JP5658135B2 - 表面改質フッ素樹脂フィルムと熱可塑性樹脂との複合体の製造方法 - Google Patents
表面改質フッ素樹脂フィルムと熱可塑性樹脂との複合体の製造方法 Download PDFInfo
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- JP5658135B2 JP5658135B2 JP2011289525A JP2011289525A JP5658135B2 JP 5658135 B2 JP5658135 B2 JP 5658135B2 JP 2011289525 A JP2011289525 A JP 2011289525A JP 2011289525 A JP2011289525 A JP 2011289525A JP 5658135 B2 JP5658135 B2 JP 5658135B2
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- thermoplastic resin
- fluororesin
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- 229920005992 thermoplastic resin Polymers 0.000 title claims description 79
- 239000002131 composite material Substances 0.000 title claims description 21
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- 229920001971 elastomer Polymers 0.000 claims description 30
- 239000005060 rubber Substances 0.000 claims description 24
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- 238000000465 moulding Methods 0.000 claims description 18
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 16
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 16
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- 239000011347 resin Substances 0.000 claims description 15
- 238000010884 ion-beam technique Methods 0.000 claims description 13
- -1 polypropylene Polymers 0.000 claims description 10
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 claims description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000806 elastomer Substances 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 6
- 238000007788 roughening Methods 0.000 claims description 6
- 229920005672 polyolefin resin Polymers 0.000 claims description 5
- 150000001336 alkenes Chemical class 0.000 claims description 4
- 238000002788 crimping Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 3
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- 229920001155 polypropylene Polymers 0.000 claims description 3
- 150000001925 cycloalkenes Chemical class 0.000 claims description 2
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 description 78
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
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- 229910001873 dinitrogen Inorganic materials 0.000 description 1
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- WSUTUEIGSOWBJO-UHFFFAOYSA-N dizinc oxygen(2-) Chemical compound [O-2].[O-2].[Zn+2].[Zn+2] WSUTUEIGSOWBJO-UHFFFAOYSA-N 0.000 description 1
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- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
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Description
また、フッ素樹脂は、その化学的安定性から、シート状またはフィルム状のものを接着剤により他の材料にラミネートして使用量の削減を図ることが難しく、例えば、化学的安定性を生かすことができる医薬品容器の栓等への利用が普及しなかった。
表面の改質効果の経時的な減少が生ずる場合、特許文献1に開示された方法で表面改質されたフッ素樹脂系生成物の使用可能期間(在庫期間)は、短期に制限される。そして、需要予測の誤りによりフッ素樹脂系生成物を材料とする次工程の生産量が減少すれば、在庫するフッ素樹脂系生成物が材料として不適格(不良品)となるおそれがある。
保持装置4は、往復移動するイオン照射装置2のいずれの位置においても、ガラス基板21の表面とイオン照射装置2との往復移動方向に直交する方向の距離が一定となる位置に、静止可能に配される。ここで「静止可能」としたのは、後述するように、保持装置4が処理室3と前室5との間を移動可能なことによる。
図4はイオン照射装置2によるイオンビーム照射の様子を示す図である。初めに、改質対象であるフッ素樹脂フィルムRFが、保持装置4のガラス基板21に固定される。フッ素樹脂とはフッ素原子を含むポリマーを意味し、たとえばポリテトラフルオロエチレン(PTFE)、変性PTFE、テトラフルオロエチレン・パーフルオロアルキルビニルエーテル共重合体(PFA)、エチレンテトラフルオロエチレン共重合体(ETFE)、ポリクロロトリフルオロエチレン(PCTFE)などが挙げられる。これらのポリマーは単体でも良く、2種類以上のポリマーの混合物であっても良い。これらのうちPTFEは最も摩擦係数が低く耐熱性も優れる為好ましい。また変性PTEFは破断伸びが高く成形性が良い為好ましい。
本発明でフィルムとは特に形状に限定されず、成形物の形状に合わせて任意に設定される。経済性の観点から厚みは薄い方が好ましいが、成形あるいは使用条件に伴う変形を考慮し任意に設定できる。フィルムの厚さは、10μm〜150μmが好ましい。
図1を参照して、フッ素樹脂フィルムRFが固定されたガラス基板21が、前室5内において保持装置4に一体化される。
自動弁27,28が開かれ、自動弁29,30,31が閉じられた状態で、真空装置6の前段真空ポンプ25が起動され、前室5および処理室3が減圧される。
前室5および処理室3が所定の真空度、例えば102Paに達したら、保持装置4が前室5から処理室3に移動され、前室5と処理室3との間の扉が閉じられる。
続いて自動弁27,28が閉じられ、自動弁29が開かれ、前段真空ポンプ25が停止されると、後段真空ポンプ26が起動される。処理室3は、後段真空ポンプ26により、一層高い真空度、例えば10−2Paにまで減圧される。
イオン照射装置2がいずれか一方の移動端からいずれか他方の移動端まで設定された回数移動したのち、イオン照射装置2の移動およびその動作が停止され、表面改質が終了する。ここで行われる表面改質は、照射されるイオンビームによりフッ素樹脂フィルムRFの表面および表面近傍の内部の分子構造を破壊し、表面の粗面化を行うものである。
図5〜図7に示される医療用ゴム製品は、プレフィルドシリンジPC内の薬液を押し出すためのピストン7である。図6、図7を参照して、ピストン7は、略円柱状の一方の端面(底面)が傘状(底面の径に較べ高さが極めて小さな円錐台の周面状)の押圧面35である。ピストン7の他方の端面には、軸心方向に設けられた雌ネジ36が開口する。ピストン7は、表面改質装置1により表面が粗面化されたフッ素樹脂フィルム(PTFEフィルム)と熱可塑性樹脂とを重ね合わせて加硫成形されることにより製造される。そのため、ピストン7は、大部分が熱可塑性樹脂で形成され、押圧面35および周面37には、熱可塑性樹脂に接合されたフッ素樹脂フィルムRFが露出する。
ゴム複合体は、医療用に限られず、ゴムが有する弾性とフッ素樹脂が有する自己潤滑性、耐薬品性、耐熱性等が求められる種々の用途、例えば工業設備のパッキン等に使用することができる。
一般にアノードレイヤーイオンソースにおいて、イオン源にかける電圧の数値の約半分の平均エネルギーをイオンに与えることが知られており、上記エネルギーを与える設定電圧は、平均エネルギーが0.8〜2.5keVであれば1.6〜5.0kV、1.2〜1.8keVであれば2.4〜3.6kVである。
以下に示す各種フッ素樹脂フィルムを使用して、下記の共通条件のもと、表1に示す印加電圧と処理回数でイオンビームを照射した。表1に、目視により行ったフィルムの変色の有無の観察結果を示す。
(1)イオン照射装置:IZOVAC社製 IZOVA BEAM CLEANING SYSTEM(アノードレイヤーイオンソース)/イオン照射装置は、ランテクニカルサービス株式会社の駆動装置により駆動
(2)設定真空度:10−2Pa
(3)フッ素樹脂フィルム:
PTFE:日本バルカー工業製、バルフロン(登録商標)、厚さ100μm
変性PTFE:日本バルカー工業製、ニューバルフロンEX1(バルフロン:登録商標)、厚さ100μm
PFA:ダイキン工業製、ネオフロンPFAフィルム(ネオフロン:登録商標)、厚さ100μm
ETFE:旭硝子株式会社製、FluonETFE(登録商標)、厚さ100μm
(4)イオン照射装置とフッ素樹脂フィルムとの距離:イオン照射装置2の移動方向に直交する方向について照射側面15の幅方向中央(図3,4の符合C)からフッ素樹脂フィルムまでの距離(図4のD)が100mm
プロセスガス:Ar,流量40sccm,処理速度 20mm/sec
熱可塑性樹脂:オレフィン系熱可塑性樹脂(日本ポリケミカル株式会社製「BC6(商品名)」)
スチレン系エラストマー:(アロン化成株式会社製「エラストマーAR−710(商品名)」)
動的架橋型熱可塑性エラストマー:(自社製)
海相−ポリプロピレン「BC6」、日本ポリケミカル株式会社製
架橋ゴム相−エチレンプロピレンジエンゴム「エスプレン670F」、住友化学株式会社製
架橋剤−ハロゲン化アルキルフェノール樹脂架橋剤「タッキロール250−III」、田岡化学工業(株)製
酸化亜鉛−酸化亜鉛2種、三井鉱山(株)製
JIS K7121−1987 示差走査熱量測定(DSC)法による融解ピーク温度の測定は、エスアイアイ・ナノテクノロジー株式会社製DSC6220を使用し、入力補償示差走査熱量測定により行った。試験片の質量は約8mgを使用し、10℃/分の速度で昇温した。
イオンビーム照射フィルムを熱可塑性樹脂との接着処理用に100mm×100mmサイズに切断した。また、各種熱可塑性樹脂を用い、射出成型機にて100mm×100mm×2.5mmのシートに成形した。
熱可塑性樹脂と表面改質フッ素樹脂フィルムとの接着は、熱プレス成型機により行った。熱プレス成型機に100mm×100mm×2mmのキャビティを有する金型を設置し、内部に熱可塑性樹脂シートと表面改質フッ素樹脂フィルムを該改質面が熱可塑性樹脂シートに面するように設置し、かつ後述の剥離強度測定の為の掴み代を作る為に未処理のフッ素樹脂フィルム(PTFEフィルム、40mm×100mm×0.1mm)を熱可塑性樹脂シートと表面改質フッ素樹脂フィルムの間に設置した。
金型に0.5MPaの圧力を加えながら加熱を開始し、所定の温度まで上昇させた。所定の温度に到達後、所定の圧力に増加させ、更に10分間保持した。圧力を保ったまま冷却を開始し、室温到達後圧力の開放と金型からのサンプルの取り出しを行った。
剥離強度は、得られた複合体を幅20mmの短冊状に切り分け、長手方向一端でフッ素樹脂フィルムと熱可塑性樹脂とを上下別々のチャックに挟み、一方を50mm/minの速度で上昇させたときの抵抗力を計測して求めた。
なお、表の剥離強度中、<0.1と示したものは全く接着しておらず測定結果が得られなかったサンプルを示す。また、数値の前に>の記号をつけたサンプルは使用したフッ素樹脂フィルムが破断したサンプルを意味し、実際の剥離強度は本試験で得られた数値以上であったことを示す。
なお、表の剥離強度中、<0.1と示したものは全く接着しておらず測定結果が得られなかったサンプルを示す。また、数値の前に>の記号をつけたサンプルは使用したフッ素樹脂フィルムが破断したサンプルを意味し、実際の剥離強度は本試験で得られた数値以上であったことを示す。
2 イオン照射装置
3 処理室
4 保持装置
5 前室
6 真空装置
7 ピストン
11 スリット
12 空間
13 アノード
14 ガス流路
15 照射側面
16 内極
17 外極
21 ガラス基板
25 前段真空ポンプ、
26 後段真空ポンプ
27、28、29、30、31 自動弁
35 押圧面
36 雌ネジ
37 周面
Claims (5)
- フッ素樹脂フィルムの表面に、印加電圧が1.5kV以上3.5kV以下のアノードレイヤーイオンソースからのイオンビームを照射して表面を粗面化する工程、および、
粗面化して得られた表面改質フッ素樹脂フィルムと熱可塑性樹脂を、該熱可塑性樹脂が流動状態を示す状態で圧着させる工程
を含むことを特徴とするフッ素樹脂と熱可塑性樹脂の複合体の製造方法であって、
熱可塑性樹脂が、ポリプロピレン樹脂、シクロオレフィン樹脂、スチレン系樹脂、オレフィン系樹脂に未架橋ゴム相としてエチレンプロピレン成分を含むオレフィン系エラストマー(TPO)、オレフィン系樹脂に架橋ゴム相としてエチレンプロピレンジエン成分を含むTPE−Vであるフッ素樹脂と熱可塑性樹脂の複合体の製造方法。 - フッ素樹脂フィルムのフッ素樹脂がポリテトラフルオロエチレン、変性ポリテトラフルオロエチレン、テトラフルオロエチレン−パーフルオロアルキルビニルエーテル共重合体、またはエチレン−テトラフルオロエチレン共重合体であることを特徴とする請求項1に記載の製造方法。
- 圧着工程を、熱可塑性樹脂の融点以上の温度で行うことを特徴とする請求項1または2に記載の製造方法。
- 圧着工程を、熱可塑性樹脂の成形温度以上の温度で行うことを特徴とする請求項1〜3のいずれかに記載の製造方法。
- 圧着が1MPa以上であることを特徴とする請求項1〜4のいずれかに記載の製造方法。
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