溶胶—凝胶法制备纳米镍锌铁氧体的研究

发布时间：2018-07-22 14:08

【摘要】：铁氧体是一种用途十分广泛的非金属磁性材料。其中具有尖晶石结构的NiZn铁氧体,作为一种多元复合金属氧化物,在磁电子学高频应用领域占有举足轻重的作用。人们对铁氧体粉体的制备方法一直进行着研究探讨,随着电子器件向小型化和轻量化方向的转变和发展,同时对材料的电磁性能提出了更高的要求,传统的生产工艺已经不能够完全满足现在发展的要求。本文将纳米技术引入Ni-Zn铁氧体的制备过程,为了研究Ni-Zn铁氧体纳米颗粒的结构和磁性能,采用溶胶-凝胶自燃法以金属硝酸盐为原料、柠檬酸为络合剂制备Ni_(1-x)Zn_xFe_2O_4纳米颗粒得到一系列样品,并利用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、透射电子显微镜(TEM)、振动样品磁强计(VSM)分别对样品的形貌、晶格结构和磁性能进行表征。XRD、TEM测试结果表明,利用溶胶凝胶自燃法制得的产物不需经过高温热处理即可得到具有单一尖晶石相的Ni_(1-x)Zn_xFe_2O_4纳米颗粒,当x=0.5的样品粒径为10-20nm;VSM对样品磁性能的测量表明,样品的饱和磁化强度M_s随Ni含量的增加呈先增大后减小的趋势,在x=0.5时有最大值,为39.378 A·m2/kg。并研究了不同pH值对产物Ni_(0.5)Zn_(0.5)Fe_20_4的物相影响,利用差示扫描量热仪对干凝胶热分解行为进行研究,通过XRD、TEM对产物的物相、微观结构的研究,结果表明产物晶粒的尺寸和分散性随pH值的变化而有较明显的变化。本文结合纳米爆炸合成法,在溶胶凝胶中添加黑索今,使混合体系进行热爆炸来制备分散效果较好的纳米Ni_(0.5)Zn_(0.5)Fe_20_4粉体。通过TEM,XRD对产物进行表征,得知此法生成的纳米Ni_(0.5)Zn_(0.5)Fe_20_4在粒径尺寸,分散效果,铁氧体相转变完全上要好于普通方法。另外添加物黑索今在进行纳米爆炸产生高能量的冲击波对纳米粉体进行松团,防止纳米粉体团聚。应用这种技术可以生产具有统一形态和平均尺寸为10nm的纳米级无团聚的Ni_(0.5)Zn_(0.5)Fe_20_4粉末。
[Abstract]:Ferrite is a widely used non-metallic magnetic material. Among them, NiZn ferrite with spinel structure plays an important role in the field of magnetoelectronics high frequency application as a kind of multicomponent composite metal oxide. The preparation methods of ferrite powders have been studied and discussed. With the development of electronic devices in the direction of miniaturization and lightweight, the electromagnetic properties of the materials are required to be higher. The traditional production process can no longer fully meet the requirements of the current development. In this paper, nano-technology was introduced into the preparation process of Ni-Zn ferrite. In order to study the structure and magnetic properties of Ni-Zn ferrite nanoparticles, the sol-gel spontaneous combustion method was used to use metal nitrate as raw material. The Ni _ (1-x) Zn-xFe _ 2O _ 4 nanoparticles were prepared with citric acid as the complex agent, and a series of samples were obtained. The morphology, lattice structure and magnetic properties of the samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). The Ni _ (1-x) ZnxFe _ 2O _ 4 nanoparticles with single spinel phase can be obtained by the sol-gel spontaneous combustion method without heat treatment at high temperature. The magnetic properties of the samples are measured when the size of x _ (0.5) is 10-20 nm VSM. With the increase of Ni content, the saturation magnetization M _ s of the samples increased first and then decreased, and reached a maximum value of 39.378 A m ~ 2 / KG at x ~ (0.5). The effect of pH value on the phase of the product Ni0.5 Zn0.5 Fe20S4 was studied. The thermal decomposition behavior of the xerogel was studied by differential scanning calorimetry (DSC). The phase and microstructure of the product were studied by XRDX TEM. The results show that the grain size and dispersity of the product vary obviously with the change of pH value. In this paper, the nano-Ni0.5 Zn0.5 Fe20S4 powder with good dispersion effect was prepared by adding RDX into the sol-gel by the method of nano-explosion synthesis, and the mixed system was prepared by thermal explosion. The product was characterized by TEM XRD, and it was found that the nano-Ni0.5 Zn0.5 Fe204 produced by this method was better than the ordinary method in particle size, dispersion effect and ferrite phase transition. In addition, the additive RDX produces high energy shock wave to loose the nano-powder and prevent the nano-powder from agglomeration. Using this technique, nano-scale agglomerated Ni _ (0.5) Zn _ (0.5) Fe _ 2O _ 4 powders with uniform morphology and average size of 10nm can be produced.
【学位授予单位】：中北大学
【学位级别】：硕士
【学位授予年份】：2011
【分类号】：TB383.1

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