JP5221237B2 - 微粒子固定化無機材料及びその製造方法 - Google Patents
微粒子固定化無機材料及びその製造方法 Download PDFInfo
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- JP5221237B2 JP5221237B2 JP2008203483A JP2008203483A JP5221237B2 JP 5221237 B2 JP5221237 B2 JP 5221237B2 JP 2008203483 A JP2008203483 A JP 2008203483A JP 2008203483 A JP2008203483 A JP 2008203483A JP 5221237 B2 JP5221237 B2 JP 5221237B2
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- inorganic material
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
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- RMTGISUVUCWJIT-UHFFFAOYSA-N n-[3-[3-aminopropoxy(dimethoxy)silyl]propyl]-1-phenylprop-2-en-1-amine;hydrochloride Chemical compound Cl.NCCCO[Si](OC)(OC)CCCNC(C=C)C1=CC=CC=C1 RMTGISUVUCWJIT-UHFFFAOYSA-N 0.000 description 1
- PAEWTYICSQXXHB-UHFFFAOYSA-N niobium oxolead Chemical compound [Pb]=O.[Nb] PAEWTYICSQXXHB-UHFFFAOYSA-N 0.000 description 1
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- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- 239000002893 slag Substances 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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- 239000005341 toughened glass Substances 0.000 description 1
- MFWMNCMEHADIFK-UHFFFAOYSA-M tributyl(3-trimethoxysilylpropyl)azanium;bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCC[Si](OC)(OC)OC MFWMNCMEHADIFK-UHFFFAOYSA-M 0.000 description 1
- IZYSGILYXDPPNF-UHFFFAOYSA-M tributyl(3-trimethoxysilylpropyl)azanium;chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCC[Si](OC)(OC)OC IZYSGILYXDPPNF-UHFFFAOYSA-M 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- JLGNHOJUQFHYEZ-UHFFFAOYSA-N trimethoxy(3,3,3-trifluoropropyl)silane Chemical compound CO[Si](OC)(OC)CCC(F)(F)F JLGNHOJUQFHYEZ-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- FYZFRYWTMMVDLR-UHFFFAOYSA-M trimethyl(3-trimethoxysilylpropyl)azanium;chloride Chemical compound [Cl-].CO[Si](OC)(OC)CCC[N+](C)(C)C FYZFRYWTMMVDLR-UHFFFAOYSA-M 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910000663 tzm Inorganic materials 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 239000005314 uranium glass Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Images
Landscapes
- Surface Treatment Of Glass (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Paints Or Removers (AREA)
- Laminated Bodies (AREA)
- Aftertreatments Of Artificial And Natural Stones (AREA)
Description
以下に、本発明の第1実施形態の微粒子固定化無機材料及びその製造方法について詳述する。
市販の二酸化チタン粒子(石原産業株式会社製、TTO-S-1)をメタノールに10.0質量%分散してpHを3.0に塩酸で調製した後、ビーズミルにより平均粒子径15nmに粉砕分散した。得られた分散溶液にシランモノマーとして不飽和結合を有する3-メタクリロキシプロピルトリメトキシシラン(信越化学工業株式会社製、KBM-503)を微粒子に対して3.0質量%加えた後、この粉砕分散溶液を、冷却管を備えたフラスコに移してフラスコをオイルバスで加熱し、4時間還流下で処理することにより二酸化チタン微粒子表面にシランモノマーを脱水縮合反応により化学結合させて被覆を形成した。ビーズミルにより再度粉砕分散したところ、得られた分散溶液中の二酸化チタン微粒子の平均粒子径は14nmであった。なお、ここでいう平均粒子径とは、体積平均粒子径のことをいう。
基材に純アルミニウム系A1050P板の表面を奥野製薬工業株式会社製、弱アルカリ性脱脂剤トップアルクリーン161を30g/L含む、50℃に加温した水溶液に5分間浸漬した後、アルカリ洗浄剤アルクリーン水溶液で洗浄し、次いでイオン交換水で洗浄した。その後、希硝酸5質量%に30秒間浸漬してアルカリ成分を中和除去し、その後、メタノールに浸漬後、70℃の雰囲気下で10分間乾燥して清浄な自然酸化薄膜を形成した以外は実施例1と同様である。
基材にタフビッチ銅C1100P板を用い、希塩酸5質量%に30秒間浸漬した以外は実施例2と同様である。
基材に高級ステンレス鋼SUS304板を用いた以外は実施例2と同様である。
市販のジルコニア微粒子(日本電工株式会社製、PCS)をメタノールに対して10.0質量%、シランモノマーとして3−メタクリロキシプロピルトリメトキシシラン(信越化学工業株式会社製、KBM-503)を微粒子に対して5.0質量%加えてpHを4.0に塩酸で調製した後、ビーズミルにより平均粒子径16nmに粉砕分散した。その後、凍結乾燥機により固液分離して120℃で加熱してシランモノマーをジルコニア微粒子の表面に脱水縮合反応により化学結合させて被覆を形成した。
バインダー成分としてパーフルオロアルキル基とシラノール基を有するオリゴマー(信越化学工業株式会社製KP-801M)を、シランモノマーで被覆されたジルコニア微粒子の含有量に対して10質量%加える以外は実施例5と同様である。
ステンレス鋼SUS304の板を奥野製薬工業株式会社製、弱アルカリ性脱脂剤トップアルクリーン161を30g/L含む、50℃に加温した水溶液に5分間浸漬し、SUS表面の汚れを除去した。次に、60質量%の50℃に加温した濃硝酸溶液に、洗浄したSUS304板を10分間浸漬して緻密な酸化薄膜を形成した。酸化薄膜を形成したSUS304板表面にシランカップリング剤として3-メルカプトプロピルトリメトキシシラン(信越化学工業株式会社製、KBM-803)を0.5質量%加えたイソプロピルアルコールをスプレーにて塗布し、120℃、5分間乾燥してSUS304表面にシランカップリング剤を脱水縮合により結合させ、その後、実施例5で用いたバインダーを含むシランモノマー被覆ジルコニア分散液をスプレーにて塗布し、100℃、5分間乾燥後、電子線を200kVの加速電子で5Mrad照射することで、ジルコニア微粒子が固定されたSUS304板を得た。
純アルミニウム系A1050P板を、水酸化ナトリウムを3質量%含む50℃に加温した水溶液に30秒間浸漬し、水洗後、5質量%硝酸水溶液に浸漬してアルカリ成分を除去した。水洗後、15質量%の硫酸を含む20℃の水溶液に浸漬し、対極にカーボン電極を設置して、アルミニウム板を陽極として1.5A/dm2の電流密度で30分間電流を印加し、7ミクロンの厚さの多孔質酸化皮膜を形成した以外は実施例7と同様である。
洗浄したガラス板に3-メルカプトプロピルトリメトキシシラン(信越化学工業株式会社製、KBM-803)を加えたイソプロピルアルコールを塗布しないこと以外は実施例1と同様である。
洗浄した純アルミニウム系A1050P板に清浄な自然酸化薄膜を形成し、3-メルカプトプロピルトリメトキシシラン(信越化学工業株式会社製、KBM-803)を0.5質量%加えたイソプロピルアルコールを塗布しない以外は実施例2と同様である。
洗浄したSUS304板の表面に60質量%の50℃に加温した濃硝酸溶液にSUS板を浸漬して緻密な酸化薄膜を形成し、3-メルカプトプロピルトリメトキシシラン(信越化学工業株式会社製、KBM-803)を0.5質量%加えたイソプロピルアルコールを塗布しない以外は実施例7と同様である。
各種無機材料表面に固定した無機微粒子の密着性はJIS K 5400の碁盤目セロテープ(登録商標)剥離試験で試験し、剥離の状態は光学顕微鏡にて確認した。
200:微粒子固定化無機材料(第2実施形態)
300:微粒子固定化無機材料(第3実施形態)
400:微粒子固定化無機材料(第4実施形態)
500:微粒子固定化無機材料(第5実施形態)
600:微粒子固定化無機材料(第6実施形態)
100a〜600a:カップリング層
100b〜600b:無機微粒子層
300c:無機微粒子層
1:基体
2:カップリング剤
4a、4b:無機微粒子
5:シランモノマー
7:バインダー
Claims (14)
- 少なくとも表面が無機材料からなる基体と、
前記基体の表面の水酸基との縮合反応にて結合したカップリング剤を含み、前記基体の表面に形成されたカップリング層と、
シランモノマーが表面に固定された無機微粒子を含み、前記カップリング層のカップリング剤と前記無機微粒子のシランモノマーとが互いの不飽和結合又はチオール基の共有結合により結合し、前記無機微粒子同士のシランモノマーが共有結合して、前記カップリング層の表面に形成された無機微粒子層と、
を有することを特徴とする微粒子固定化無機材料。 - 前記無機微粒子の表面に固定されたシランモノマーは、不飽和結合部またはチオール基のいずれかを有することを特徴とする請求項1に記載の微粒子固定化無機材料。
- 前記カップリング層は、
前記カップリング剤が有するシラノール基が前記基体表面の水酸基との縮合反応にて結合して、前記基体の表面に形成されたことを特徴とする請求項1または2に記載の微粒子固定化無機材料。 - 前記共有結合が、グラフト重合であることを特徴とする請求項1から3のいずれかに記載の微粒子固定化無機材料。
- 前記グラフト重合が、放射線グラフト重合であることを特徴とする請求項4に記載の微粒子固定化無機材料。
- 請求項1から5に記載の微粒子固定化無機材料を用いてなることを特徴とする建装材。
- 請求項6に記載の建装材を用いてなることを特徴とするタイル。
- 請求項6に記載の建装材を用いてなることを特徴とするガラス。
- 請求項1から5に記載の微粒子固定化無機材料を用いてなることを特徴とする内装材。
- 請求項1から5に記載の微粒子固定化無機材料を用いてなることを特徴とする金属繊維構造物。
- 請求項10記載の金属繊維構造物を用いてなることを特徴とする印刷用メッシュ。
- 請求項10記載の金属繊維構造物を用いてなることを特徴とする防虫網。
- 請求項10記載の金属繊維構造物を用いてなることを特徴とするフィルター。
- 少なくとも表面が無機材料からなる基体の表面の水酸基とカップリング剤とを縮合反応にて結合して、前記基体の表面に前記カップリング剤を含むカップリング層を形成する工程と、
前記カップリング剤と無機微粒子の表面に固定されたシランモノマーとを互いの不飽和結合又はチオール基の共有結合により結合させるとともに、前記無機微粒子同士のシランモノマーを共有結合させて、前記カップリング層の表面に前記無機微粒子を含む無機微粒子層を形成する工程と、
を有することを特徴とする微粒子固定化無機材料の製造方法。
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