JPWO2018194064A1 - 積層体及びその製造方法 - Google Patents
積層体及びその製造方法 Download PDFInfo
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- JPWO2018194064A1 JPWO2018194064A1 JP2019513654A JP2019513654A JPWO2018194064A1 JP WO2018194064 A1 JPWO2018194064 A1 JP WO2018194064A1 JP 2019513654 A JP2019513654 A JP 2019513654A JP 2019513654 A JP2019513654 A JP 2019513654A JP WO2018194064 A1 JPWO2018194064 A1 JP WO2018194064A1
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Images
Classifications
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Abstract
Description
本発明の一実施形態に係る積層体は、プラスチック基材(A)と、プラスチック基材(A)の表面に設けられ、JIS K 7244に規定される昇温速度2℃/分の動的粘弾性試験により測定される25℃における貯蔵弾性率が0.01〜5GPaであり、tanδの値が0.1〜2.0である有機ポリマー硬化物層(B)と、有機ポリマー硬化物層(B)の表面に設けられ、有機ポリマーと金属酸化物ナノ粒子とが共有結合している有機無機複合層(C)と、有機無機複合層(C)の表面に設けられ、セラミック又は金属の二次粒子が堆積した無機層(D)とを含む。
プラスチック基材(A)は、有機ポリマー若しくは樹脂、又はその溶液を用いて成型された成型物やフィルムであれば特に限定されない。プラスチック基材(A)は、ポリエチレン、ポリプロピレン等に代表されるポリオレフィン系樹脂;ポリエチレンテレフタレート樹脂、ポリブチレンテレフタレート(PBT)樹脂、ポリカーボネート(PC)樹脂、ポリカーボネート−ポリブチレンテレフタレート(PC/PBT)樹脂等の熱可塑性ポリエステル樹脂;アクリロニトリル−スチレン樹脂、アクリロニトリル−ブタジエン−スチレン(ABS)樹脂、アクリロニトリル−スチレン−アクリレート(ASA)樹脂等のスチレン系樹脂;ポリメチルメタクリレート樹脂、アクリル樹脂、塩化ビニル、塩化ビニリデン、ポリアミド樹脂、ポリフェニレンエーテル樹脂、ポリオキシメチレン樹脂、ポリウレタン樹脂、エポキシ樹脂、ポリイミド、ポリアミドイミド、テフロン(登録商標)等の耐熱樹脂;繊維強化プラスチック(Fiber-Reinforced Plastics)等のコンポジット樹脂;トリアセチルセルロース等のセルロース類、ウレタンゴム、ブタジエンゴム、スチレンーブタジエンゴム、アクリルゴム、イソプレンゴム、フッ素ゴム等のゴム類等が例示される。これらは、併用されてもよい。
後述する無機材料をエアロゾルデポジション法により成膜する際、当該プロセス法により成膜された無機層には、成膜後に収縮応力を生じる。基材がガラス基板等のような強固な無機材料である場合、密着が充分であれば、基材そのものの靭性の高さにより、応力を内蔵したまま保持することができる。一方、基材がプラスチックである場合、プラスチックは応力を保持するだけの密着力、破壊靭性を持たない。そのため、しばしば収縮応力のために基材から無機層が剥離する、無機層にクラックが発生する、緻密な無機層が形成されない等の不具合が発生し得る。
本実施形態に係る有機無機複合層(C)は、有機ポリマーをマトリックスとして金属酸化物ナノ粒子が分散した構造を有し、金属酸化物ナノ粒子表面と有機ポリマーとの間に共有結合を有する材料で構成される。金属酸化物ナノ粒子は、平均粒子径が50nm以下であるとエアロゾルデポジション法により形成される無機層(D)との密着性に優れ、クラックのない無機層が形成されやすいため好ましい。
(I)シラン変性ポリマー(c1)を含む溶液を塗布、硬化する工程、
(II)反応性シルセスキオキサン化合物(c2)を硬化する工程、
(III)表面反応性金属酸化物ナノ粒子(c3)と光硬化性樹脂(c4)とを塗布、硬化する工程等を備えている。これらの工程は、いずれか1つの工程が行われてもよく、複数の工程が行われてもよい。
工程c1では、有機ポリマーや樹脂に対してアルコキシシランを化学反応によって導入したシラン変性ポリマー(c1)が用いられる。アルコキシシランの導入には、アルコキシシランをそのまま共有結合させる方法、アルコキシシランをあらかじめ縮合してから共有結合させる方法、シランカップリング剤を用いる方法等の従来公知の方法が有機ポリマーや樹脂の種類に応じて適宜選択されればよい。いずれの方法でも、アルコキシシランをゾル−ゲル反応によって硬化させることで、有機ポリマーと共有結合したシリカ粒子が得られる。中でも、アルコキシシランをあらかじめ縮合してから共有結合させる方法は、生成するシリカ粒子の粒子径を制御しやすく、所望の粒子径のシリカ粒子を得やすいため好ましい。アルコキシシランオリゴマーを有機ポリマーや樹脂に共有結合させたシラン変性ポリマーの作製方法が特に限定されない。一例を挙げると、シラン変性ポリマーは、例えば、特開2001−059011号公報、特開2004−300238号公報、特開2004−269793号公報、特開2000−281756号公報等の参考特許に記載の方法等で作製され得る。
工程c2では、光又は熱硬化性の官能基を有するシルセスキオキサン(c2)が用いられる。反応性シルセスキオキサン(c2)の官能基は特に限定されない。一例を挙げると、官能基は、エポキシ基、チオール基、アクリル基、メタクリル基、ビニル基、オキセタニル基、アミノ基、アルコキシ基、ヒドロシリル基等である。反応性シルセスキオキサン(c2)の作製方法が特に限定されない。一例を挙げると、反応性シルセスキオキサン(c2)は、特開2007−217673号公報、特開2007−291313号公報、特開2009−108109号公報等の参考特許に記載の方法等で作製され得る。
工程c3では、表面反応性金属酸化物ナノ粒子(c3)と光硬化性樹脂(c4)とが用いられる。表面反応性金属酸化物ナノ粒子(c3)は特に限定されない。一例を挙げると、表面反応性金属酸化物ナノ粒子(c3)は、酸化ケイ素(シリカ)、酸化ジルコニウム、酸化チタン、酸化アルミニウム、酸化亜鉛、酸化ニオブ、酸化インジウム、酸化スズ、酸化セリウム、酸化アンチモン、酸化モリブデン等のナノ粒子である。表面反応性金属酸化物ナノ粒子(c3)は、表面処理時の反応性が優れる点から、特にシリカナノ粒子が好ましい。表面反応性金属酸化物ナノ粒子(c3)は、併用されてもよい。
セラミックや金属の二次粒子を堆積させた無機層(D)は、エアロゾルデポジション法によって形成される。なお、本実施形態において、「二次粒子」とは、セラミックや金属の粒子を吹付け構成される無機層が堆積される際に当該粒子が有機無機複合層中に入り込み/又は結合した粒子をいう。
(I)シラン変性ポリマー(c1)を含む溶液を塗布し硬化する工程、
(II)反応性シルセスキオキサン化合物(c2)を塗布し硬化する工程、
(III)表面反応性金属酸化物ナノ粒子(c3)と光硬化性樹脂(c4)とを塗布し硬化する工程、
のうち少なくとも1つを含む、(3)に記載の積層体の製造方法。
(有機ポリマー硬化物層(B)の形成)
アクリル系紫外線硬化塗料XSR−5N(荒川化学工業(株)製、多官能ウレタンアクリレート、アクリルエステル、光重合開始剤の混合物)9.0gにメチルエチルケトン4.5g、プロピレングリコールモノメチルエーテル11.4g、ナノシリカの有機溶剤分散体PGM−2140Y(粒子径10〜15nm、日産化学(株)製)12.6gを加え、充分に攪拌して塗料を調製した。この塗料をポリカーボネートシート(A1)(帝人(株)製 厚さ2mm)の上にワイヤーバーを用いて塗工し、80℃で90秒乾燥後、50mJ/cm2の紫外線を照射し約10μmの仮硬化した有機ポリマー硬化物層(B)がコーティングされた積層体(B1)を得た。なお、本塗料で得られる膜単独の25℃における貯蔵弾性率は3.2GPa、tanδは0.14であった。これらの値は、DMS−6100という装置(販売者:セイコーインスツルメンツ(株))を用いてJIS K 7244に規定の試験方法に準拠し、測定開始温度−60℃、測定終了温度100℃、昇温速度2℃/分、測定周波数10Hzの測定条件で動的粘弾性測定を実施することにより算出された。
シラン変性ポリマー(c1)として、シラン変成エポキシ樹脂「コンポセランE102B」(荒川化学工業(株)製)を用いた。コンポセランE102B 48.7gに、酸無水物系硬化剤「リカシッド MH−700」(新日本理化(株)製)4.6g、硬化触媒「キュアゾール 2E4MZ」(四国化成(株)製)0.6g、メチルエチルケトン 46.1gを加え、充分に攪拌して塗料を調製した。この塗料を先に得られた積層体(B1)の上にワイヤーバーを用いて塗工し、80℃で90秒乾燥後、120℃で30分間硬化させ、その後600mJ/cm2の紫外線を照射し、約3μmの有機無機複合層(C)が形成された積層体(C1)を得た。
図1に示されるような、成膜チャンバ、エアロゾルチャンバ、真空ポンプ及びキャリアガス発生装置を備える一般的な構成のエアロゾルデポジション(AD)装置を使用した。また、無機層(D)の形成には、酸化アルミニウム粉末を用いた。粉末の成膜前処理として、120℃〜250℃にて、乾燥処理を行い、乾燥した酸化アルミニウム粉末を用いて、AD法により室温で無機材料層を形成し試料を作製した。成膜においては、乾燥空気を3〜5L/分の流量で、エアロゾルチャンバに導入し、酸化アルミニウム微粒子(二次粒子)を分散したエアロゾルを生成した。以上の条件によって積層体上にAD法を行い積層体(D1)を得た。
(有機ポリマー硬化物層(B)の形成)
アクリル系紫外線硬化塗料XSR−5N(荒川化学工業(株)製)9.0gにメチルエチルケトン4.5g、プロピレングリコールモノメチルエーテル11.4g、ナノシリカの有機溶剤分散体PGM−2140Y(粒子径10〜15nm、日産化学(株)製)12.6gを加え、充分に攪拌して塗料を調製した。この塗料をポリカーボネートシート(A1)(帝人(株)製 厚さ2mm)の上にワイヤーバーを用いて塗工し、80℃で90秒乾燥後、50mJ/cm2の紫外線を照射し半硬化させることで約10μmのコーティングが設けられた積層体(B2)を得た。なお、本塗料を最終硬化させて得られる膜単独の25℃における貯蔵弾性率は3.2GPa、tanδは0.14であった。
シルセスキオキサン(c2)として、チオール基を有するシルセスキオキサン化合物「コンポセランSQ107」(荒川化学工業(株)製)を用いた。コンポセランSQ107 31.1gに、トリアリルイソシアヌレート「タイク」(日本化成(株)製)12.5g、開始剤「イルガキュア184」(BASF製)0.07g、プロピレングリコールモノメチルエーテル 56.3gを加え、充分に攪拌して塗料を調製した。この塗料を先に得られた積層体(B2)の上にワイヤーバーを用いて塗工し、80℃で90秒乾燥後、600mJ/cm2の紫外線を照射し下層の(B2)層共々完全硬化させることで、約3μmの有機無機複合層(C)が設けられた積層体(C2)を得た。
図1に示されるような、成膜チャンバ、エアロゾルチャンバ、真空ポンプ及びキャリアガス発生装置を備える一般的な構成のエアロゾルデポジション(AD)装置を使用した。また、無機層(D)の形成には、酸化アルミニウム粉末を用いた。粉末の成膜前処理として、120℃〜250℃にて、乾燥処理を行い、乾燥した酸化アルミニウム粉末を用いて、AD法により室温で無機材料層を形成し試料を作製した。成膜においては、乾燥空気を3〜5L/分の流量で、エアロゾルチャンバに導入し、酸化アルミニウム微粒子を分散したエアロゾルを生成した。以上の条件によって積層体(C2)に対して、AD法を行い積層体(D2)を得た。
ポリカーボネートシート(A1)(帝人(株)製 厚さ2mm)の上に、上記積層体(C1)を得た際と同様の条件で有機無機複合層を形成し、積層体(C1’)を得た。この積層体に、上記積層体(D1)を得た際と同様の条件で無機層を形成し、積層体(D1’)を得た。
使用する塗料の固形分をアクリル系紫外線硬化塗料XSR−5N(荒川化学工業(株)製)のみに変更した以外は上記積層体(B1)を得た際と同様の条件で約10μmのコーティングが設けられた積層体(B2’)を得た。なお、得られた膜単独の25℃における貯蔵弾性率は1.2GPa、tanδは0.18であった。この積層体に、上記積層体(D1)を得た際と同様の条件で無機層を形成し、積層体(D2’)を得た。
上記実施例1〜2及び比較例1〜2により作製された積層体に対して、無機層(D)が、
(1)適切な目標膜厚(5μm前後)であるか、
(2)成膜後初期クラックが発生しないか、
(3)アルコール滴下の外的刺激によりクラックの成長がないか、
(4)研磨等による刺激により、白濁やクラックの成長がないかについて確認した。結果を表1に示す。なお、表1に示されるアルコールテストは、AD法により成膜された膜が所望の強度を有していない場合、アルコール等の液体を滴下すると滴下部分からクラックが生じることから、膜の強度を評価するために行われる試験である。
XSR−5N:アクリル系紫外線硬化塗料 XSR−5N
E102B:コンポセランE102B
SQ107:コンポセランSQ107
※1 研磨テストにおいて膜剥離が生じたが、クラックは発生しなかった。
※2 初期クラックが発生していたため、この試験は行わなかった。
12 台座
13 積層体
14 ロータリーポンプ
15 ガスボンベ
16 無機材料
17 エアロゾル発生器
18 ノズル
Claims (4)
- プラスチック基材(A)と、
前記プラスチック基材(A)の表面に設けられ、JIS K 7244に規定される昇温速度2℃/分の動的粘弾性試験により測定される25℃における貯蔵弾性率が0.01〜5GPaであり、tanδの値が0.1〜2.0である有機ポリマー硬化物層(B)と、
前記有機ポリマー硬化物層(B)の表面に設けられ、有機ポリマーと金属酸化物ナノ粒子とが共有結合している有機無機複合層(C)と、
前記有機無機複合層(C)の表面に設けられ、セラミック又は金属の二次粒子を含む無機層(D)とを含む、積層体。 - 前記有機ポリマー硬化物層(B)は、光硬化性樹脂の硬化物を含む、請求項1に記載の積層体。
- プラスチック基材(A)の表面に、JIS K 7244に規定する昇温速度2℃/分の動的粘弾性試験により測定される25℃における貯蔵弾性率が0.01〜5GPaであり、かつ、tanδの値が0.1〜2.0である有機ポリマー硬化物層(B)を形成する工程と、
前記有機ポリマー硬化物層(B)の表面に、有機ポリマーと金属酸化物ナノ粒子とが共有結合している有機無機複合層(C)を形成する工程と、
前記有機無機複合層(C)の表面に、エアロゾルデポジション法にてセラミック又は金属の二次粒子を堆積させた無機層(D)を形成する工程とを含む、積層体の製造方法。 - 前記有機無機複合層(C)を形成する工程は、以下の(I)〜(III)
(I)シラン変性ポリマー(c1)を含む溶液を塗布し硬化する工程、
(II)反応性シルセスキオキサン化合物(c2)を塗布し硬化する工程、
(III)表面反応性金属酸化物ナノ粒子(c3)と光硬化性樹脂(c4)とを塗布し硬化する工程、
のうち、少なくとも1つを含む、請求項3に記載の積層体の製造方法。
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