JP2018529812A - 3dプリンティング用組成物 - Google Patents
3dプリンティング用組成物 Download PDFInfo
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Abstract
Description
本出願は、2015年09月25日に出願された大韓民国特許出願第10−2015−0136968号に基づく優先権の利益を主張し、該当韓国特許出願の文献に開示されたすべての内容は本明細書の一部として組み入れるものとする。
本出願は、3Dプリンティング用樹脂組成物、これを利用した3Dプリンティング方法及びこれを含む立体形状に関する。
MXaOb
磁性体粒子として軟磁性体(Soft Type)であるFeOFe2O3粒子(Multi−Magnetic Domains、平均粒径約50nm:Field Emission Scanning Electron Microscopeで測定(DLS利用))、エポキシ樹脂として国都化学製KSR−177及び硬化剤として四国化成製C11ZAのイミダゾール系硬化剤を、各々5:90:5(FeOFe2O3:KSR−177:C11ZA)の重量割合で混合して樹脂組成物を製造した。
磁性体流体の粒径が100nmであること以外は、実施例1と同一の方法で樹脂組成物を製造し、立体形状を形成した。
磁性体粒子、樹脂及び硬化剤の含量が各々10:90:5の重量割合で含まれること以外は、実施例1と同一の方法で樹脂組成物を製造し、立体形状を形成した。
磁性体粒子の粒径が200nmであること以外は、実施例1と同一の方法で樹脂組成物を製造し、立体形状を形成した。
磁性体粒子としてMnOFe2O3粒子(Multi−Magnetic Domains、平均粒径約100nm:Field Emission Scanning Electron Microscopeで測定(DLS利用))を使用したこと以外は、実施例2と同一の方法で樹脂組成物を製造し、立体形状を形成した。
磁性体粒子として強磁性体(Hard Type)であるFeOFe2O3粒子(Single−Magnetic Domain、平均粒径約100nm)、ビスフェノール系エポキシ樹脂及び硬化剤を、各々5:95:5の重量割合で混合して樹脂組成物を製造した。
磁性体粒子として強磁性体(Hard Type)であるFe粒子(Single−Magnetic Domain、平均粒径約50nm)を使用し、磁性体粒子、樹脂及び硬化剤の含量が各々5:90:5の重量割合で含まれること以外は、比較例1と同一の方法で樹脂組成物を製造し、立体形状を形成した。
磁性体粒子として強磁性体(Hard Type)であるStOFe2O3粒子(Single−Magnetic Domain、平均粒径約100nm)を使用し、磁性体粒子、樹脂及び硬化剤の含量が各々5:90:5の重量割合で含まれること以外は、比較例1と同一の方法で樹脂組成物を製造し、立体形状を形成した。
常温で乾燥した磁性体粒子を振動試料型磁力計(SQUID−Vibrating Sample Magnetometer、韓国基礎科学支援研究院測定)に入れて、外部磁場を±1teslaでのH−Sカーブ(VSMカーブ)を利用して保磁力及び飽和磁化値Msを測定した。
実施例及び比較例で磁場印加直後にサーモカプラを差し込んで立体形状内部の温度を確認する。
(1)肉眼、触感
組成物の硬化後、硬化物が冷却された後に覆したときに流れるか否かを確認した後、金属スパチュラにより硬化物の押され程度を確認することで硬化を確認した。前記で流れ性があって硬化物が押される場合、硬化されなかったことを確認し得る。
組成物の熱硬化の前後、エポキシ基のintensity(約900cm−1)とフェニル基のintensity(約1500cm−1)の割合を利用して転換率(%)で計算し、硬化程度を確認する。
磁場の印加後の熱硬化されたサンプルを、切断DSCにより温度上昇速度10℃/minで300℃まで上昇させる時に発生する吸熱ピーク区間での残存熱量(J/g)を測定し、硬化程度を確認する。
Claims (24)
- 2以上の磁区を有し、
外部磁場のないときは磁区が不規則に配列されて外部磁場により磁化される磁性体粒子及び
熱硬化性樹脂を含む
3Dプリンティング用組成物。 - 磁性体粒子は、保磁力が1〜200kOeの範囲内にある
請求項1に記載の3Dプリンティング用組成物。 - 磁性体粒子は、25℃で飽和磁化値が20〜150emu/gの範囲内にある
請求項1または2に記載の3Dプリンティング用組成物。 - 磁性体粒子の平均粒径は、20〜300nmの範囲内にある
請求項1から3のいずれか1項に記載の3Dプリンティング用組成物。 - 磁区の平均サイズは、10〜50nmの範囲内にある
請求項1から4のいずれか1項に記載の3Dプリンティング用組成物。 - 磁性体粒子は、下記化学式1を満足する
請求項1から5のいずれか1項に記載の3Dプリンティング用組成物。
[化学式1]
MXaOb
前記化学式1で、Mは、金属または金属酸化物であり、
Xは、Fe、Mn、Co、NiまたはZnを含み、
|a×c|=|b×d|を満足し、
前記cは、Xの陽イオン電荷であり、
前記dは、酸素の陰イオン電荷である。 - Mは、Fe、Mn、Mg、Ca、Zn、Cu、Co、Sr、Si、Ni、Ba、Cs、K、Ra、Rb、Be、Li、Y、Bまたはこれらの酸化物である
請求項6に記載の3Dプリンティング用組成物。 - 磁性体粒子は、化学式1の化合物の混合物または化学式1の化合物に無機物がドーピングされた化合物を含む
請求項6または7に記載の3Dプリンティング用組成物。 - 磁性体粒子は、熱硬化性樹脂100重量部に対して、0.01〜25重量部で含まれる
請求項1から8のいずれか1項に記載の3Dプリンティング用組成物。 - 磁性体粒子は、磁性体クラスタを形成する
請求項1から9のいずれか1項に記載の3Dプリンティング用組成物。 - 磁性体粒子は、磁性転換によって振動する
請求項1から10のいずれか1項に記載の3Dプリンティング用組成物。 - 前記熱硬化性樹脂は、少なくとも一つ以上の熱硬化性官能基を含む
請求項1から11のいずれか1項に記載の3Dプリンティング用組成物。 - 熱硬化性官能基は、エポキシ基、グリシジル基、イソシアネート基、ヒドロキシ基、カルボキシル基またはアミド基を含む
請求項12に記載の3Dプリンティング用組成物。 - 熱硬化剤をさらに含む
請求項1から13のいずれか1項に記載の3Dプリンティング用組成物。 - 熱硬化剤は、アミン硬化剤、イミダゾール硬化剤、フェノール硬化剤、リン硬化剤または酸無水物硬化剤を含む
請求項14に記載の3Dプリンティング用組成物。 - フィラーをさらに含む
請求項1から15のいずれか1項に記載の3Dプリンティング用組成物。 - フィラーは、有機フィラー、無機フィラー、またはこれらの混合物を含む
請求項16に記載の3Dプリンティング用組成物。 - 分散剤をさらに含む
請求項1から17のいずれか1項に記載の3Dプリンティング用組成物。 - 請求項1から18のいずれか1項に記載の3Dプリンティング用組成物を塗布して立体形状を形成する段階を含む
3Dプリンティング方法。 - 塗布された組成物に磁場を印加する段階をさらに含む
請求項19に記載の3Dプリンティング方法。 - 磁場を印加する段階は、100kHz〜1GHzの周波数で50A〜500Aの電流で20秒〜60分間磁場をかける
請求項20に記載の3Dプリンティング方法。 - 磁場を印加する段階は、少なくとも2段階以上のマルチプロファイル方式を含む
請求項20または21に記載の3Dプリンティング方法。 - マルチプロファイル方式は、
100kHz〜1GHzの周波数で、10A〜80Aの電流で20秒〜10分間磁場を印加する第1段階、
80A〜130Aの電流で20秒〜10分間磁場を印加する第2段階及び
150A〜500Aの電流で5秒〜5分間磁場を印加する第3段階
を含む
請求項22に記載の3Dプリンティング方法。 - 請求項1から18のいずれか1項に記載の3Dプリンティング用組成物の硬化物を含む
立体形状。
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