JP2010503033A - コア−シェル型ナノ粒子 - Google Patents
コア−シェル型ナノ粒子 Download PDFInfo
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- JP2010503033A JP2010503033A JP2009527049A JP2009527049A JP2010503033A JP 2010503033 A JP2010503033 A JP 2010503033A JP 2009527049 A JP2009527049 A JP 2009527049A JP 2009527049 A JP2009527049 A JP 2009527049A JP 2010503033 A JP2010503033 A JP 2010503033A
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- polymer
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- nanoparticles
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- 150000004706 metal oxides Chemical class 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 61
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- 125000001453 quaternary ammonium group Chemical group 0.000 description 3
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- 150000003512 tertiary amines Chemical group 0.000 description 3
- 125000001302 tertiary amino group Chemical group 0.000 description 3
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- 238000004627 transmission electron microscopy Methods 0.000 description 3
- BCAGFJXMCZSAHD-UHFFFAOYSA-N 1,2-bis(2-iodoethoxy)ethane Chemical compound ICCOCCOCCI BCAGFJXMCZSAHD-UHFFFAOYSA-N 0.000 description 2
- VTPNYMSKBPZSTF-UHFFFAOYSA-N 1-ethenyl-2-ethylbenzene Chemical compound CCC1=CC=CC=C1C=C VTPNYMSKBPZSTF-UHFFFAOYSA-N 0.000 description 2
- XHUZSRRCICJJCN-UHFFFAOYSA-N 1-ethenyl-3-ethylbenzene Chemical compound CCC1=CC=CC(C=C)=C1 XHUZSRRCICJJCN-UHFFFAOYSA-N 0.000 description 2
- WHFHDVDXYKOSKI-UHFFFAOYSA-N 1-ethenyl-4-ethylbenzene Chemical compound CCC1=CC=C(C=C)C=C1 WHFHDVDXYKOSKI-UHFFFAOYSA-N 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- CEYHHQSTMVVZQP-UHFFFAOYSA-N 2-ethenoxyethanamine Chemical compound NCCOC=C CEYHHQSTMVVZQP-UHFFFAOYSA-N 0.000 description 2
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
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- 239000004115 Sodium Silicate Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- OKJPEAGHQZHRQV-UHFFFAOYSA-N Triiodomethane Natural products IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 description 2
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- FUSUHKVFWTUUBE-UHFFFAOYSA-N buten-2-one Chemical compound CC(=O)C=C FUSUHKVFWTUUBE-UHFFFAOYSA-N 0.000 description 2
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Abstract
【選択図】なし
Description
(a)ポリマーを含むコア材料と、
(b)金属酸化物を含むシェル材料と
を含むコア−シェル型ナノ粒子を含む、光学コーティングの形成に好適な組成物が提供される。
(a)ポリマーを含むコア材料と、
(b)金属酸化物、好ましくはシリカを含むシェル材料と
を含むコア−シェル型ナノ粒子を含むコーティング組成物であって、上記ナノ粒子がロッド状または芋虫状の形態を有する、組成物が提供される。特定の実施形態においては、ポリマーは、カチオン的に安定化されたコポリマーミセル、より好ましくは、ジブロックまたはトリブロックコポリマーを含む。他の好ましい実施形態においては、ポリマーは、カチオン的に安定化されたラテックスを含む。
(a)コア−シェル型ナノ粒子を含む組成物を基材に適用するステップと、
(b)上記組成物を硬化させることによってネットワークを強化し、そしてポリマーコアを除去するステップと
を含み、このコア−シェル型ナノ粒子が、ポリマーを含むコア材料と、金属酸化物を含むシェル材料とを含む、方法が提供される。
(式中、raは、コアの半径であり、rbは、外側のシェルの半径である)。
[実施例1]
ブトゥアン(Buetuen),V;アームズ(Armes),S.P.;ビリンガム(Billingham),N.C.、Chem.Commun.、1997年、671〜672頁に記載の方法に従いグループ移動重合を用いてモノマーを逐次付加させることによりPDPA23−PDMA68ジブロックコポリマーを合成した。一連の単分散に近いポリ(メチルメタクリレート)を較正基準として用いたゲル浸透クロマトグラフィー分析から、Mnが18000であり、Mw/Mnが1.08であることが示された。PDPAおよびPDMAブロックの平均重合度は、1H NMR分光を用いることにより、それぞれ23および68と推定された。
実施例1のようにグループ移動重合を用いてモノマーを逐次付加することによりPDPA23−PDMA68ジブロックコポリマーを合成した。
グループ移動重合を用いてモノマーを逐次添加することによりPDPA23−PDMA68ジブロックコポリマーを合成し、PDPA23−PDMA68ジブロックコポリマーの非架橋型ミセルを実施例1に記載したように調製した。
PEO45−PDMA29−PDPA76トリブロックコポリマーをPEOベースのマクロ開始剤を用いた原子移動ラジカル重合により合成した。まず、マクロ開始剤(1.00g、0.463mmol)を25mlの一頚フラスコに加え、次いで、吸引/窒素サイクルを3回行うことにより脱気した後、DMA(2.18g、13.88mmol、目標架橋度30)、2,2’−ビピリジン(144.5mg、0.925mmol)、次いで、脱気した95/5v/vIPA/水混合物3.2mlを加えた。この溶液を40℃の油浴に入れて均質になるまで撹拌した。次いで、塩化銅(I)(45.8mg、0.463mmol)を加えて反応を40℃で3.5時間窒素中で連続撹拌しながら実施した。この時間が経過した後、1H NMR分光で測定したDMAモノマーの反応率は96%に到達した。
予め低重合させたテトラエトキシシランを調製するために、テトラエトキシシラン(58.4g)の2−プロパノール(159.0g)溶液を撹拌しながら、水(53.6g、12.2重量%)および酢酸(5.9g)を添加した。24時間後、この混合物を2−プロパノール(160.7g)で所望の濃度に希釈した。結果として得られた混合物のpH値を濃硝酸(1.3g)を加えて1.0に低下させた。
ネオクリルXK−30(4.41g、DSMネオレジンズより入手可能な42.5%アクリルコポリマー)を水(10.00g)で処理した。次いで、テトラメトキシシラン(10.00ml)を室温で2時間かけて加えた。添加が完了した後、混合物を室温で1.5時間撹拌し、次いで、エタノールで希釈した(108.4g)。
Claims (15)
- コア−シェル型ナノ粒子を含む光学コーティング組成物であって、前記ナノ粒子が、
(a)ポリマーを含むコア材料と、
(b)金属酸化物を含むシェル材料と
を含む、組成物。 - 前記コア材料が、カチオン性である、請求項1に記載の組成物。
- 前記ポリマーが、ポリエステル、ポリアミド、ポリウレタン、ポリスチレン、ポリ(メタ)アクリレート、これらのコポリマーおよび組合せから選択される、請求項1または2に記載の組成物。
- 前記ポリマーが、ラテックス、ジブロックコポリマー、トリブロックコポリマー、およびこれらの組合せから選択される、請求項1〜3のいずれか一項に記載の組成物。
- 前記ポリマーが、カチオン性ポリマーから選択される、請求項1〜4のいずれか一項に記載の組成物。
- 金属酸化物が、シリカである、請求項1〜5のいずれか一項に記載の組成物。
- 前記組成物が、バインダーを含む、請求項1〜6のいずれか一項に記載の組成物。
- 前記組成物が、無機酸化物を含むバインダーを含む、請求項1〜7のいずれか一項に記載の組成物。
- 前記ナノ粒子の潜在的な空隙率が5%〜90%である、請求項1〜8のいずれか一項に記載の組成物。
- 請求項1〜9のいずれか一項に記載の組成物で少なくとも一部がコーティングされた基材。
- 請求項1〜10のいずれか一項に記載の組成物でコーティングされた基材を含む物品。
- コア−シェル型ナノ粒子を含むコーティング組成物であって、前記ナノ粒子が、
(a)ポリマーを含むコア材料と、
(b)金属酸化物を含むシェル材料と
を含み、前記ナノ粒子が、ロッドまたは芋虫状の形態を有する、組成物。 - コア−シェル型ナノ粒子を含む組成物を基材に適用するステップと、前記組成物を硬化させるステップとを含む、光学コーティングの形成方法であって、前記コア−シェル型ナノ粒子が、ポリマーを含むコア材料と、金属酸化物を含むシェル材料とを含む、方法。
- コア−シェル型ナノ粒子の、光学コーティングのための使用。
- コア−シェル型ナノ粒子の、薄膜コーティングのための使用。
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