纳米锰锌铁氧体粉体的沸腾回流法制备及性能研究
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摘要
纳米磁性材料是当今磁性材料研究的热点,软磁材料中品种最多、用量最大、应用最广泛的是软磁铁氧体材料。纳米锰锌铁氧体材料作为一种重要的软磁材料具有广阔的应用前景。本文对纳米软磁锰锌铁氧体粉体的制备方法及性能进行了研究。
     本文采用沸腾回流法,以δ-FeOOH为前驱体,直接合成了尖晶石结构的MnZn铁氧体纳米粉体。研究了共沉淀pH值、反应时间等工艺因素对产物的影响,得出了合适的共沉淀沸腾回流法制备工艺;采用XRD、TEM、VSM等测试手段对产品进行了表征,对回流相转化反应动力学、热力学、反应机理、磁性能等进行了分析研究。研究表明,通过调节pH值和回流时间可以得到从小于10nm到大于20nm不同粒径的锰锌铁氧体粉体,获得完全产物的最佳回流时间为6h。pH值对反应剧烈程度及磁性能有很大影响,共沉淀pH值为13.0左右时获得的制备态纳米粉末尺寸约为20nm,饱和磁化强度达46A.m2/kg。
     为了抑制纳米粉体的团聚,将物理分散与化学分散结合起来,利用物理手段解团聚,然后加入分散剂实现颗粒的稳定化,可以达到较好的分散效果,得到了具有良好分散性的锰锌铁氧体纳米粉体。
     本文还研究了稀土元素(La、Nd、Gd)取代对尖晶石铁氧体结构和磁性能的影响。当稀土离子取代尖晶石铁氧体晶格中的Fe3+时,稀土离子可能会进入尖晶石晶格,也可能形成化合物进入晶界。经研究发现由于稀土离子(La3+、Nd3+、Gd3+)的有效磁距与离子半径的差异,稀土离子的掺入会减少尖晶石铁氧体的晶格常数和晶粒尺寸,而其矫顽力Hc得以提高,饱和磁化强度变化与稀土离子的添加量有关。
Magnetic nanomaterial is currently the hot topic of the current research. The soft magnetic ferrite is one of the most important soft magnetic materials with a wide range of applications. In this dissertation, the preparation and properties of soft magnetic MnZn ferrites were discussed.
     The spinel-type Mn-Zn ferrite nano-powders were sythesized by co-precipitation and refluxing method usingδ-FeOOH as a precursor. The structure and properties of the prepared samples were characterized by XRD, SEM, VSM. The influences of processing parameters such as the pH value of co-precipitation, reaction temperature and reaction time were systematically investigated. The reaction kinetics, thermodynamics, reaction mechanics, magnetic property, thermostability is also studied. The results showed that the optimum refluxing time for complete reaction is 6h. The size of MnZn ferrites nano-powders varied between<10nm and>20nm. It was also found that the mean size of the nano-powders can be controlled by pH value of the co-precipitation solution. As-prepared powders with mean particle size of 20nm and saturation magnetization of 46A·m2/kg were obtained when the pH value is 13.
     To obtain well-dispersed physical and chemical methods can be used. In this work, physical dispertion was used to decompose the glomeration, and doping agent to obtain stabilization particle. The ultra fine nanoparticles on that aggregation were prepared successfully finally.
     The effects of Rare-earth (La, Nd, Gd) doping on the structure and magnetic properties of MnZn ferrite nanopowders are discussed in the dissertation. RE ion may either replace Fe3+ and entered into spinel crystal lattice or aggregate on the grain boundary in the form of compound. Due to the difference in available magnetic moment and ion's radius for La3+ Nd3+and Gd3+, the crystal lattice and grain size decreased and the coercive force increased with RE ion doping.
引文
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