Meneses-Rodríguez D, Muñoz-Sandoval E, Ramírez-Manzanares G, Ramírez-González D, Díaz-Castañon S, Faloh-Gandarilla J C, Morelos-Gómez A, López-Urías F, Terrones M
Laboratory for Nanoscience and Nanotechnology Research (LINAN) and Advanced Materials Department, IPICYT7 Camino a la Presa San José 2055, Col. Lomas 4asección, San Luis Potosí S.L.R, 78216, México.
J Nanosci Nanotechnol. 2010 Sep;10(9):5576-82. doi: 10.1166/jnn.2010.3082.
We report the production, characterization, thermal transformations (400-1000 degrees C), and magnetic properties of nanoparticles encapsulated in nitrogen-doped multiwall carbon nanotubes (CNx-MWNT), which were embedded in silicon oxide (SiOx) matrices via sol-gel techniques. The vapor chemical deposition (CVD) method with ferrocene-benzelamine mixtures was used to synthesize Fe and Fe3C nanoparticles inside CNx-MWNTs. Composites consisting of CNx-MWNTs (filler) and SiOx (matrix) were fabricated and thermally treated to different temperatures and exposure times (t). All samples were characterized using scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), thermogravimetic analysis (TGA), and magnetometry (vibrating sample). We found that upon thermal treatment, the ferromagnetic nanoparticles modify their morphology, composition and aspect ratio, thus resulting in drastic changes in the magnetic and structural properties. In particular, as produced encapsulated nanoparticles mainly consisting of Fe and Fe3C phases were thermally modified into magnetite (Fe3O4). We have also observed that the hysteresis loops are very sensitive to the thermal treatment of the sample. Thus we can control the magnetic properties of the samples using thermal treatments.
我们报告了封装在氮掺杂多壁碳纳米管(CNx-MWNT)中的纳米颗粒的制备、表征、热转变(400 - 1000摄氏度)和磁性,这些纳米颗粒通过溶胶 - 凝胶技术嵌入氧化硅(SiOx)基质中。采用二茂铁 - 苄胺混合物的气相化学沉积(CVD)方法在CNx-MWNTs内部合成Fe和Fe3C纳米颗粒。制备了由CNx-MWNTs(填料)和SiOx(基质)组成的复合材料,并在不同温度和暴露时间(t)下进行热处理。使用扫描电子显微镜(SEM)、扫描透射电子显微镜(STEM)、热重分析(TGA)和磁强计(振动样品)对所有样品进行表征。我们发现,经过热处理后,铁磁纳米颗粒的形态、成分和纵横比发生了变化,从而导致磁性和结构性能发生剧烈变化。特别是,最初制备的主要由Fe和Fe3C相组成的封装纳米颗粒经过热改性变成了磁铁矿(Fe3O4)。我们还观察到磁滞回线对样品的热处理非常敏感。因此,我们可以通过热处理来控制样品的磁性。