masking oil include a method in which the masking oil is heated and evaporated in a vacuum and attached to the film through a mask provided with holes or slits at predetermined intervals.
一般に高分子フィルムを用いたフィルムコンデンサは、コアに金属蒸着フィルムを巻回した丸型コンデンサ、金属蒸着フィルムを巻回した後にプレスし、扁平にした扁平型コンデンサ、あるいは扁平型コンデンサを切り出して蒸着フィルムを積層構造にした積層コンデンサ等があるが、本発明の金属蒸着フィルムは、いずれのコンデンサに対してもコンデンサの容量のばらつきを改善するのに有効である。 Generally, a film capacitor using a polymer film is a round capacitor in which a metal vapor-deposited film is wound around a core, a metal vapor-deposited film is wound and pressed, and a flat capacitor or a flat capacitor that is flattened is cut out and vapor-deposited. There are laminated capacitors having a laminated film structure, and the metal-deposited film of the present invention is effective in improving the variation in the capacitance of the capacitor for any capacitor.
特に容量のばらつきが発生しやすい扁平型コンデンサ、あるいは積層型コンデンサに優れた改善効果を示し、中でもフィルムのプレス成形が行い難く密着性が弱い、積層型コンデンサに著しい改善効果を示し、本発明の金属蒸着フィルムを用いることによってばらつきが極めて少ない容量の安定したコンデンサを作ることが出来る。 In particular, it shows excellent improvement effects for flat capacitors or multilayer capacitors that tend to vary in capacitance, and especially shows remarkable improvement effects for multilayer capacitors that are difficult to press-mold films and have poor adhesion. By using a metal vapor-deposited film, it is possible to make a stable capacitor with very little variation.
（物性値の測定及び評価方法）
（１）高分子フィルムの金属蒸着層を有する面の反対面の金属付着量
試料となる金属蒸着フィルムを測定容器に入るよう幅１０ｍｍ×長さ１０ｍｍ採取し、その中央部を飛行時間型２次イオン質量分析法で２回ずつ測定し、その平均値を金属付着量（ｃｏｕｎｔｓ）とした。
飛行時間型２次イオン分析には、ＴＯＦ．ＳＩＭＳ ５（ＩＯＮ−ＴＯＦ社製）を使用した。
測定条件は、以下で測定した。
１次イオン：Ｂｉ３ ＋＋、
１次イオンエネルギー：２５ｋＶ、
パルス幅：３．１ｎｓ、
バンチング：あり、
帯電中和：あり、
測定真空度：４×１０−７Ｐａ
２次イオン極性：正および負、
質量範囲（ｍ／ｚ）：０〜１５００ｕ
ラスターサイズ：５００μｍ□
スキャン数：３２ｓｃａｎ
ピクセル数：１２８ｐｉｘｅｌ
後段加速：１０ｋＶ。
(Measurement and evaluation method of physical properties)
(1) Amount of metal adhesion on the opposite side of the polymer film having the metal vapor deposition layer The sample of the metal vapor deposition film as a sample was taken 10 mm in width and 10 mm in length so as to enter the measurement container, and the central part was time-of-flight type secondary Measurement was performed twice by ion mass spectrometry, and the average value was defined as the amount of metal adhesion (counts).
For time-of-flight secondary ion analysis, TOF. SIMS 5 (manufactured by ION-TOF) was used.
Measurement conditions were measured as follows.
Primary ion: Bi 3 ++ ,
Primary ion energy: 25 kV,
Pulse width: 3.1 ns
Bunching: Yes,
Charge neutralization: Yes,
Measuring degree of vacuum: 4 × 10 −7 Pa
Secondary ion polarity: positive and negative,
Mass range (m / z): 0 to 1500 u
Raster size: 500μm
Number of scans: 32scan
Number of pixels: 128 pixels
Post acceleration: 10 kV.
（２）コンデンサ容量精度
素子巻き後メタリコン及びリード端子付けしたコンデンサ素子を、安藤電気（株）製 ＬＣＲ ＭＥＴＥＲ ＴＹＰＥ ＡＧ−４３１１で１Ｖｒｍｓの電圧をかけ、周波数１ｋＨｚでコンデンサの容量を測定した。実施例で作成した素子１００個について測定し、容量偏差が±５．０％以上のものを容量精度不良とし、５％未満を容量精度良好とした。また、素子１００個のうち容量精度不良である素子の個数を容量不良率（％）とした。
(2) Capacitor capacity accuracy After the element was wound, the capacitor with the metallicon and lead terminals attached thereto was applied with a voltage of 1 Vrms by LCR METER TYPE AG-4431 manufactured by Ando Electric Co., Ltd., and the capacity of the capacitor was measured at a frequency of 1 kHz. Measurement was performed on 100 elements prepared in the example, and those with a capacity deviation of ± 5.0% or more were regarded as poor capacity precision, and less than 5% were regarded as good capacity precision. Further, the number of elements having a capacity accuracy defect out of 100 elements was defined as a capacity defect rate (%).
（３）絶縁抵抗
日置電機株式会社製超絶縁抵抗計SM-8220にて、２５０Ｖにて１分値を測定した。
実施例においては、２００００MΩ以上を良好とした。
(3) Insulation resistance One minute value was measured at 250 V with a super insulation resistance meter SM-8220 manufactured by Hioki Electric Co., Ltd.
In the examples, 20000 MΩ or more was considered good.
（４）膜抵抗
４端子法により、１００ｍｍの電極間の金属膜の抵抗を測定し、測定値を測定幅と電極間距離で除し、幅１０ｍｍ、電極間距離１０ｍｍ当たりの膜抵抗を算出した。単位はΩ／□と表示する。
(4) Membrane resistance The resistance of a metal film between 100 mm electrodes was measured by the 4-terminal method, and the measured value was divided by the measurement width and the distance between the electrodes to calculate the membrane resistance per 10 mm width and 10 mm distance between the electrodes. . The unit is displayed as Ω / □.
（５）金属蒸着フィルムの総厚み
ＪＩＳ Ｃ ２１５１（1990年制定2006年改訂）に従い、１０枚重ねの金属蒸着フィルムの厚みを電子マイクロメータで測定し、５点平均した平均値を金属蒸着フィルム枚数(１０)で除して金属蒸着フィルム厚みとした。
(5) Total thickness of the metal vapor deposition film According to JIS C 2151 (established in 1990, revised in 2006), the thickness of the 10 metal vapor deposition films was measured with an electronic micrometer, and the average value obtained by averaging 5 points was the number of metal vapor deposition films. Divided by (10) to obtain a metal vapor deposited film thickness.
（実施例１）
厚さ３μｍ、幅620mmのポリプロピレンフィルムに、蒸着機内でフィルム走行速度４００ｍ／ｍｉｎで搬送させながら、フッ素系マスキングオイルフォンブリンＹ０４（ソルベイ ソレクシス社製）を蒸着し、幅２ｍｍのマージン部を形成し、次いでアルミニウムを抵抗値が３Ω／□に蒸着した。コンデンサ用蒸着フィルムの非蒸着面に酸素、アルゴンを各々２００ｃｃ／ｍｉｎ流しながら、１００ｋＨｚ、３００Ｖのパルス状直流電圧をかけ、持続するグロー放電にて処理したコンデンサ用蒸着フィルムを作成した。グロー放電電極には、断面が直径５ｃｍの棒円筒状のステンレス金属を用いた。
Example 1
Fluorine-based masking oil fomblyin Y04 (manufactured by Solvay Solexis) is vapor-deposited on a polypropylene film with a thickness of 3 μm and a width of 620 mm while being transported at a film running speed of 400 m / min. Then, aluminum was vapor-deposited with a resistance value of 3Ω / □. A vapor deposition film for a capacitor was prepared by applying a pulsed DC voltage of 100 kHz and 300 V to the non-deposition surface of the vapor deposition film for a capacitor at a flow rate of 200 cc / min. For the glow discharge electrode, a rod-cylindrical stainless metal having a diameter of 5 cm was used.
グロー放電処理したフィルム面を飛行時間型２次イオン質量分析で分析測定すると、グロー放電電極に用いたステンレス金属に由来するクロムと鉄が各々３００、５００ｃｏｕｎｔｓの強度で検出された。 When the film surface subjected to the glow discharge treatment was analyzed and measured by time-of-flight secondary ion mass spectrometry, chromium and iron derived from the stainless metal used for the glow discharge electrode were detected at an intensity of 300 and 500 counts, respectively.
次いでこの金属蒸着フィルムをマージン部幅１ｍｍ、フィルム幅１４ｍｍにスリット後、素子巻きを行い３μＦの素子を作成した。次いで、１０５℃、３０ｋｇ、６分の条件でプレスを行い、容量不良率及び絶縁抵抗を評価した。容量不良率は０％、絶縁抵抗は３１０００ＭΩと良好であった。 Next, this metal vapor-deposited film was slit into a margin width of 1 mm and a film width of 14 mm, and then wound on an element to produce a 3 μF element. Next, pressing was performed under the conditions of 105 ° C., 30 kg, 6 minutes, and the capacity defect rate and the insulation resistance were evaluated. The capacity defect rate was 0% and the insulation resistance was as good as 31000 MΩ.
（実施例２）
実施例２では、あらかじめ厚さ３μｍ、幅620mmのポリプロピレンフィルムに、幅700mm、長さ70mmの銅電極を有するスパッタリング装置にて、フィルム走行速度１０ｍ／ｍｉｎで搬送させ、酸素、アルゴンを各々２００ｃｃ／ｍｉｎ流しながら、スパッタリング電極に３００ｋＨｚ、２００Ｖのパルス状直流電圧をかけて放電させることによって、飛行時間型２次イオン質量分析による強度８０００ｃｏｕｎｔｓの範囲になるように銅を付着させ、その後このスパッタリングされた面と反対の面に実施例１と同じように、フッ素系マスキングオイルフォンブリン（アウジモント社製）を蒸着した後アルミニウムと亜鉛の合金を蒸着し、更に金属腐食防止用シリコーンオイル（東レダウ製ＳＨ２００）を蒸着し、マージン部幅２ｍｍ、金属蒸着層の抵抗値６Ω／□のコンデンサ用蒸着フィルムを作成した。次いでこの金属蒸着フィルムをフィルム幅１４ｍｍにスリット後、素子巻きを行い３μＦの素子を作成した。次いで、１０５℃、３０ｋｇ、６分の条件でプレスを行い、容量不良率及び絶縁抵抗を評価した。容量不良率は１％、絶縁抵抗は５１０００ＭΩと良好であった。
(Example 2)
In Example 2, a polypropylene film having a thickness of 3 μm and a width of 620 mm was previously transported at a film running speed of 10 m / min by a sputtering apparatus having a copper electrode having a width of 700 mm and a length of 70 mm, and oxygen and argon were each 200 cc / While flowing for min, the sputtering electrode was discharged by applying a pulsed DC voltage of 300 kHz and 200 V to attach copper so that the strength was in the range of 8000 counts by time-of-flight secondary ion mass spectrometry, and then this sputtering was performed. In the same manner as in Example 1, a fluorine-based masking oil fomblin (Audimont) was vapor-deposited on the surface opposite to the surface, and then an alloy of aluminum and zinc was vapor-deposited. Further, a silicone oil for preventing metal corrosion (SH200 manufactured by Toray Dow). ), The margin width is 2mm, the resistance of the metal deposition layer A vapor deposition film for capacitors having a resistance value of 6Ω / □ was prepared. Subsequently, this metal vapor deposition film was slit to a film width of 14 mm, and then wound on an element to produce a 3 μF element. Next, pressing was performed under the conditions of 105 ° C., 30 kg, 6 minutes, and the capacity defect rate and the insulation resistance were evaluated. The capacity defect rate was 1% and the insulation resistance was as good as 51000 MΩ.
（比較例１）
比較例１では実施例１で行ったグロー放電処理を実施しなかった以外は、実施例１と同じ方法で蒸着フィルムを製造し、コンデンサを作製した。容量不良率及び絶縁抵抗を評価したところ、容量不良率は６％と不良であった。絶縁抵抗は２５０００ＭΩであった。
(Comparative Example 1)
In Comparative Example 1, a vapor deposition film was manufactured by the same method as in Example 1 except that the glow discharge treatment performed in Example 1 was not performed, and a capacitor was manufactured. When the capacity defect rate and the insulation resistance were evaluated, the capacity defect rate was 6%. The insulation resistance was 25000 MΩ.
（比較例２）
比較例２は実施例２で用いたあらかじめスパッタリングされていないポリプロピレンを用いた以外は実施例２と同じ条件で蒸着した。容量不良率及び絶縁抵抗を評価したところ、容量不良率は８％と不良であった。絶縁抵抗は４９０００ＭΩであった。
(Comparative Example 2)
Comparative Example 2 was vapor-deposited under the same conditions as in Example 2 except that the unsputtered polypropylene used in Example 2 was used. When the capacity defect rate and the insulation resistance were evaluated, the capacity defect rate was 8%. The insulation resistance was 49000 MΩ.
（比較例３）
ポリプロピレンフィルムにスパッタリング装置にて、飛行時間型２次イオン質量分析による強度で２０００００ｃｏｕｎｔｓの範囲になるように銅を付着させる以外は、実施例２と同様の方法で蒸着フィルムを作成した。容量不良率及び絶縁抵抗を評価したところ、容量不良率は２％と良好であったが、絶縁抵抗は１４０００ＭΩと不良であった。
(Comparative Example 3)
A vapor deposition film was prepared in the same manner as in Example 2 except that copper was deposited on the polypropylene film with a sputtering apparatus so that the strength by time-of-flight secondary ion mass spectrometry was in the range of 200000 counts. When the capacity defect rate and the insulation resistance were evaluated, the capacity defect rate was as good as 2%, but the insulation resistance was as poor as 14000 MΩ.
これらの実施例から明らかな様に、本発明による金属蒸着フィルムは、本発明の効果であるコンデンサの容量バラツキが大幅に改良されたものである。 As is clear from these examples, the metal-deposited film according to the present invention has greatly improved capacitance variation of the capacitor, which is the effect of the present invention.
１：高分子フィルム
２：金属蒸着層
３：マージン部
４：マスキングオイル
５：金属
1: Polymer film 2: Metal deposition layer 3: Margin part 4: Masking oil 5: Metal
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