微波辅助制备Fe_3O_4纳米材料及表征

Preparation and Characterization for Nanometer Material Fe_3O_4 with the Assistance of Microwave Technology

考察了在微波辅助技术的前提下3 2Fe/Fe++摩尔比、氨水用量和微波功率变量因素对制备3 4Fe O纳米材料的影响,并筛选出较优的制备条件。同时,对该样品进行X-射线衍射(XRD)和高分辨率透射电镜(TEM)扫描分析。其结果表明:(1)3 2Fe/Fe++摩尔比1:1、氨水用量15mL、油酸钠1.00g、微波辐射功率200W和反应30min为制备3 4Fe O纳米材料的最优条件;(2)根据Scherer公式计算,该样品的平均粒径为10nm^20nm,且样品微粒形状规则,近似球形,晶体形状较好,粒径大小较为均一;(3)通过对比研究制备3 4Fe O纳米微粒的微波辅助合成法、共沉淀法和沉淀氧化法,从XRD谱图分析可知,用微波辅助合成法制得的3 4Fe O纳米微粒的特征衍射峰明显,分散性好,且强度较高,说明该法所制得的3 4Fe O微粒晶化度较高。

At the premise of assistant microwave technology, we studied the influence of preparation for nanometer material Fe3O4 through observing some variables, such as Fe3＋/Fe2＋in molar ratio, NH3＆#183;H2O in quantity and microwave in frequency. By optimization on preparation for Fe3O4 particles, the sample of Fe3O4 particles was successfully accessed and diagnosed by X-ray diffraction （XRD） and high resolution transmission electron microscopes （TEM）. The findings demonstrated that（1）these variables, which are 1/1 Fe3＋/Fe2＋in molar ratio, 15ml NH3＆#183;H2O and 200W microwave in frequency, are the best optimum condition in preparation of Fe3O4 particles with proceeding for 30min in the presence of 1.00g sodium oleate as defrother. （2） by analyzing XRD and TEM spectrograms and Scherrer formula, the feature peaks of Fe3O4 particles are remarkable in XRD spectrogram, whose shape is near to regular ball and whose length is generally homogeneous with 10-20nm on average. （3） In comparison of co-deposition and deposition-oxidation approaches with microwave assistance, the purity of Fe3O4 particles, prepared by the assistance of microwave technology, are much higher than other methods by analyzing XRD spectrograms.