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采用溶剂热还原法,以FeCl3.6H2O和乙二醇为原料,在200℃相对低温条件下成功合成四氧化三铁微米球。通过改变实验条件,可在115～435nm有效调控Fe3O4亚微米球的粒径。采用X射线衍射仪(XRD)、透射电子显微镜(TEM)和扫描电子显微镜(SEM)对样品的结构、粒径、形貌和组成进行了分析,并于室温测试了它的磁学性能。结果表明,产物Fe3O4亚微米球为反尖晶石结构,330nmFe3O4亚微米球的矫顽力(Hc)为6644.93A/m,饱和磁化强度(Ms)为81.2emu/g,剩余磁化强度(Mr)为14.6emu/g。研究了乙二醇和NaOH的浓度、反应时间对产物形貌的影响,结果表明,乙二醇在Fe3O4亚微米球的形成过程中起着关键作用,并提出了可能的生长机理。
Using solvothermal reduction method, FeCl3.6H2O and ethylene glycol as raw materials, the relatively low temperature of 200 ℃ under the conditions of the successful synthesis of Fe3O4 microspheres. By changing the experimental conditions, the size of Fe3O4 submicron spheres can be effectively controlled at 115 ~ 435nm. The structure, particle size, morphology and composition of the samples were analyzed by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The magnetic properties of the samples were tested at room temperature. The results show that the Fe3O4 submicron spheres have a negative spinel structure, the coercivity (Hc) of the 330nm Fe3O4 submicron spheres is 6644.93A / m, the saturation magnetization (Ms) is 81.2emu / g, the residual magnetization (Mr) 14.6emu / g. The effects of the concentration of ethylene glycol and NaOH and the reaction time on the morphology of the product were studied. The results showed that ethylene glycol played a key role in the formation of Fe3O4 submicron sphere and proposed the possible growth mechanism.