JP2013519756A - 分散多モード表面改質ナノ粒子を含む樹脂系 - Google Patents
分散多モード表面改質ナノ粒子を含む樹脂系 Download PDFInfo
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Abstract
Description
更に他の実施形態では、例えば、ウレタン(メタ)アクリレート、ポリエチレングリコール(マルチ)(メタ)アクリレート、及びエポキシ(マルチ)(メタ)アクリレートを含め、(メタ)アクリレート樹脂を使用してもよい。本明細書で使用するとき、用語(メタ)アクリレートは、アクリレート及び/又はメタクリレートを指し、すなわち、エチル(メタ)アクリレートは、エチルアクリレート及び/又はエチルメタクリレートを指す。
第二モードの粒子の数割合は、次のように定義される。
一般に、より小さいナノ粒子の数割合(NF2)、即ち、より小さい平均粒径D2を有する第二モードのナノ粒子の数割合は、より大きいナノ粒子の数割合(NF1)、即ち、より大きい平均粒径D1を有する第一モードのナノ粒子の数割合とほぼ等しく、実施形態によってはこの数割合以上のこともある。
本発明者は、ナノ粒子を含む樹脂系の粘度が一般に温度の上昇と共に高まることを確認した。これは、一般に、温度の上昇と共に樹脂自体の粘度が低下するという理解と一致している。しかしながら、ある程度のナノ粒子が加えられた樹脂系の場合、本発明者は、更に、温度の上昇により粘度が最初に低下した後で、更なる温度上昇によりナノ粒子を含む有樹脂系の粘度が驚くほど高くなることがあることを発見した。即ち、温度を高めることによって樹脂自体の粘度が低下するとき、ナノ粒子の存在によって、ナノ粒子含有樹脂系の全体的な粘度を上昇させる新しい流動学的挙動が起こる点に達する。本明細書で使用されるとき、用語「粒子スタッキング」は、この新しい流動学的現象を記述するために使用される。
TGAを使用して樹脂分散系のシリカ含量を測定した。分散系の約20mgの試料を白金TGAパンに入れた。パンをTGA(Q500、TA Instruments,Inc.,New Castle,DE)に装填し、空気パージガス中で30℃から900℃まで20℃/分の割合で高めた。実行後に、850℃で残っている試料の重量(初期重量の割合として)を不燃材料の重量比率として取得し、シリカ固体である生成物の重量比率として報告した。
以下の手順を除き、実施例EX−8、EX−9及びEX−11に関して説明した手順にしたがって、実施例EX−10を調製した。
Claims (20)
- 樹脂成分と、前記樹脂成分中に分散された表面改質ナノ粒子とを含む樹脂系であって、前記表面改質ナノ粒子が、多モード粒径分布であって、
平均粒径D1を有する第一モードであって、D1が50ナノメートル以上250ナノメートル以下であり、前記第一モード内のナノ粒子の数がN1である第一モードと、
平均粒径D2を有する第二モードであって、D2がD1未満であり、前記第二モードのナノ粒子の数がN2である第二モードとを含む多モード粒径分布を有し、
D2に対するD1の比率が、1.5を超え、N1に対するN2の比率が、0.5を超え、
モードにおけるナノ粒子の平均粒径と数が、透過型電子顕微鏡法によって測定される、樹脂系。 - D2が、15ナノメートル未満であり、N1に対するN2の比率が、1.5を超える、請求項1に記載の樹脂系。
- D2に対するD1の比率が、10を超える、請求項2に記載の樹脂系。
- N1に対するN2の比率が、1.5以上100以下である、請求項3に記載の樹脂系。
- D2が、20ナノメートル以上50ナノメートル以下である、請求項1に記載の樹脂系。
- D2に対するD1の比率が、2〜3である、請求項5に記載の樹脂系。
- N1に対するN2の比率が、1以上2以下である、請求項5又は6の樹脂系。
- D1が、60nm以上100nm以下である、請求項1〜7のいずれか一項に記載の樹脂系。
- 前記樹脂系が、反応成分と表面改質ナノ粒子の総重量に対して少なくとも40重量%のナノ粒子を含む、請求項1〜8のいずれか一項に記載の樹脂系。
- 前記樹脂成分が、硬化性樹脂を含む、請求項1〜9のいずれか一項に記載の樹脂系。
- 前記硬化性樹脂が、エポキシ樹脂を含む、請求項10に記載の樹脂系。
- 前記樹脂成分が、更に、反応性希釈剤を含む、請求項1〜11のいずれか一項に記載の樹脂系。
- 前記樹脂成分が、レオロジー試験法にしたがって測定されたとき、30℃で100Pa・s未満の複素粘度を有する、請求項1〜12のいずれか一項に記載の樹脂系。
- 前記樹脂系が、前記樹脂成分と前記ナノ粒子の全重量に対して少なくとも30重量%のナノ粒子を含み、前記樹脂成分中の前記ナノ粒子の分散系が、レオロジー試験法によって測定されたとき、30℃で60Pa・s未満の複素粘度を有する、請求項1〜13のいずれか一項に記載の樹脂系。
- 前記ナノ粒子が、シリカ表面を有するコアを有するナノ粒子を含む、請求項1〜14のいずれか一項に記載の樹脂系。
- 前記ナノ粒子が、前記シリカ表面へ共有結合された第1の群と、前記樹脂成分の少なくとも1つの要素と反応性を有する第2の群とを含む少なくとも1つの表面改質剤を含む、請求項15に記載の樹脂系。
- 前記樹脂系が、0.5重量%未満の溶剤を含む、請求項1〜16のいずれか一項に記載の樹脂系。
- 前記樹脂系が、硬化された、請求項1〜17のいずれか一項に記載の樹脂系を含む物品。
- 前記物品が、前記樹脂系を含浸させた繊維を含む合成物である、請求項18に記載の物品。
- 前記樹脂系が、基板の表面上の被覆である、請求項18に記載の物品。
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US30340610P | 2010-02-11 | 2010-02-11 | |
US61/303,406 | 2010-02-11 | ||
PCT/US2011/024147 WO2011100289A1 (en) | 2010-02-11 | 2011-02-09 | Resin system comprising dispersed multimodal surface -modified nanoparticles |
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JP2013519756A true JP2013519756A (ja) | 2013-05-30 |
JP2013519756A5 JP2013519756A5 (ja) | 2014-03-27 |
JP5798129B2 JP5798129B2 (ja) | 2015-10-21 |
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EP (1) | EP2534199B1 (ja) |
JP (1) | JP5798129B2 (ja) |
KR (1) | KR101910202B1 (ja) |
CN (1) | CN102741338B (ja) |
ES (1) | ES2706398T3 (ja) |
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KR20200135773A (ko) * | 2018-03-22 | 2020-12-03 | 로저스코포레이션 | 다중 모드 유전체 필러를 포함하는 용융 가공성 열가소성 복합재 |
WO2023136331A1 (ja) * | 2022-01-13 | 2023-07-20 | 日産化学株式会社 | 粒度分布を有するシリカゾル及びその製造方法 |
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- 2011-02-09 EP EP11705348.8A patent/EP2534199B1/en not_active Not-in-force
- 2011-02-09 WO PCT/US2011/024147 patent/WO2011100289A1/en active Application Filing
- 2011-02-09 JP JP2012552938A patent/JP5798129B2/ja active Active
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- 2011-02-09 CN CN201180007990.6A patent/CN102741338B/zh not_active Expired - Fee Related
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JP2021516711A (ja) * | 2018-03-22 | 2021-07-08 | ロジャーズ コーポレーション | 複数の異なる誘電充填材を含む溶融加工可能な熱可塑性複合材 |
KR102441151B1 (ko) | 2018-03-22 | 2022-09-07 | 로저스코포레이션 | 다중 모드 유전체 필러를 포함하는 용융 가공성 열가소성 복합재 |
JP7179862B2 (ja) | 2018-03-22 | 2022-11-29 | ロジャーズ コーポレーション | 複数の異なる誘電充填材を含む溶融加工可能な熱可塑性複合材 |
JP2019178303A (ja) * | 2018-03-30 | 2019-10-17 | 太陽インキ製造株式会社 | 硬化性樹脂組成物、ドライフィルム、硬化物、および、電子部品 |
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WO2023136331A1 (ja) * | 2022-01-13 | 2023-07-20 | 日産化学株式会社 | 粒度分布を有するシリカゾル及びその製造方法 |
JP7360098B1 (ja) | 2022-01-13 | 2023-10-12 | 日産化学株式会社 | 粒度分布を有するシリカゾル及びその製造方法 |
CN117177941A (zh) * | 2022-01-13 | 2023-12-05 | 日产化学株式会社 | 具有粒度分布的硅溶胶和其制造方法 |
Also Published As
Publication number | Publication date |
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ES2706398T3 (es) | 2019-03-28 |
KR101910202B1 (ko) | 2018-10-19 |
US8871853B2 (en) | 2014-10-28 |
US20150099833A1 (en) | 2015-04-09 |
US9718954B2 (en) | 2017-08-01 |
EP2534199A1 (en) | 2012-12-19 |
PL2534199T3 (pl) | 2019-04-30 |
WO2011100289A1 (en) | 2011-08-18 |
KR20120134119A (ko) | 2012-12-11 |
US20120309870A1 (en) | 2012-12-06 |
CN102741338B (zh) | 2015-04-15 |
CN102741338A (zh) | 2012-10-17 |
EP2534199B1 (en) | 2019-01-16 |
JP5798129B2 (ja) | 2015-10-21 |
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