JP4805840B2 - 表面改質されたナノ粒子を含有する溶液 - Google Patents
表面改質されたナノ粒子を含有する溶液 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
- B01J13/0026—Preparation of sols containing a liquid organic phase
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31511—Of epoxy ether
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31678—Of metal
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31786—Of polyester [e.g., alkyd, etc.]
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- Paints Or Removers (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Description
表面微細構成−方法I
試験すべきサンプルを金/パラジウム(Au/Pd)でスパッタリングして、コントラストを強化した。「ウィコ(WYKO)」NT−300光学干渉計(アリゾナ州ツクソンのウィコ(Wyko)(Tucson,AZ))から得られたもの)を用いて、2.0ミリメートル(mm)×2.5mmの少なくとも2つの面を測定した。得られた画像をフィルター掛けして、傾斜を除去した。以下の表面微細構成数値を得られたデータから計算した。
Ra(ナノメートル(nm))−粗さ平均
Rq(mm)−二乗平均粗さ
試験すべきサンプルを金/パラジウム(Au/Pd)でスパッタリングして、コントラストを強化した。「ウィコ(WYKO)」NT−300光学干渉計(アリゾナ州ツクソンのウィコ(Wyko)(Tucson,AZ))から得られたもの)を用いて、2.4ミリメートル(mm)×1.9mmの4つの面をVSIモードで測定した。得られた画像をフィルター掛けして、傾斜を除去した。以下の表面微細構成数値を得られたデータから計算した。
Ra(nm)−粗さ平均
Rq(mm)−二乗平均粗さ
トリアルコキシシランカップリング剤を用いて粒子表面を疎水的に改質した表面改質シリカナノ粒子を次の通り調製した。
メカニカルスターラーおよびリフラックスコンデンサが装着された500ミリリットル(mL)丸底三口フラスコに250グラム(g)の「ナルコ(NALCO)」2326を秤量して入れた。15.36gのIOTMSおよび281.25gのMOPの溶液をビーカー内で別個に調製した。
メカニカルスターラーおよびリフラックスコンデンサが装着された500mL丸底三口フラスコに250グラムgの「ナルコ(NALCO)」2326を秤量して入れた。21.76gのIOTMSおよび281.25gのMOPの溶液をビーカー内で別個に調製した。「ナルコ(NALCO)」2326ゾルを攪拌しつつ、開口を経由してフラスコにIOTMS/MOP溶液を添加した。その後、ビーカーを追加45.5gのMOPでリンスし、それを攪拌された混合物に後で添加した。完全に添加した後、フラスコの開口を閉じ、フラスコを油浴に入れた。その後、油浴を80℃に加熱し、反応を放置して約16時間にわたり進めた。ゾルをフロースルーオーブン内で150℃で乾燥させて、表面改質ナノ粒子(SILICA−B)を回収した。
N−(3−トリエトキシシリルプロピル)メトキシエトキシエチルカルバメート(PEG2TES)を次の通り調製した。マグネチックスターラーが装着された250mL丸底フラスコに35gのDIGLYMEおよび77gのMEKを添加し、回転蒸発に供して水を除去した。その後、68.60gの3−(トリエトキシシリル)プロピルイソシアネートをフラスコに添加し、その後、約3ミリグラムのDBTDLを添加し、混合物を攪拌した。反応は穏やかな発熱を伴って進行した。反応を約16時間にわたり行った。その時点で、IR分光分析によると、イソシアネートの存在が示されなかった。90℃での回転蒸発を経由して溶媒の残りを除去して、104.46gのPEG2TESを多少粘性の液体としてもたらした。
トルエン中のPMMA20重量%の溶液をビーカー内で調製して、PMM原液を提供した。この溶液のサンプルに改質粒子(SILICA−AまたはSILICA−B)、1−メトキシ−2−プロパノールアセテート(PMアセテート)およびトルエンを以下の表で示した量で添加した。PMMA濃度を被覆可能な溶液の全重量の10重量%で維持した。表に記載したPAアセテート濃度は溶媒(すなわちPMアセテート+トルエン)の全重量を基準にした重量%である。改質粒子濃度はポリマー(PMMA)の全乾燥重量を基準にした重量%である。
幅2インチ(5.1cm)×長さ3インチ(7.6cm)のガラススライド(ニューヨーク州コーニングのコーニング社(Corning,Inc.(Corning,NY))から得られたもの)上に溶液を被覆した。ミクロピペット(エッペンドルフ(Eppendorf))を用いて、流体の75マイクロリットルをスライド上に置き、放置して重力下で流した。被覆されたスライドを250°F±2°F(121℃)の温度に設定されたホットプレート上に直接約2.5分にわたり置いた。その後、乾燥させたサンプルを目視で検査し、上述した「方法I」または「方法II」により表面微細構成を試験した。
PMアセテートおよびSILICA−Bの異なる量を用いて上の「被覆可能な溶液の調製」により溶液を調製した。PMアセテートがないか、またはSILICA−Bがない比較例も調製した。上述した「被覆されたスライドの調製」によりガラススライド上に溶液を被覆した。乾燥させたサンプルの表面微細構成を「方法I」により試験した。用いたPMアセテートおよびSILICA−Bの量および表面微細構成結果を表3に示している。
PMアセテートおよびSILICA−Aの異なる量を用いて上記「被覆可能な溶液の調製」により8種類の溶液を調製した。PMアセテートがない比較例も調製した。上記「被覆されたスライドの調製」によりガラススライド上に溶液を被覆した。乾燥させたサンプルの表面微細構成を「方法I」により試験した。用いたPMアセテートおよびSILICA−Aの量および表面微細構成結果を表3に示している。
200グラムのSILICA−Cおよび56.7gのHDDAを1リットル丸底大口フラスコ内で組み合わせた。回転蒸発を経由して溶媒を除去した。得られた材料は室温で高粘度のゲルであった。SILICA−C/HDDAゲルは約40重量%のSILICA−Cを含んでいた。
室温で成分を組み合わせて20gのサンプルを得ることにより、SILICA−Aおよび液体(IOA、トルエンまたはPMアセテート)の異なる量を調製した。C25クエット幾何学を用いる「ボーリン・C−VOR・レオメータ(BOHLIN C−VOR Rheometer)」(ニュージャージー州イーストブランズウィックのボーリン・インストルメンツ(Bohlin Instruments,Inc.(East Brunswick,NJ))によりサンプルごとの溶液レオロジーを測定した。制御された応力スイープを25℃で1×10-3〜1×10+3の剪断応力範囲内で完了した。「ペルチエ(PELTIER)」ユニットを用いて温度を±0.2℃内に制御した。ニュートンモデルを測定されたデータおよび記録された粘度に当てはめた。溶液の組成および粘度結果を表5に示し、図5にグラフで示している。
IOA、トルエンおよびSILICA−Bの異なる量に関する組成に対する粘度の三元プロットを作成した。C25クエット幾何学を用いる「ボーリン・C−VOR・レオメータ(BOHLIN C−VOR Rheometer)(ニュージャージー州イーストブランズウィックのボーリン・インストルメンツ(Bohlin Instruments(East Brunswick,NJ)から得られたもの)により溶液レオロジーを測定した。制御された応力スイープを25℃で1×10-3〜1×10+3の剪断応力範囲内で完了した。温度を+/−0.2℃の範囲内で、ペルチェ(PELTIER)を用いて制御した。ニュートンモデルを測定されたデータおよび記録された粘度に当てはめた。溶液の組成および粘度結果を表6に示し、図6にグラフで示している。
Claims (3)
- (a)表面改質ナノ粒子、
(b)蒸気圧VP1を有する第1の液体、および
(c)VP1より低い蒸気圧VP2を有し、第1の液体に混和性である第2の液体、
を含む塗料溶液であって、
前記ナノ粒子が第2の液体より第1の液体に相溶性が大であり、
前記第2の液体は硬化性である塗料溶液。 - 塗膜均一性を強化する方法であって、
(a)請求項1に記載の塗料溶液を基材の表面に被着させる工程、
(b)第1の液体の少なくとも一部を除去する工程、および
(c)第2の液体を硬化および/または架橋させる工程
を含む方法。 - 請求項2に記載の方法によって製造された被覆基材。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/722,177 | 2003-11-25 | ||
US10/722,177 US7189768B2 (en) | 2003-11-25 | 2003-11-25 | Solution containing surface-modified nanoparticles |
PCT/US2004/033586 WO2005056698A1 (en) | 2003-11-25 | 2004-10-12 | Solution containing surface-modified nanoparticles |
Publications (3)
Publication Number | Publication Date |
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JP2007512412A JP2007512412A (ja) | 2007-05-17 |
JP2007512412A5 JP2007512412A5 (ja) | 2007-11-29 |
JP4805840B2 true JP4805840B2 (ja) | 2011-11-02 |
Family
ID=34591973
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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JP2006541155A Expired - Fee Related JP4805840B2 (ja) | 2003-11-25 | 2004-10-12 | 表面改質されたナノ粒子を含有する溶液 |
Country Status (8)
Country | Link |
---|---|
US (1) | US7189768B2 (ja) |
EP (1) | EP1697469B1 (ja) |
JP (1) | JP4805840B2 (ja) |
KR (1) | KR101129780B1 (ja) |
CN (1) | CN1886469B (ja) |
AT (1) | ATE389698T1 (ja) |
DE (1) | DE602004012606T2 (ja) |
WO (1) | WO2005056698A1 (ja) |
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US7189768B2 (en) | 2007-03-13 |
EP1697469B1 (en) | 2008-03-19 |
ATE389698T1 (de) | 2008-04-15 |
KR20060130568A (ko) | 2006-12-19 |
DE602004012606T2 (de) | 2009-04-30 |
WO2005056698A1 (en) | 2005-06-23 |
CN1886469B (zh) | 2011-07-13 |
EP1697469A1 (en) | 2006-09-06 |
KR101129780B1 (ko) | 2012-03-26 |
JP2007512412A (ja) | 2007-05-17 |
US20050113489A1 (en) | 2005-05-26 |
CN1886469A (zh) | 2006-12-27 |
DE602004012606D1 (de) | 2008-04-30 |
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