JP6583645B2 - 有機無機ハイブリッドナノ粒子 - Google Patents
有機無機ハイブリッドナノ粒子 Download PDFInfo
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- JP6583645B2 JP6583645B2 JP2017193762A JP2017193762A JP6583645B2 JP 6583645 B2 JP6583645 B2 JP 6583645B2 JP 2017193762 A JP2017193762 A JP 2017193762A JP 2017193762 A JP2017193762 A JP 2017193762A JP 6583645 B2 JP6583645 B2 JP 6583645B2
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Description
a)有機コロイド粒子をテンプレートとして提供する工程と;
b)無機酸化物前駆体を添加する工程と;
c)テンプレート上に前駆体から無機シェル層を形成し、コアシェルナノ粒子を得る工程と、
を含む製造方法に関する。
a)有機コロイド粒子をテンプレートとして提供する工程と;
b)少なくとも1種の無機酸化物前駆体を添加する工程と;
c)テンプレート上に前駆体から無機シェル層を形成し、コアシェルナノ粒子を得る工程と、
を含み、テンプレートが合成高分子両性電解質を含む、または、換言すれば、有機コロイド粒子が合成高分子両性電解質をベースにしている、
有機無機ハイブリッドコアシェルナノ粒子の製造方法を提供する。
・第三級アミン基を有するモノマー等の、プロトンと結合することができるペンダント基を有する化合物を含む、少なくとも1種のカチオン性または塩基性モノマー(M1)と;
・カルボン酸基を含有するモノマー等の、プロトンを生成することができるペンダント基を有する化合物を含む、少なくとも1種のアニオン性または酸性モノマー(M2)と;
・少なくとも1種の中性または非イオン性モノマー(M3)、好ましくは、非水溶性または疎水性のコモノマーと;
・任意選択により少なくとも1種の架橋性モノマー(M4)と;
から得られる共重合体である。
・少なくとも1種のモノマーM1を0.1〜40モル%と;
・少なくとも1種のモノマーM2を0.1〜40モル%と;
・少なくとも1種のモノマーM3を18〜98.8モル%と;
・少なくとも1種のモノマーM4を0〜2モル%(M1、M2、M3、およびM4の合計は合わせて100%となる)と;
から得られる共重合体である。
・少なくとも1種のモノマーM1を5〜40モル%と;
・少なくとも1種のモノマーM2を0.5〜20モル%と;
・少なくとも1種のモノマーM3を38〜94.5モル%と;
・少なくとも1種のモノマーM4を0〜2モル%と;
から得られるカチオン性共重合体であり、高分子両性電解質はM2モノマー単位よりM1モノマー単位を多く含み、正味の正電荷を有する。
・アミノ官能性(メタ)アクリレート類および(メタ)アクリルアミド類からなる群から選択される少なくとも1種のモノマーM1を8〜20モル%と;
・カルボン酸基を有する(メタ)アクリル系モノマーからなる群から選択される少なくとも1種のモノマーM2を1〜4モル%と;
・C1〜C18アルキル(メタ)アクリレート類からなる群から選択される少なくとも1種のモノマーM3を76〜91モル%と;
から得られるカチオン性共重合体である。
・基材に本発明のコーティング組成物を塗布する工程と;
・塗布された被膜層を乾燥および硬化させる工程と;
を含む、基材上に多孔質無機酸化物被膜を製造する方法に関する。
・基材に本発明のコーティング組成物を塗布する工程と;
・塗布された被膜層を乾燥および硬化させる工程と;
を含む、反射防止(AR)コーティングされた透明基材の製造方法に関する。
[材料および方法]
[高分子両性電解質分散液]
表1は、欧州特許第2178927号明細書の実験部分に記載の手順に従って得られる、水性分散液の形態の複数の共重合体の幾つかの特性を示す。これらの分散液は、水中での共重合体の濃度が約20質量%およびpHが約4(ギ酸で酸性にした)であり、約80℃で約30分間の加熱を行った。PA1〜PA4は、両性電解質三元共重合体であり、PE1は、比較のカチオン性共重合体である。共重合体のMwは、25〜40kDaの範囲であった。
マルバーン・ナノ(Malvern Nano)ZSを使用して、25℃のKCl水溶液(1mmol/L)10ml中に分散液1滴を添加したものについて後方散乱モードで、分散粒子の粒子サイズを測定した。この装置は、希釈試料のゼータ電位測定にも使用した(M3 PALSおよびMPT−2装置を用いた)。
被膜を製造し、硬化させて少なくとも1日経過した後に、ガードコ(Gardco)3363鉛筆硬度試験機を用い、基材に対して300gの公称荷重を使用して、片面コーティングされた基材で被膜の硬度を評価した。ASTM D3363試験方法に従い、最初の1cmを無視して表面の損傷を判断した。
島津(Shimadzu)UV−2450分光光度計を用いて、コーティングされた透明基材の反射および透過を評価した。反射率測定用付属装置を用いて、入射角度5°で相対鏡面反射率を測定した。透過を測定するために、積分球付属装置を試料室に取り付け、入射角度は0°とした。波長域425〜675nmについて平均反射値を算出する。特記しない限り、両面コーティングされた基材で測定を行う。
PA3の水性分散液を10%HClを用いて約pH2.5の酸性にし、60℃より高温に加熱し、室温に冷却した後、希釈してDLS装置に入れ;粒子サイズ、pHおよびゼータ電位を同時に測定できるようにした。アンモニア水を一定量ずつ添加することにより、分散液のpHを徐々に上昇させた。粒子サイズは約pH6.5まで約25nmのままであり、その後、粒子サイズは急速に増大することが判明した。ゼータ電位はこの範囲で約35mVから−5mVに低下し、正味電荷が正から負に変化したことが分かる。
DLSに必要な希釈工程を行わずに実施例1を繰り返し、アンモニア水の各添加後に、分散液を約90℃に加熱した。加熱の前後に粒子サイズおよびpHを測定した。図1に示す結果から、pHと温度の両方を変化させることにより、この高分子両性電解質コロイド分散液の平均粒子サイズを20〜50nmの範囲に調節できることが分かる。pH6.5にした試料は、加熱時にゲル化したことに留意されたい。
pH4のPA3分散液の試料を希釈してDLS装置に入れ;粒子サイズを温度の関数として測定した。図2に示すグラフから、分散液は少なくとも約80℃以下で安定であることが分かる。pHを約3に調節した後、実験を繰り返したが、その場合、温度が約60℃より高温に上昇すると、粒子サイズは減少した。同様に、pHを約2に調節した後、粒子サイズは減少した。
これらの実験では、異なる量のシリカ前駆体をPA3分散液に添加した後、得られたコロイド分散液を使用してコーティング組成物を製造し、その後、コーティングされたガラス基材を製造した。
実施例4を繰り返したが、異なる量のTMOSを使用し、TEOSゾルの添加量を無添加(実施例5)から、算出されたSiO2対高分子両性電解質の比が2.5となる量まで変えた。組成データおよび測定した反射特性を表2に要約する。TEOSの量を増加すると反射が幾分高くなる(またはAR特性が幾分低下する)と結論付けることができる。これは、TEOSが分散粒子の結合剤として機能し、そのため気孔率が低下することにより説明でき、それにより機械的特性が予想通り向上する。
実施例4と同様に、コロイドコアシェルPA3/TMOS分散液を製造した後、硝酸でpH2.5の酸性にして減圧下で約80℃に加熱し、その時、水の蒸発を観察した。この分散液は初期固形分含有率が約4質量%であったが、この時点では約13.5質量%と測定された(また、依然として透明であった)。
MMA、DMAEMAおよびMAAモノマー単位を含有する高分子両性電解質は、開始剤としての過硫酸アンモニウム、連鎖移動剤としてのチオグリコール酸イソオクチル、およびリン酸ベースのアニオン性界面活性剤(Rhodafac RS−710)の存在下、MMAとDMAEMA(mol比85:15)を85℃で60分間乳化重合することにより調製した。このようにして得られた分散液の安定性を改善するために、非イオン性界面活性剤を添加した。室温に冷却した後、ギ酸溶液を30分間添加してpH4にした。得られた高分子両性電解質分散液の固形分含有率は20質量%であり、粒子サイズは約78nm(z−平均粒子サイズ;PDI0,1)であり、Mwは40kDa(GPC)であった。
Claims (28)
- コアシェルナノ粒子を含むコロイド分散液であって、
前記コアシェルナノ粒子が、有機コアと、無機酸化物前駆体から形成された無機シェルとを備え、
前記有機コアが合成有機高分子両性電解質を含み、
前記コアシェルナノ粒子が、動的光散乱(DLS)で測定した場合、20〜200nmの平均粒子サイズを有し、
前記合成有機高分子両性電解質が、
・第三級アミン基を有する、少なくとも1種のカチオン性または塩基性モノマー(M1)と;
・カルボン酸基を含有する、少なくとも1種のアニオン性または酸性モノマー(M2)と;
・少なくとも1種の中性または非イオン性モノマー(M3)と;
・任意選択により少なくとも1種の架橋性モノマー(M4)と;
から得られる共重合体である、コロイド分散液。 - 前記M1が、ペンダントのアミノ官能基を有するビニルモノマーである、請求項1に記載のコロイド分散液。
- 前記合成有機高分子両性電解質は、ビニル系コモノマーから作製された付加重合体である、請求項1または2に記載のコロイド分散液。
- 前記合成有機高分子両性電解質が、
(a)少なくとも1種のモノマーM1を0.1〜40モル%と;
(b)少なくとも1種のモノマーM2を0.1〜20モル%と;
(c)少なくとも1種のモノマーM3を18〜98.8モル%と;
(d)少なくとも1種のモノマーM4を0〜2モル%と;
から得られる共重合体である、請求項1〜3のいずれか一項に記載のコロイド分散液。 - 前記合成有機高分子両性電解質が、
(a)少なくとも1種のモノマーM1を5〜40モル%と;
(b)少なくとも1種のモノマーM2を0.5〜20モル%と;
(c)少なくとも1種のモノマーM3を38〜94.5モル%と;
(d)少なくとも1種のモノマーM4を0〜2モル%と;
から得られるカチオン性共重合体である、請求項4に記載のコロイド分散液。 - 前記高分子両性電解質が、
(a)アミノ官能性(メタ)アクリレート類および(メタ)アクリルアミド類からなる群から選択される少なくとも1種のモノマーM1を8〜20モル%と;
(b)カルボン酸基を有する(メタ)アクリル系モノマーからなる群から選択される少なくとも1種のモノマーM2を1〜4モル%と;
(c)C1〜C18アルキル(メタ)アクリレート類からなる群から選択される少なくとも1種のモノマーM3を76〜91モル%と;
から得られるカチオン性共重合体である、請求項1〜5のいずれか一項に記載のコロイド分散液。 - DLSで測定した場合、前記コアシェルナノ粒子の平均粒子サイズが20〜150nmである、請求項1〜6のいずれか一項に記載のコロイド分散液。
- 前記コアシェルナノ粒子が、機能性化合物をさらに含む、請求項1〜7のいずれか一項に記載のコロイド分散液。
- 前記有機コアは、合成高分子両性電解質、水、有機溶媒、界面活性剤および機能性化合物を含む、請求項1〜8のいずれか一項に記載のコロイド分散液。
- 前記機能性化合物が有機化合物または溶媒を含む、請求項8または9に記載のコロイド分散液。
- 前記有機コアが、合成高分子両性電解質、水、および有機溶媒から実質的になる、請求項1〜7のいずれか一項に記載のコロイド分散液。
- 前記無機酸化物前駆体が、金属塩、金属キレート、および有機金属化合物の少なくとも一つを含む、請求項1〜11のいずれか一項に記載のコロイド分散液。
- 前記無機シェルが、Si、Al、Ti、およびZrの酸化物からなる群から選択される少なくとも1種を含む、請求項1〜12のいずれか一項に記載のコロイド分散液。
- 前記無機酸化物前駆体が、アルコキシシランを含む、請求項1〜13のいずれか一項に記載のコロイド分散液。
- 前記アルコキシシランが、テトラメトキシシランおよび/またはテトラエトキシシランを含む、請求項14に記載のコロイド分散液。
- 前記無機シェルが、TEM、クライオTEM、SAXS、SANS、またはAFMで測定した際に、1〜20nmの厚さを有する、請求項1〜15のいずれか一項に記載のコロイド分散液。
- 前記無機シェルが、無機酸化物中の金属としてSiを80モル%以上含む、請求項1〜16のいずれか一項に記載のコロイド分散液。
- 請求項1〜17のいずれか一項に記載のコロイド分散液を含む、組成物。
- 請求項1〜17のいずれか一項に記載のコロイド分散液と、少なくとも1種の溶媒と、任意選択により少なくとも1種の結合剤とを含む、基材上に反射防止層を製造するための、コーティング組成物。
- 前記結合剤が、Si、Al、Ti、およびZrの金属塩、金属キレート、および有機金属化合物からなる群から選択される少なくとも1種の無機酸化物前駆体である、請求項19に記載のコーティング組成物。
- コーティングされた基材の製造方法であって、
請求項19または20に記載のコーティング組成物を前記基材に塗布する工程と;
前記塗布された被膜層を乾燥および任意に硬化させる工程と;
を含む、方法。 - 反射防止コーティングされた基材を製造するための、請求項21に記載の方法。
- 反射防止コーティングされた透明基材を製造するための、請求項22に記載の方法。
- 請求項1〜17のいずれか一項に記載のコロイド分散液の製造方法であって、
a)有機コロイド粒子をテンプレートとして提供する工程と;
b)少なくとも1種の無機酸化物前駆体を添加する工程と;
c)前記テンプレート上に前記前駆体から無機シェル層を形成し、コアシェルナノ粒子を得る工程と;
を含み、
前記有機コロイド粒子が合成有機高分子両性電解質を含み、前記コアシェルナノ粒子が動的光散乱(DLS)で測定した場合、20〜200nmの平均粒子サイズを有し、
前記合成有機高分子両性電解質が、
・第三級アミン基を有する、少なくとも1種のカチオン性または塩基性モノマー(M1)と;
・カルボン酸基を含有する、少なくとも1種のアニオン性または酸性モノマー(M2)と;
・少なくとも1種の中性または非イオン性モノマー(M3)と;
・任意選択により少なくとも1種の架橋性モノマー(M4)と;
から得られる共重合体である、方法。 - 前記有機コロイド粒子が、前記合成有機高分子両性電解質を水性媒体に分散させることにより、およびpHと温度の両方を変化させて粒子サイズを調節することにより提供される、請求項24に記載の方法。
- 前記有機コロイド粒子が、前記合成有機高分子両性電解質を水性媒体に分散させることにより、および温度、pH、塩濃度、および溶媒組成を含む条件を選択して粒子サイズを調節することにより提供される、請求項24に記載の方法。
- 前記工程a)が、機能性化合物が前記有機コロイド粒子に含まれるように、機能性化合物を得られた分散液に添加することをさらに含む、請求項24〜26のいずれか一項に記載の方法。
- 前記コアシェルナノ粒子が、DLSで測定した場合、20〜150nmの平均粒子サイズを有する、請求項24〜27のいずれか一項に記載の方法。
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