JP4234338B2 - Film deposition method - Google Patents
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- JP4234338B2 JP4234338B2 JP2001389389A JP2001389389A JP4234338B2 JP 4234338 B2 JP4234338 B2 JP 4234338B2 JP 2001389389 A JP2001389389 A JP 2001389389A JP 2001389389 A JP2001389389 A JP 2001389389A JP 4234338 B2 JP4234338 B2 JP 4234338B2
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- 238000000151 deposition Methods 0.000 title claims description 34
- 239000010408 film Substances 0.000 claims description 141
- 238000007740 vapor deposition Methods 0.000 claims description 84
- 239000000463 material Substances 0.000 claims description 57
- 230000008021 deposition Effects 0.000 claims description 22
- 238000010894 electron beam technology Methods 0.000 claims description 16
- 239000004760 aramid Substances 0.000 claims description 13
- 229920003235 aromatic polyamide Polymers 0.000 claims description 13
- 238000004090 dissolution Methods 0.000 claims description 13
- 239000010409 thin film Substances 0.000 claims description 7
- 238000001771 vacuum deposition Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 description 15
- 230000005291 magnetic effect Effects 0.000 description 14
- 238000001816 cooling Methods 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 229920006254 polymer film Polymers 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000011112 polyethylene naphthalate Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 230000005294 ferromagnetic effect Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 229910020630 Co Ni Inorganic materials 0.000 description 1
- 229910002440 Co–Ni Inorganic materials 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
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- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005347 demagnetization Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/225—Oblique incidence of vaporised material on substrate
- C23C14/226—Oblique incidence of vaporised material on substrate in order to form films with columnar structure
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は、フィルムの蒸着方法に関し、詳しくは、蒸着準備段階における蒸着材料の溶解のための加熱によってもフィルムの熱負けや破断等が発生せず、かつ、この段階でのフィルムのロスの発生を最小限に抑えることができるフィルムの蒸着方法に関する。
【０００２】
【従来の技術】
データバックアップ用および映像記録用としての磁気テープ、包装用フィルム、電極フィルムなどの多岐にわたる用途に、高分子フィルムへの蒸着技術が応用されている。
【０００３】
中でも磁気記録用途においては、磁気記録システムの大容量化や小型化に伴い媒体の高密度化やテープの薄型化が要求されている中で、蒸着型の磁気記録媒体は、塗布型媒体に比し、バインダを含まないために磁性層の充填率が高く、飽和磁化を大きくすることが可能であり、また、薄膜化が可能であるために短波長の記録に対しても記録減磁を抑えることができるなど、高密度記録において有利であるという利点を有している。
【０００４】
蒸着媒体としては、従来、被蒸着材料に高分子フィルムとしてポリエチレンテレフタレート（ＰＥＴ）やポリエチレンナフタレート（ＰＥＮ）を用い、蒸着材料に磁性層を形成する強磁性金属としてＣｏまたはＣｏ−Ｎｉ合金を用いたものが知られており、これらの蒸着技術においては、金属を蒸発させるために電子ビームを用いて、高分子フィルムを冷却ドラムに抱かせた状態で走行させながら、連続蒸着を行うことが一般的である。
【０００５】
この場合、蒸着を行うに際し蒸着材料を連続的に安定して蒸発させるためには、蒸着材料およびるつぼの事前加熱作業（溶かし込み）を行うことが必要となるが、この作業においては、蒸着源加熱に伴う輻射熱により高分子フィルムが熱負けして、破断に至ってしまうという問題があった。このため、開閉可能な遮蔽板を蒸着材料と高分子フィルムとの間に配置して熱を遮断したり、高分子フィルムを冷却ドラムに抱かせるなどの手法が用いられてはいるが、これらだけでは十分ではないため、フィルムを低速で走行させながら溶かし込み作業を行う手法が採られている。
【０００６】
【発明が解決しようとする課題】
しかしながら、上記手法を用いて蒸着を行った場合でも、低速とはいえ溶かし込み時の走行部分はロスとなることから、この溶かし込み作業はフィルムの使用効率を大幅に悪化させる要因となっていた。
【０００７】
また、近年の磁気記録媒体に対する大容量記録の要請から、テープ１巻あたりの巻き長さを長くするためにテープ全厚を薄くする必要が生じており、高分子フィルムの材料についても、薄くした場合でも強度を確保することのできる高ヤング率材料へ移行してきている。
【０００８】
高ヤング率フィルムとしては、芳香族ポリアミド（アラミド）フィルムが代表的であるが、かかるアラミドフィルムを用いた場合、耐熱性がＰＥＴやＰＥＮよりも高くなる反面、電子ビームを蒸着源に投入した際に発生する二次電子または反跳電子によってフィルムが極端に帯電してしまい、フィルムを低速走行させながら溶かし込みを行う方法においては、冷却ドラムへのフィルムの帯電貼り付きによって剥離時のフィルム破断が発生しやすくなり、走行も不安定となるという問題が発生していた。
【０００９】
そこで本発明の目的は、長尺フィルムの蒸着準備段階における蒸着材料の溶解に際し、溶解のための加熱に伴うフィルムへの熱や帯電の影響を排して、フィルムの熱負けや破断の発生がなく、かつ、従来に比しフィルムのロスの発生を低減することができ、従ってフィルムの走行、蒸着を安定して行うことができるフィルムの蒸着方法を提供することにある。
【００１０】
【課題を解決するための手段】
上記課題を解決するために、本発明のフィルムの蒸着方法は、芳香族ポリアミドからなる長尺フィルム上に、真空蒸着により薄膜を形成するフィルムの蒸着方法において、電子ビームにより蒸着材料の溶解を行う間は該蒸着材料と前記長尺フィルムとの間の遮蔽板を閉じた状態で前記長尺フィルムを１ｍ／ｍｉｎ以下の極低速スピードにて走行させ、前記蒸着材料の溶解が完了したところで該長尺フィルムの走行を加速させ、同時に、前記遮蔽板を開くことを特徴とするものである。
【００１１】
さらに、本発明のフィルムの蒸着方法は、芳香族ポリアミドからなる長尺フィルム上に、真空蒸着により薄膜を形成するフィルムの蒸着方法において、電子ビームにより蒸着材料の溶解を行う間は該蒸着材料と前記長尺フィルムとの間の遮蔽板を閉じた状態で前記長尺フィルムを１ｍ／ｍｉｎ以下の極低速スピードにて走行させ、前記蒸着材料の溶解が完了したところで該長尺フィルムの走行を加速させ、その後、前記遮蔽板を開くことを特徴とするものである。
【００１２】
本発明によれば、長尺フィルムにつき所定の材料を用い、かつ、蒸着作業を所定の条件、手順に従い行うことにより、フィルムに対する熱の影響を最低限に抑え、熱の影響を受けるフィルムの範囲を最小限にして、冷却ドラム剥離時のフィルム破断を防止することができるとともに、蒸着時においては良好な走行状態を維持し、安定した蒸着作業を行うことができる。
【００１３】
【発明の実施の形態】
以下、本発明の具体的な実施の形態についてより詳細に説明する。
本発明の蒸着方法においては、ヤング率が高く耐熱性にも優れた芳香族ポリアミドを被蒸着材料となる高分子支持体フィルムとして用い、このフィルム上に真空蒸着により蒸着材料の薄膜を形成する。
【００１４】
本発明に用いることのできる蒸着装置の一例を図１に示す。図示する蒸着装置１は斜め蒸着装置と呼ばれるものであり、この装置を用いる斜め蒸着法では、蒸着材料の蒸気を被蒸着材料の表面に特定の角度で入射させ、被蒸着材料に対し傾いた柱状結晶粒子からなる蒸着材料の薄膜を形成する。具体的には、真空容器中において、長尺フィルム状の被蒸着材料としての芳香族ポリアミドフィルム２を供給ロール３から繰り出し、回転する冷却ドラム４の表面に添わせて搬送しながら、定置された蒸着るつぼ５内の蒸着材料に電子銃６から電子ビーム６Ｂを照射して蒸着材料の溶湯を形成し、蒸着材料の蒸発物を発生させて斜め蒸着を行うことにより、長尺フィルム２の表面上に蒸着材料の薄膜を形成することができる。
【００１５】
図中、冷却ドラム４を覆うように設けられている遮蔽板９は、蒸着材料の入射角を規制するためのものであり、この遮蔽板９には、長尺フィルム２の所定部位にのみ蒸発金属が蒸着するように、開口が形成されている。この開口には、図示するようにシャッター１０が設けてあり、このシャッター１０が蒸着の初期および終期には矢印の方向にスライドして遮蔽板９の開口の開放および遮断を行い、不要な蒸着を防止する働きを有している。
【００１６】
本発明においては、上記蒸着を行うに際して、蒸着準備段階として行う蒸着材料の溶解の際に、遮蔽板９を閉じたまま、即ち、遮蔽板９の開口をシャッター１０により塞いだままの状態で、長尺フィルム２を静止させるかまたは１ｍ／ｍｉｎ以下の極低速スピードにて走行させる。これにより、長尺フィルム２に対する蒸着材料の溶解のための加熱に伴う輻射熱の影響を最低限に抑えつつ、熱の影響を受ける長尺フィルム２の範囲、即ち、フィルムのロスを最小限に抑えることができる。長尺フィルム２としてＰＥＴやＰＥＮを用いた場合、溶かし込みの際にフィルムを静止させ、または、１ｍ／ｍｉｎ以下程度の極低速にて走行させると、熱劣化によりフィルムの状態が著しく悪化し、フィルムの走行性自体に悪影響が及んで、蒸着準備完了後においてももはやフィルムを安定に走行させることができなくなる。そこで本発明においては、蒸着準備段階における上記フィルム走行条件と併せ、耐熱性に優れた芳香族ポリアミドを長尺フィルム２の材料としたことにより、フィルムの熱負けや穴あきを防止し、走行性を良好に保ちつつ安定に蒸着を行うことが可能となったものである。また、本発明においては、芳香族ポリアミドのフィルムにおいて生じやすいフィルムの帯電による貼り付き、さらにはこれによる破断や、走行状態の不安定化をも生じることがない。
【００１７】
上述のようにして蒸着準備を行った後は、蒸着準備が整ったところで長尺フィルム２の本走行を開始させ、シャッター１０を開く。即ち、シャッター１０は、長尺フィルム２の本走行を開始させた後、走行確認後に開いてもよいが、本走行の開始と同時に開いてもよい。なお、ここで「本走行」とは、蒸着時のフィルムの走行を意味し、上述の蒸着準備段階における極低速走行と区別される。本走行時のフィルムの走行速度は５０〜３００ｍ／ｍｉｎ程度である。
【００１８】
本発明においては、蒸着準備段階における上記手順が重要であり、蒸着に関するその他の条件は常法に従い適宜決定すればよく、特に制限されない。特には、本発明の蒸着方法は、磁気記録媒体の製造において、非磁性基体としての長尺フィルム２上に真空蒸着により磁性層を形成するに際し好適に用いることができる。
【００１９】
磁性層の蒸着材料としては、好適には、強磁性金属材料を用いる。かかる強磁性金属材料としては、例えば、Ｆｅ、Ｃｏ、Ｎｉ等の単独若しくは混合材料、または、Ｃｏ−Ｎｉ−Ｃｒ、Ｆｅ−Ｎｉ−Ｎ、Ｃｏ−Ｎｉ−Ｔａなどの三成分系などが挙げられるが、特に制限されるべきものではない。この場合、斜め蒸着法においては、非磁性基体２が走行可能な真空容器内を１０-3Ｐａまで排気した後、電子銃６の電子ビームを用いて蒸着材料を加熱、溶融させ、蒸着させることが好ましい。
【００２０】
蒸着の際には、表面保護と磁気特性制御のために酸化性ガスを導入してもよい。導入すべき酸化性ガスとしては、酸素、オゾン、亜酸化窒素などより適宜選択することができる。これらのガスを蒸着部に導入するためのガス供給ノズル（図示せず）は、例えば、図示する遮蔽板９とシャッター１０との間に設ければよい。
【００２１】
本発明の蒸着方法は、形成する磁性層が単層でも、あるいは２層以上の多層膜でも適用可能であるが、かかる磁性層全体の厚みは１０〜５００ｎｍの範囲内で制御することが好ましい。この厚みが１０ｎｍより薄い場合はスチル耐久性が不安定となり、一方、５００ｎｍより厚いと損失増大のために電磁変換特性が低下する。また、本発明において斜め蒸着を行うにあたっては、冷却ドラムの回転方向は同方向でも逆方向でもよく、要求される電磁変換特性を満足するように設計すればよく、特に限定されるものではない。
【００２２】
なお、図示する装置において、電子ビーム６Ｂの蒸着るつぼ５内への照射位置の確認は、例えば、真空容器側面に設けられた、遮光用シャッター装置１１を備えた電子ビーム監視用覗き窓にて行うことができる。また、符号８は、真空容器内を所定の圧力に保つために設けられている真空排気ポンプを示す。
【００２３】
【実施例】
以下、本発明を実施例に基づき具体的に説明する。
実施例１
図１に示す斜め蒸着装置１を用いて、真空度１×１０3Ｐａにて、電子ビーム加熱により、高分子支持体フィルム（ベースフィルム）２としての厚み４．０μｍのアラミドフィルム（東レ（株）製、ミクトロン４ＭＡ３０）上に、蒸着るつぼ５内に収納された蒸着材料としてのＣｏを蒸着し、磁性層を形成した。
【００２４】
蒸着に際しては、蒸着材料であるＣｏの溶解時は、シャッター１０を閉じた状態で、かつ、ベースフィルム２を冷却ドラム４に抱かせた状態で静止させ、溶解のための加熱作業として電子ビームのエミッション電流を目的の蒸着膜厚が得られる電流まで徐々に上げてゆき、蒸着材料の溶解の完了とともにベースフィルム２の走行をスタートさせ、これと同時にシャッター１０を開いて蒸着を開始して、所定の走行速度まで加速した。この時のフィルムの走行状態および目的とする蒸着膜厚１００ｎｍが達成されるまでのフィルムのロス長さを下記の表１に示す。なお、蒸着膜厚はオンラインで光透過率を計測することにより測定した。
【００２５】
実施例２
実施例１において、蒸着材料の溶解の完了とともに電子ビームのエミッション電流を実施例１の半分の値まで下げた後、フィルム走行をスタートさせ、これと同時にシャッター１０を開いて、加速中にエミッション電流を実施例１と同じ値まで上げた以外は実施例１と同様にして蒸着を行った。この時のフィルムの走行状態および目的とする蒸着膜厚が達成されるまでのフィルムのロス長さを下記の表１に示す。
【００２６】
実施例３
実施例１において、蒸着材料の溶解の完了とともに電子ビームのエミッション電流を実施例１の半分の値まで下げた後、フィルム走行のスタート、加速を行い、加速走行が始まったことを確認後即座にシャッター１０を開いた以外は実施例１と同様にして蒸着を行った。この時のフィルムの走行状態および目的とする蒸着膜厚が達成されるまでのフィルムのロス長さを下記の表１に示す。
【００２７】
実施例４
実施例１において、蒸着材料の溶解時は１ｍ／ｍｉｎのスピードでフィルムを走行させ、蒸着材料の溶解の完了後にフィルム走行を加速して、これと同時にシャッター１０を開いた以外は実施例１と同様にして蒸着を行った。この時のフィルムの走行状態および目的とする蒸着膜厚が達成されるまでのフィルムのロス長さを下記の表１に示す。
【００２８】
実施例５
実施例４において、蒸着材料の溶解の完了とともに電子ビームのエミッション電流を実施例４の半分の値まで下げた後、フィルム走行を加速させ、これと同時にシャッター１０を開いて、加速中にエミッション電流を実施例４と同じ値まで上げた以外は実施例４と同様にして蒸着を行った。この時のフィルムの走行状態および目的とする蒸着膜厚が達成されるまでのフィルムのロス長さを下記の表１に示す。
【００２９】
実施例６
実施例４において、蒸着材料の溶解の完了とともに電子ビームのエミッション電流を実施例４の半分の値まで下げた後、フィルム走行を加速させ、加速走行が始まったことを確認後即座にシャッター１０を開いて、加速中にエミッション電流を実施例４と同じ値まで上げた以外は実施例４と同様にして蒸着を行った。この時のフィルムの走行状態および目的とする蒸着膜厚が達成されるまでのフィルムのロス長さを下記の表１に示す。
【００３０】
比較例１
実施例１において、蒸着材料の溶解に際しフィルムを１０ｍ／ｍｉｎのスピードで走行させようとしたが、この時点でフィルム切れが発生した。
【００３１】
比較例２
実施例１において、蒸着材料の溶解に際しフィルムを５ｍ／ｍｉｎのスピードで走行させようとしたが、フィルムが蛇行し、フィルム切れが発生した。
【００３２】
比較例３
実施例１において、高分子支持体フィルム２として厚み６．５μｍのＰＥＴフィルムを用い、蒸着材料の溶解時はフィルムを１０ｍ／ｍｉｎのスピードで走行させ、蒸着材料の溶解の完了後にフィルム走行を加速して、これと同時にシャッター１０を開いた以外は実施例１と同様にして蒸着を行った。この時のフィルムの走行状態および目的とする蒸着膜厚が達成されるまでのフィルムのロス長さを下記の表１に示す。
【００３３】
比較例４
実施例１において、高分子支持体フィルム２として厚み６．５μｍのＰＥＴフィルムを用いた以外は実施例１と同様にして蒸着を行った。この時のフィルムの走行状態および目的とする蒸着膜厚が達成されるまでのフィルムのロス長さを下記の表１に示す。
【００３４】
比較例５
実施例１において、高分子支持体フィルム２として厚み４．７μｍのＰＥＮフィルムを用い、蒸着材料の溶解時はフィルムを１０ｍ／ｍｉｎのスピードで走行させ、蒸着材料の溶解の完了後にフィルム走行を加速して、これと同時にシャッター１０を開いた以外は実施例１と同様にして蒸着を行った。この時のフィルムの走行状態および目的とする蒸着膜厚が達成されるまでのフィルムのロス長さを下記の表１に示す。
【００３５】
比較例６
実施例１において、高分子支持体フィルム２として厚み４．７μｍのＰＥＮフィルムを用いた以外は実施例１と同様にして蒸着を行った。この時のフィルムの走行状態および目的とする蒸着膜厚が達成されるまでのフィルムのロス長さを下記の表１に示す。
【００３６】
【表１】
【発明の効果】
以上説明してきたように、本発明によれば、長尺芳香族ポリアミドフィルムを用いた蒸着方法において、蒸着材料の溶解によるフィルムの熱負けや破断の発生がなく、かつ、従来に比しフィルムのロスの発生を低減することができ、従ってフィルムの走行、蒸着を安定して行うことができるフィルムの蒸着方法を提供することができる。
【図面の簡単な説明】
【図１】本発明に係る斜め蒸着装置を示す概略模式図である。
【符号の説明】
１ 斜め蒸着装置
２ 長尺フィルム
３ 供給ロール
４ 冷却ドラム
５ 蒸発るつぼ
６ 電子銃
６Ｂ 電子ビーム
７ 巻き取りロール
８ 真空排気ポンプ
９ 遮蔽板
１０ シャッター
１１ 遮光用シャッター装置[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a film deposition method, and more specifically, heat loss or breakage of a film does not occur even by heating for dissolving a deposition material in a deposition preparation stage, and loss of a film occurs at this stage. The present invention relates to a film deposition method capable of minimizing the above.
[0002]
[Prior art]
Deposition techniques for polymer films are applied to a wide variety of uses such as magnetic tapes for data backup and video recording, packaging films, and electrode films.
[0003]
In particular, in magnetic recording applications, with the increase in capacity and miniaturization of magnetic recording systems, it is required to increase the density of the medium and reduce the thickness of the tape. In addition, since the binder is not included, the filling ratio of the magnetic layer is high, the saturation magnetization can be increased, and since the film can be thinned, the recording demagnetization is suppressed even for short wavelength recording. It has the advantage of being advantageous in high density recording.
[0004]
As a deposition medium, conventionally, polyethylene terephthalate (PET) or polyethylene naphthalate (PEN) is used as a polymer film as a material to be deposited, and Co or Co-Ni alloy is used as a ferromagnetic metal for forming a magnetic layer as a deposition material. In these vapor deposition techniques, it is common to use an electron beam to evaporate the metal and perform continuous vapor deposition while running the polymer film in a cooling drum. Is.
[0005]
In this case, in order to continuously and stably evaporate the vapor deposition material when performing vapor deposition, it is necessary to perform a preheating operation (melting) of the vapor deposition material and the crucible. There has been a problem that the polymer film loses heat due to the radiant heat accompanying heating, leading to breakage. For this reason, techniques such as disposing an openable / closable shielding plate between the vapor deposition material and the polymer film to shut off heat or holding the polymer film on the cooling drum are used. However, since this is not sufficient, a technique is adopted in which the film is melted while running at a low speed.
[0006]
[Problems to be solved by the invention]
However, even when vapor deposition is performed using the above method, the running part at the time of melting becomes a loss even though the speed is low, so this melting work has been a factor that greatly deteriorates the use efficiency of the film. .
[0007]
Also, due to the recent demand for large-capacity recording on magnetic recording media, it has become necessary to reduce the total thickness of the tape in order to increase the winding length per tape roll, and the polymer film material has also been reduced. Even in such cases, there is a shift to high Young's modulus materials that can ensure strength.
[0008]
A typical example of the high Young's modulus film is an aromatic polyamide (aramid) film. When such an aramid film is used, the heat resistance is higher than that of PET or PEN. In the method in which the film is extremely charged by secondary electrons or recoil electrons generated in the film and melted while the film is running at a low speed, the film breaks at the time of peeling due to charging and sticking of the film to the cooling drum. The problem that it became easy to generate | occur | produce and driving | running | working also became unstable occurred.
[0009]
Therefore, the object of the present invention is to eliminate the influence of heat and electrification on the film accompanying the heating for melting when the deposition material is melted in the stage of vapor deposition preparation of the long film, and heat loss or breakage of the film occurs. It is another object of the present invention to provide a film vapor deposition method that can reduce the occurrence of film loss as compared with the prior art, and thus can stably run and vapor deposit the film.
[0010]
[Means for Solving the Problems]
In order to solve the above-described problems, the film deposition method of the present invention is a film deposition method in which a thin film is formed by vacuum deposition on a long film made of aromatic polyamide, and the deposition material is dissolved by an electron beam. The long film was run at an extremely low speed of 1 m / min or less with the shielding plate between the vapor deposition material and the long film closed, and the dissolution of the vapor deposition material was completed when the long film was dissolved. The travel of the length film is accelerated, and at the same time, the shielding plate is opened.
[0011]
Furthermore, the film deposition method of the present invention is a film deposition method in which a thin film is formed by vacuum deposition on a long film made of an aromatic polyamide, and the deposition material is dissolved while the deposition material is dissolved by an electron beam. The long film is run at an extremely low speed of 1 m / min or less with the shielding plate between the long film and the long film is closed, and when the evaporation material is completely dissolved, the long film is accelerated. And then opening the shielding plate.
[0012]
According to the present invention, by using a predetermined material for a long film and performing a vapor deposition operation according to predetermined conditions and procedures, the influence of heat on the film is minimized, and the range of films affected by heat As a result, the film can be prevented from being broken when the cooling drum is peeled off, and a good running state can be maintained during vapor deposition to perform stable vapor deposition.
[0013]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, specific embodiments of the present invention will be described in more detail.
In the vapor deposition method of the present invention, an aromatic polyamide having a high Young's modulus and excellent heat resistance is used as a polymer support film as a vapor deposition material, and a thin film of the vapor deposition material is formed on the film by vacuum vapor deposition.
[0014]
An example of a vapor deposition apparatus that can be used in the present invention is shown in FIG. The vapor deposition apparatus 1 shown in the figure is called an oblique vapor deposition apparatus. In the oblique vapor deposition method using this apparatus, the vapor of the vapor deposition material is incident on the surface of the vapor deposition material at a specific angle, and is tilted with respect to the vapor deposition material. A thin film of a vapor deposition material made of crystal particles is formed. Specifically, in the vacuum container, the aromatic polyamide film 2 as a long film-like material to be deposited was unwound from the
[0015]
In the drawing, a shielding plate 9 provided so as to cover the
[0016]
In the present invention, when performing the above-described vapor deposition, when the vapor deposition material is melted as a vapor deposition preparation stage, the shielding plate 9 is kept closed, that is, the opening of the shielding plate 9 is closed by the
[0017]
After the preparation for vapor deposition is performed as described above, when the vapor deposition preparation is completed, the long film 2 starts to travel and the
[0018]
In the present invention, the above procedure in the vapor deposition preparation stage is important, and other conditions relating to vapor deposition may be appropriately determined according to a conventional method, and are not particularly limited. In particular, the vapor deposition method of the present invention can be suitably used when a magnetic layer is formed by vacuum vapor deposition on a long film 2 as a nonmagnetic substrate in the production of a magnetic recording medium.
[0019]
As a vapor deposition material for the magnetic layer, a ferromagnetic metal material is preferably used. Examples of the ferromagnetic metal material include single or mixed materials such as Fe, Co, and Ni, or ternary systems such as Co—Ni—Cr, Fe—Ni—N, and Co—Ni—Ta. However, it should not be particularly limited. In this case, in the oblique vapor deposition method, after evacuating the inside of the vacuum vessel in which the non-magnetic substrate 2 can travel to 10 −3 Pa, the vapor deposition material is heated and melted by using the electron beam of the electron gun 6 and vapor deposited. Is preferred.
[0020]
During vapor deposition, an oxidizing gas may be introduced for surface protection and magnetic property control. The oxidizing gas to be introduced can be appropriately selected from oxygen, ozone, nitrous oxide, and the like. A gas supply nozzle (not shown) for introducing these gases into the vapor deposition section may be provided between the shielding plate 9 and the
[0021]
The vapor deposition method of the present invention can be applied to a single magnetic layer or a multilayer film of two or more layers, but the thickness of the entire magnetic layer is preferably controlled within a range of 10 to 500 nm. If the thickness is less than 10 nm, the still durability becomes unstable. On the other hand, if the thickness is more than 500 nm, the electromagnetic conversion characteristics deteriorate due to increased loss. In addition, when performing oblique vapor deposition in the present invention, the rotation direction of the cooling drum may be the same direction or the reverse direction, and may be designed so as to satisfy the required electromagnetic conversion characteristics, and is not particularly limited.
[0022]
In the illustrated apparatus, the irradiation position of the
[0023]
【Example】
Hereinafter, the present invention will be specifically described based on examples.
Example 1
Using an oblique vapor deposition apparatus 1 shown in FIG. 1, a 4.0 μm thick aramid film (Toray Industries, Inc.) as a polymer support film (base film) 2 by electron beam heating at a vacuum degree of 1 × 10 3 Pa. Co) as a vapor deposition material accommodated in the vapor deposition crucible 5 was vapor-deposited on Mikutron 4MA30), and a magnetic layer was formed.
[0024]
During the deposition, when Co, which is a deposition material, is melted, the
[0025]
Example 2
In Example 1, the electron beam emission current was lowered to half the value of Example 1 upon completion of dissolution of the vapor deposition material, and then the film travel was started. At the same time, the
[0026]
Example 3
In Example 1, the electron beam emission current was lowered to half the value of Example 1 along with the completion of dissolution of the vapor deposition material, and then the film running was started and accelerated. Immediately after confirming that the accelerated running started Vapor deposition was performed in the same manner as in Example 1 except that the
[0027]
Example 4
In Example 1, when the deposition material was dissolved, the film was run at a speed of 1 m / min, and after the dissolution of the deposition material was completed, the film running was accelerated, and at the same time, the
[0028]
Example 5
In Example 4, the electron beam emission current was lowered to half the value of Example 4 upon completion of dissolution of the vapor deposition material, and then the film travel was accelerated. At the same time, the
[0029]
Example 6
In Example 4, the electron beam emission current was lowered to half the value of Example 4 along with the completion of the dissolution of the vapor deposition material, and then the film travel was accelerated. Vapor deposition was performed in the same manner as in Example 4 except that the emission current was increased to the same value as in Example 4 during acceleration. Table 1 below shows the film running state and the loss length of the film until the target deposited film thickness is achieved.
[0030]
Comparative Example 1
In Example 1, an attempt was made to run the film at a speed of 10 m / min during the dissolution of the vapor deposition material.
[0031]
Comparative Example 2
In Example 1, the film was caused to run at a speed of 5 m / min when the vapor deposition material was dissolved, but the film meandered and the film was broken.
[0032]
Comparative Example 3
In Example 1, a PET film having a thickness of 6.5 μm was used as the polymer support film 2, and the film was run at a speed of 10 m / min when the deposition material was dissolved, and the film running was accelerated after the dissolution of the deposition material was completed. At the same time, vapor deposition was performed in the same manner as in Example 1 except that the
[0033]
Comparative Example 4
In Example 1, vapor deposition was performed in the same manner as in Example 1 except that a PET film having a thickness of 6.5 μm was used as the polymer support film 2. Table 1 below shows the film running state and the loss length of the film until the target deposited film thickness is achieved.
[0034]
Comparative Example 5
In Example 1, a 4.7 μm-thick PEN film was used as the polymer support film 2, and the film was run at a speed of 10 m / min when the vapor deposition material was dissolved, and the film running was accelerated after the dissolution of the vapor deposition material was completed. At the same time, vapor deposition was performed in the same manner as in Example 1 except that the
[0035]
Comparative Example 6
In Example 1, vapor deposition was performed in the same manner as in Example 1 except that a PEN film having a thickness of 4.7 μm was used as the polymer support film 2. Table 1 below shows the film running state and the loss length of the film until the target deposited film thickness is achieved.
[0036]
[Table 1]
【The invention's effect】
As described above, according to the present invention, in the vapor deposition method using the long aromatic polyamide film, there is no occurrence of heat loss or breakage of the film due to dissolution of the vapor deposition material, and the film has a thickness higher than that of the conventional film. It is possible to provide a film vapor deposition method that can reduce the generation of loss, and thus can stably carry and run the film.
[Brief description of the drawings]
FIG. 1 is a schematic diagram showing an oblique deposition apparatus according to the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Diagonal vapor deposition apparatus 2
Claims (2)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001389389A JP4234338B2 (en) | 2001-12-21 | 2001-12-21 | Film deposition method |
| US10/324,008 US6852362B2 (en) | 2001-12-21 | 2002-12-20 | Film vapor deposition method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001389389A JP4234338B2 (en) | 2001-12-21 | 2001-12-21 | Film deposition method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2003193220A JP2003193220A (en) | 2003-07-09 |
| JP4234338B2 true JP4234338B2 (en) | 2009-03-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001389389A Expired - Fee Related JP4234338B2 (en) | 2001-12-21 | 2001-12-21 | Film deposition method |
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| Country | Link |
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| US (1) | US6852362B2 (en) |
| JP (1) | JP4234338B2 (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004326083A (en) * | 2003-04-09 | 2004-11-18 | Seiko Instruments Inc | Method for manufacturing mirror, and mirror device |
| US8027335B2 (en) * | 2004-05-05 | 2011-09-27 | Prodea Systems, Inc. | Multimedia access device and system employing the same |
| JP2007035161A (en) * | 2005-07-27 | 2007-02-08 | Tdk Corp | Manufacturing apparatus and manufacturing method of magnetic recording medium |
| JP4962848B2 (en) * | 2006-11-30 | 2012-06-27 | 東レフィルム加工株式会社 | Deposition film thickness control method for web-like deposition material |
| US20170344703A1 (en) | 2006-12-29 | 2017-11-30 | Kip Prod P1 Lp | Multi-services application gateway and system employing the same |
| US11316688B2 (en) | 2006-12-29 | 2022-04-26 | Kip Prod P1 Lp | Multi-services application gateway and system employing the same |
| US9602880B2 (en) | 2006-12-29 | 2017-03-21 | Kip Prod P1 Lp | Display inserts, overlays, and graphical user interfaces for multimedia systems |
| WO2008085206A2 (en) | 2006-12-29 | 2008-07-17 | Prodea Systems, Inc. | Subscription management of applications and services provided through user premises gateway devices |
| US9569587B2 (en) | 2006-12-29 | 2017-02-14 | Kip Prod Pi Lp | Multi-services application gateway and system employing the same |
| US11783925B2 (en) | 2006-12-29 | 2023-10-10 | Kip Prod P1 Lp | Multi-services application gateway and system employing the same |
| US9494746B2 (en) | 2011-11-10 | 2016-11-15 | Panduit Corp. | Shuttered LC adapter |
| US20240401185A1 (en) * | 2023-06-05 | 2024-12-05 | Li-Metal Corp. | Coating drum and system for vapor deposition |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1235808A (en) * | 1984-03-22 | 1988-04-26 | Tetsuo Oka | Vertical magnetic recording medium and process for preparation thereof |
| JPS6129417A (en) * | 1984-07-20 | 1986-02-10 | Tdk Corp | Magnetic video recording medium |
| US5161233A (en) * | 1988-05-17 | 1992-11-03 | Dai Nippon Printing Co., Ltd. | Method for recording and reproducing information, apparatus therefor and recording medium |
| JP2566096B2 (en) * | 1992-04-14 | 1996-12-25 | 富士写真フイルム株式会社 | Magnetic recording media |
| US5731068A (en) * | 1995-02-24 | 1998-03-24 | Kao Corporation | Magnetic recording medium |
-
2001
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| US6852362B2 (en) | 2005-02-08 |
| JP2003193220A (en) | 2003-07-09 |
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