Pati S S, Kalyani S, Mahendran V, Philip John
J Nanosci Nanotechnol. 2014 Aug;14(8):5790-7. doi: 10.1166/jnn.2014.8842.
Magnetite nanoparticles of size ranging from 7-10 nm are prepared from aqueous solutions of Fe2+ and Fe3+ by microwave irradiation at different reaction temperatures ranging from 50 to 200 °C. The effect of reaction temperature on the structural and magnetic properties of nanoparticles is studied using X-ray diffraction (XRD), Transmission electron microscopy (TEM), Small angle X-ray scattering (SAXS), Thermo gravimetry (TGA), Differential scanning calorimetry (DSC), Vibrating sample magnetometer (VSM) and Fourier transform infrared spectroscopy (FTIR) techniques. The average size of the prepared particles, obtained from SAXS, is found to vary from 11 to 15±1 nm as the reaction temperature is increased from 50 to 200 °C. The weight gain curves under an external magnetic field show slope changes at 300 and 596 °C because of the magnetite to maghemite phase transition and ferri to paramagnetic phase transitions, respectively. The ferromagnetic γ-Fe2O3 to antiferromagnetic α-Fe2O3 phase transition temperature is found to be enhanced by 154 °C for the nanoparticles prepared at 200 °C, due to an enhanced activation energy for the cubic to a more compact hexagonal transition. The increase in the phase stability of nanoparticles prepared at elevated temperature is attributed to the diffusion of Na+ in the spinel structure. These results are useful to tailor magnetic particles with enhanced thermal stability for practical applications.
通过在50至200°C的不同反应温度下进行微波辐照,由Fe2+和Fe3+的水溶液制备尺寸范围为7-10nm的磁铁矿纳米颗粒。使用X射线衍射(XRD)、透射电子显微镜(TEM)、小角X射线散射(SAXS)、热重分析(TGA)、差示扫描量热法(DSC)、振动样品磁强计(VSM)和傅里叶变换红外光谱(FTIR)技术研究反应温度对纳米颗粒结构和磁性的影响。由SAXS得到的制备颗粒的平均尺寸随着反应温度从50°C升高到200°C而从11nm变化到15±1nm。外部磁场下的重量增加曲线分别由于磁铁矿到磁赤铁矿的相变和铁磁到顺磁的相变在300°C和596°C处显示斜率变化。对于在200°C制备的纳米颗粒,由于从立方到更致密的六方转变的活化能增加,铁磁γ-Fe2O3到反铁磁α-Fe2O3的相变温度提高了154°C。高温制备的纳米颗粒相稳定性的增加归因于Na+在尖晶石结构中的扩散。这些结果对于定制具有增强热稳定性的磁性颗粒以用于实际应用是有用的。