JP5995837B2 - 炭素及び強磁性金属又は合金を含む、ナノ粒子 - Google Patents
炭素及び強磁性金属又は合金を含む、ナノ粒子 Download PDFInfo
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- JP5995837B2 JP5995837B2 JP2013507901A JP2013507901A JP5995837B2 JP 5995837 B2 JP5995837 B2 JP 5995837B2 JP 2013507901 A JP2013507901 A JP 2013507901A JP 2013507901 A JP2013507901 A JP 2013507901A JP 5995837 B2 JP5995837 B2 JP 5995837B2
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Description
この特許出願はコバルト鉄合金粒子に限られている。FeCo粒子の飽和磁化は215emu/gであり、これはバルクのFeCoの235emu/gに近い。炭素コーティングの金属又は合金の機能化は、機能化のために極性脂質を請求する米国特許出願公開第2008/0213189号とは対照的に国際公開第99/46782には扱われていない。極性脂質は、末端に極性基を持つ脂肪族炭素鎖を持つ分子として定義されている。より具体的には、リン脂質が請求され、末端リン酸基を持つ脂肪族炭素鎖を持つ分子として定義されている。最後にアルコキシ又はチオアルキル基及びアルキルアミノ基を含む分子が請求されている。
この種類の不均一性は反応の際に十分撹拌することで防止され得る。
市販品として入手可能な、サイズが100−200μmの範囲のミクロ結晶セルロース(MCC)球状物(Cellets、neutral pellets of Syntapharm GmbH、Muelheim an der Ruhr、Germany)を、クエン酸鉄アンモニウムの水溶液内に浸漬させて負荷させた。前記球状物は、前記溶液を時々撹拌しつつ24時間、前記溶液中に放置した。次に前記含ませた球状物を液体からブフナー漏斗とガラスフィルタを用いて分離した。分離された球状物を室温で真空下で一定重量になるまで乾燥した。次に、含ませた球状物を、流動床反応装置内で不活性窒素ガス流内で熱処理により熱分解させた。加熱速度は5℃/分であり、前記サンプルを800℃で3時間維持した。これにより、約70μmのサイズを持つ強磁性性質を持つ金属炭素含有体を含むナノ粒子が得られた。還元された鉄粒子は、前記ナノ粒子の金属炭素含有体全体に均一に分散されていた。図3で示される、このサンプルの透過電子顕微鏡画像から分かるように、金属性鉄粒子を含むナノ粒子は部分的にグラファイト囲い内に包埋されており、サイズは10−100nmの範囲である。ここで説明されたサンプル内の鉄の量は、ICP−MSで測定され、8.28重量%であった。続いて濃塩酸で処理することで、水素発生が観測された。これは全ての鉄が完全に包埋されていないことを示した。発生した水素の量から、溶解された鉄の量は、最初の鉄の量の約20%として計算された。
市販品として入手可能な、サイズが100−200μmの範囲のミクロ結晶セルロース(MCC)球状物(Cellets、neutral pellets of Syntapharm GmbH、Muelheim an der Ruhr、Germany)を、クエン酸鉄アンモニウムの水溶液内に浸漬させて負荷させた。前記球状物は、前記溶液を時々撹拌しつつ24時間、前記溶液中に残された。次に前記含ませた球状物を液体からブフナー漏斗とガラスフィルタを用いて分離した。分離された球状物を室温で真空下で一定重量になるまで乾燥した。次に、含ませた球状物を、流動床反応装置内で不活性窒素ガス流内で熱処理により熱分解させた。加熱速度は5℃/分であり、前記サンプルを800℃で3時間維持した。続いて、水素−窒素(50/50)のガス流内でトルエンで処理することで、約70μmのサイズを持つ強磁性性質を持つ金属炭素含有体を含むナノ粒子が得られた。還元された鉄粒子は、前記ナノ粒子の金属炭素含有体全体に均一に分散されていた。続いて濃塩酸で処理することで、水素ガス発生は観測されなかった。これは全ての鉄粒子がナノ粒子内で完全に包埋されていることを示した。図4は、前記原サンプルを粉砕して得られた包埋鉄粒子の透過電子顕微鏡画像を示す。
市販品として入手可能な、サイズが100−200μmの範囲のミクロ結晶セルロース(MCC)球状物(Cellets、neutral pellets of Syntapharm GmbH、Muelheim an der Ruhr、Germany)を、クエン酸鉄アンモニウムの水溶液内に浸漬させて負荷させた。前記球状物は、前記溶液を時々撹拌しつつ24時間、前記溶液中に放置した。次に前記含ませた球状物を液体からブフナー漏斗とガラスフィルタを用いて分離した。分離された球状物を室温で真空下で一定重量になるまで乾燥した。次に、含ませた球状物を、チューブ加熱炉内で一定の不活性窒素ガス流内で熱処理により熱分解させた。加熱速度は5℃/分であり、前記サンプルを800℃で3時間維持した。これにより、約70μmのサイズを持つ強磁性性質を持つ金属炭素含有体を含むナノ粒子が得られた。非常に多くの非常に小さい金属性鉄粒子の生成の他、いくらかの大きな鉄粒子がナノ粒子の炭素体の外部端部に形成される(図5参照。後方散乱電子顕微鏡画像は、重原子である鉄を相対的に高強度で示す)。
グラファイト包埋された鉄粒子を含むナノ粒子を、N、N、N−トリメチル−2−オキソ−2−(ピレン−1−イル)エタンアンモニウムブロミド(以下の式(I))の水溶液内に、N.Nakashima、Y.Tomonari及びH.Murakamiの「Water−Soluble Single−Walled Carbon Nanotubes via Noncovalent Sidewall−Functionalization」(Chem.Lett.31、P.638−639、2002)により合成したピレン担持アンモニウムイオンと共に入れた。このプローブは、カーボンナノチューブのグラファイト表面と強い相互作用を持つことが知られている。ピレン担持アンモニウムイオンは前記ナノ粒子のグラファイト表面に非可逆的に吸着された。溶液から前記ピレン担持アンモニウムイオンの消費はUV−VISスペクトルにより追跡された。超音波処理の後、グラファイト包埋鉄粒子を含むナノ粒子の安定で均一な分散物が得られた。
グラファイト包埋鉄粒子を含むナノ粒子を、N−2−(2−(2−メトキシエトキシ)エトキシ)エチル)ピレン−1−カルボキサミド(以下の式(II))の水溶液中に入れた。前記ピレン担持オリゴ−エチレン−グリコール尾部は前記グラファイト表面に非可逆的に吸着された。溶液から前記ピレン担持アンモニウムイオンの消費はUV−VISスペクトルにより追跡された。超音波処理の後、グラファイト包埋鉄粒子を含むナノ粒子の安定で均一な分散物が得られた。
グラファイト包埋鉄粒子を含むナノ粒子を、N−2−(2−(2−メトキシエトキシ)エトキシ)エチル)−N、N−ジメチル−2−オキソ−2−(ピレン−1−イル)エタンアンモニウムブロミド(以下の式(III).の水溶液中に入れた。親水性及び静電基の両方を持つピレンは、グラファイト表面に非可逆的に吸着された。溶液から前記ピレン担持アンモニウムイオンの消費はUV−VISスペクトルにより追跡された。超音波処理の後、グラファイト包埋鉄粒子を含むナノ粒子の安定で均一な分散物が得られた。
Claims (15)
- 少なくとも1つの強磁性金属の金属粒子3−100個、及びグラファイトカーボン体を含む、最大直径500μm未満の粒子であり、前記金属粒子が前記グラファイトカーボン体で少なくとも部分的に包埋される、粒子。
- 請求項1に記載の粒子であり、前記強磁性金属が鉄を含む、粒子。
- 請求項2に記載の粒子であり、少なくとも1つの強磁性金属の金属粒子がさらに、ニッケル、コバルト、貴金属及びそれらの組み合わせからなる群から選択される金属を含む、粒子。
- 請求項1乃至3のいずれか一項に記載の粒子であり、前記少なくとも1つの強磁性金属の金属粒子がグラファイトカーボン体で少なくとも部分的にコーティングされ、及び金層で少なくとも部分的にコーティングされる、粒子。
- 請求項1乃至3のいずれか一項に記載の粒子であり、前記少なくとも1つの強磁性金属の金属粒子がグラファイトカーボン体で完全に包埋される、粒子。
- 請求項1乃至5のいずれか一項に記載の粒子であり、前記粒子がさらに、置換多環芳香族化合物を含み、前記置換多環芳香族化合物は前記グラファイトカーボン体の表面へ吸着される、粒子。
- 金属炭素体としての請求項1に記載の粒子を製造するためのプロセスであって、当該プロセスが、炭素含有体に鉄前駆体及び少なくとも1つのその他の金属前駆体の水溶性溶液を含ませ、前記含ませた炭素含有体を乾燥させ、続いて前記含ませた炭素含有体を不活性及び実質的に無酸素の雰囲気下で、450から600℃の温度で加熱し、それにより金属化合物を対応する金属合金へ還元することを含む、プロセス。
- 金属炭素体としての請求項1に記載の粒子を製造するためのプロセスであって、当該プロセスが、炭素含有体に強磁性金属前駆体の水溶性溶液を含ませ、前記含ませた炭素含有体を乾燥させ、続いて前記含ませた炭素含有体を不活性及び実質的に無酸素の雰囲気下で、700℃を超える温度に加熱し、それにより金属化合物を対応する金属へ還元する
ことを含む、プロセス。 - 請求項8に記載のプロセスであり、前記強磁性金属が鉄である、プロセス。
- 請求項7乃至9のいずれか一項に記載のプロセスであり、前記金属前駆体は、クエン酸、酢酸、ギ酸、ヒドロキシル酸及びクエン酸アンモニウムからなる群から選択される1又はそれ以上の有機酸の1つ又はそれ以上の塩である、プロセス。
- 請求項7乃至10のいずれか一項に記載のプロセスであり、前記炭素含有体が、ミクロ結晶性セルロース、コロイド性カーボン、活性炭素体及びそれらの混合物からなる群から選択される、プロセス。
- 請求項7に記載のプロセスであり、前記金属合金がさらに、ニッケル、コバルト、貴金属及びこれらの混合物からなる群から選択される他の金属を含む、プロセス。
- 請求項7乃至12のいずれか一項に記載のプロセスであり、前記粒子はアモルファスカーボンをさらに含み、前記粒子は酸化剤で処理され、前記アモルファスカーボンを除去し、かつグラファイト表面にカルボキシル酸基を生成する、プロセス。
- 請求項7乃至13のいずれか一項に記載のプロセスであり、前記粒子が水素及び炭素含有分子を含む流れ中で処理され、前記粒子がグラファイトカーボン体で完全に包埋される、プロセス。
- 請求項7乃至13のいずれか一項に記載のプロセスであり、前記粒子が、金化合物を含む水溶性溶液に浸漬され、前記粒子が部分的に金層でコーティングされる、プロセス。
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