Morjan I, Alexandrescu R, Dumitrache F, Birjega R, Fleaca C, Soare I, Luculescu C R, Filoti G, Kuncer V, Vekas L, Popa N C, Prodan G, Ciupina V
National Institute for Lasers, Plasma and Radiation Physics Bucharest, POB MG-36, 077125 Romania.
J Nanosci Nanotechnol. 2010 Feb;10(2):1223-34. doi: 10.1166/jnn.2010.1863.
Nano-sized iron oxide-based particles have been directly synthesized by the laser induced pyrolysis of a mixture containing iron pentacarbonyl/air (as oxidizer)/ethylene (as sensitizer). In this paper we further demonstrate the possibility to vary the chemical composition and the nanoparticle dimensions of the iron oxide-based materials by handling the oxidation procedure in the frame of the laser pyrolysis process. Thus, nanoparticles with major maghemite/magnetite content may change composition into mixtures with variable amounts of three components: major gamma-Fe2O3/Fe3O4 iron oxide, metallic Fe and cementite Fe3C. By X-ray diffraction (XRD) it is found that the relative proportion of these phases differs in function of the reaction temperature (laser power). As revealed by transmission electron microscopy (TEM), mean particle sizes between about 4 nm and 6 nm and between about 9 and 11 nm may be prepared by varying the oxidation procedure and the laser power, respectively. By the controlled heating of samples (maximum temperature 185 degrees C), increased crystallinity for the gamma-Fe2O3/Fe3O4 oxide phase was found as well as an increase of the mean particle diameters. The examination of the magnetization curves for samples obtained for different laser powers indicates notable differences in the magnetic behavior and parameters. The temperature dependent Mossbauer measurements confirm the formation of larger particles at higher laser power densities as well as the presence of inter-particle magnetic interactions. On this basis, the estimation of phase composition for the different representative samples is given.
通过激光诱导热解包含五羰基铁/空气(作为氧化剂)/乙烯(作为敏化剂)的混合物,直接合成了纳米尺寸的氧化铁基颗粒。在本文中,我们进一步证明了在激光热解过程框架内通过控制氧化过程来改变氧化铁基材料的化学成分和纳米颗粒尺寸的可能性。因此,主要含有磁赤铁矿/磁铁矿的纳米颗粒可能会转变为包含三种成分且含量可变的混合物:主要为γ-Fe₂O₃/Fe₃O₄氧化铁、金属铁和渗碳体Fe₃C。通过X射线衍射(XRD)发现,这些相的相对比例随反应温度(激光功率)而变化。如透射电子显微镜(TEM)所揭示的,分别通过改变氧化过程和激光功率,可以制备出平均粒径在约4纳米至6纳米之间和约9至11纳米之间的颗粒。通过对样品进行可控加热(最高温度185摄氏度),发现γ-Fe₂O₃/Fe₃O₄氧化物相的结晶度增加,平均粒径也增大。对不同激光功率下获得的样品的磁化曲线进行检查,结果表明其磁行为和参数存在显著差异。与温度相关的穆斯堡尔测量结果证实,在较高激光功率密度下会形成更大的颗粒,并且存在颗粒间的磁相互作用。在此基础上,给出了不同代表性样品的相组成估算。