JP5688032B2 - ポリシロキサンポリエステル及び無機ナノ粒子の複合体 - Google Patents
ポリシロキサンポリエステル及び無機ナノ粒子の複合体 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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Description
この例は、無機粒子が表面改質の無いTiO2粒子であり、これを添加された極性ポリシロキサン樹脂を用いて高い透過度のフィルムを形成できることを実証する。
ルチル型TiO2を、Chiruvoluらの米国特許出願第11/645,084号明細書(発明の名称:ポリマー及び金属/半金属酸化物ナノ粒子の複合体並びにそれら複合体の形成方法)の例1に本質的に記載されているレーザー熱分解法(引用することにより本明細書の内容とする)によって製造した。このTiO2粒子は、透過電子顕微鏡写真の検査から決定される7〜10nmの一次粒径、及び160m2/gを超えるBET表面積を有した。
AS4000樹脂は、Momentive Performance Materials (CT,USA)から市販されている、透明な、耐摩耗性シリコーンハードコート樹脂である。いくつかの他のポリシロキサンとは違って、AS4000樹脂は、極性溶媒中で相応して可溶性である極性ポリマーである。この製造業者から得られる樹脂は、メタノール、n−ブタノール及びイソプロパノールを含む溶媒の混合物に分散される。
上記のように調製したルチル型TiO2メタノール分散体(10重量%)をAS4000樹脂と混合して、50重量%又は60重量%TiO2を有する複合体を形成した。各複合体を、Laurell WS−400B−NPP−Lite装置を用いてスピンコートして、ガラス又はシリコンウェハ上にフィルムを形成した。これらのフィルムの透過度を、基準としてガラススライドを用い、SINCO UV−可視分光計上で測定した。これらフィルムの屈折率値及び厚みを、SCI FilmTek 3000装置上で測定した。測定したRI値は全て632nmでのところであった。
この例は、例1の高透過度フィルムに対する比較例である。
ルチル型TiO2を、上記例1に本質的に記載されているレーザー熱分解法によって製造した。ヘキサメチルジシラザン(HMDZ,Sigma Aldrich製)とオクタメチルシクロテトラシロキサン(D4,Gelest Inc)のブレンドを、粒子表面改質剤として用いた。ビーズミルプロセスにより、メチルエチルケトン(MEK)中で、HMDZ及びD4を用いてルチル型TiO2を改質し、以下に説明する操作を続けた。先ず、TiO2をMEK中でHMDZを用いて1時間処理し、その後ビーズミルに導入した。このミル処理中に、HMDZ及びD4をこのミル混合物に3段階で添加した。得られた二次粒径をMalvern ZetaSizer(商標)装置を用いて動的光散乱法(DLS)で評価した。DLS測定で明らかになった粒径分布を図3に示す。ここで、二次粒子の大部分は、110.2nmの直径を有した。より小さな粒子群は、約12.45nmに二次粒径のピークを有していた。したがって、TiO2粒子は、HMDZ及びD4を用いる改質後、3重量%のMEKにおいて良好な分散体を形成した。
上記のように調製された、MEK中で表面改質されたTiO2分散体0.7g量を、Gelest OE(商標)41(2パートフレキシブル光学封入剤(OE41)、Gelest, Inc.製、主成分はPDMSであり、パートA0.65g、パートB0.65g)と混合し、0.5時間超音波処理した。その後MEKを、ロータリーエバポレータを用いて液体から除去した。そしてこの液体を、ブレードコーターを用いてガラス上に複合体フィルムとしてキャストし、40μmの厚みを得た。その後このフィルムを150℃で2時間硬化させた。この複合体フィルム中のTiO2の含有量は、約35重量%であった。
Claims (22)
- 第1のポリシロキサンポリマー及び無機粒子を含んで成る複合体組成物であって、
前記無機粒子が250nm以下の平均粒径を有し、有機表面改質を実質的に有さず、そして
前記第1のポリシロキサンポリマーの側基の5〜50数パーセントが、前記無機粒子との相互作用を安定化する極性官能基を有し、
前記極性官能側基が、−ROH、−RNH2、−RSH、−RCN、−RNO、−RCOOH及び−RXから成る群より選ばれ、Xは、F、Cl、Br又はIであり、Rは、有機基である、
複合体組成物。 - 前記無機粒子が、金属酸化物を含む請求項1に記載の複合体組成物。
- 前記無機粒子が、100nm以下の平均粒径を有する請求項1に記載の複合体組成物。
- 前記無機粒子が、前記平均粒径の4倍を超える一次粒径を有する粒子を事実上含まない請求項3に記載の複合体組成物。
- 前記無機粒子の少なくとも95%の粒子が、平均一次粒径の60%を超え、且つ平均一次粒径の140%未満の一次粒径を有する請求項3に記載の複合体組成物。
- 前記第1のポリシロキサンポリマーが、極性官能基を有する請求項1に記載の複合体組成物。
- 前記第1のポリシロキサンポリマーが、ホモポリマーである請求項6に記載の複合体組成物。
- 前記第1のポリシロキサンポリマーが、コポリマーである請求項6に記載の複合体組成物。
- 第2のポリシロキサンポリマーをさらに含んで成る請求項1に記載の複合体組成物。
- 複合体を形成する方法であって、分散剤液体中に十分に分散させた無機粒子と第1のポリシロキサンポリマーを溶解させる溶媒中の前記第1のポリシロキサンポリマーとを混合して、配合物を作製することを含み、
前記無機粒子は、250nm以下の平均粒径を有し、有機表面改質を実質的に有さず、そして
前記ポリシロキサンポリマーの側基の5〜50数パーセントが、前記無機粒子との相互作用を安定化する極性官能基を有し、
前記極性官能側基が、−ROH、−RNH2、−RSH、−RCN、−RNO、−RCOOH及び−RXから成る群より選ばれ、Xは、F、Cl、Br又はIであり、Rは、有機基である、
複合体を形成する方法。 - 前記無機粒子が、金属酸化物を含む請求項10に記載の方法。
- 前記無機粒子が、流動ベースプロセスにおいて合成されている請求項10に記載の方法。
- 前記無機粒子が、アルコール中に分散されている請求項10に記載の方法。
- 前記ポリシロキサンポリマーの前駆体が、前記分散剤液体とは異なる溶媒に溶解されており、前記分散剤液体及び前記ポリマー前駆体の前記溶媒が混和性である請求項10に記載の方法。
- 前記ポリシロキサンポリマーが、極性官能基を含む請求項10に記載の方法。
- 第2のポリシロキサンポリマーを前記無機粒子及び前記第1のポリシロキサンポリマーの配合物と混合することを、さらに含んで成る請求項10に記載の方法。
- 所望の構造物中に前記配合物を作成し、そして前記配合物を乾燥して液体を除去することをさらに含んで成る請求項10に記載の方法。
- 分散用液体、無機粒子及び第1のポリシロキサンポリマーを含んで成る分散体であって、
前記無機粒子が250nm以下の平均粒径を有し、有機表面改質を実質的に有さず、そして
前記ポリシロキサンポリマーの側基の5〜50数パーセントが、前記無機粒子との相互作用を安定化する極性官能基を有し、
前記極性官能側基が、−ROH、−RNH2、−RSH、−RCN、−RNO、−RCOOH及び−RXから成る群より選ばれ、Xは、F、Cl、Br又はIであり、Rは、有機基である、
分散体。 - 前記分散用液体がアルコールを含む請求項18に記載の分散体。
- 前記無機粒子が、100nm以下の平均粒径を有する請求項18に記載の分散体。
- 前記ポリシロキサンポリマーが、極性官能基を有する請求項18に記載の分散体。
- 前記無機粒子がドーパントを含む請求項18に記載の分散体。
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US8314176B2 (en) | 2012-11-20 |
US20120289637A1 (en) | 2012-11-15 |
JP2015120919A (ja) | 2015-07-02 |
WO2010080684A3 (en) | 2010-10-14 |
WO2010080684A2 (en) | 2010-07-15 |
EP2385968B1 (en) | 2015-11-04 |
US8658726B2 (en) | 2014-02-25 |
US20130217821A1 (en) | 2013-08-22 |
JP2012514682A (ja) | 2012-06-28 |
KR101657729B1 (ko) | 2016-09-19 |
EP2385968A2 (en) | 2011-11-16 |
KR20110117140A (ko) | 2011-10-26 |
CN104072993A (zh) | 2014-10-01 |
US20100174024A1 (en) | 2010-07-08 |
CN102272218B (zh) | 2014-07-16 |
EP2385968A4 (en) | 2013-03-06 |
US8404771B2 (en) | 2013-03-26 |
CN102272218A (zh) | 2011-12-07 |
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