溶胶—凝胶法制备镍铜锌铁氧体的掺杂与磁性能研究
摘要
软磁铁氧体材料是一种应用十分广泛的功能材料,最常见的是镍锌铁氧体和锰锌铁氧体。铁氧体材料具有高磁导率、高电阻率、低损耗等优点,主要在自动控制、计算技术、仪器仪表和通讯广播等电子工业部门中应用,而且在宇宙航行、信息显示、卫星通讯和污染处理等行业也有一定的应用。锰锌铁氧体主要用在高频领域,镍锌铁氧体主要用在低频领域,锰锌铁氧体比镍锌铁氧体电阻率低5-6个数量级并且需要更高的烧结温度,镍锌铁氧体更节省能源,所以本文是通过不同的掺杂来制备NiCuZn铁氧体。铁氧体的制备方法有很多种,溶胶凝胶自蔓延法就是其中一种生产工艺简单、过程易于控制、产品纯度高的制备方法。本文是在前人研究的基础上,采用溶胶凝胶自蔓延法制备出不同掺杂的NiCuZn铁氧体,并应用X射线衍射仪,振动样品磁强计和穆斯堡尔谱仪对这些样品进行了微观结构及磁特性的研究。
本论文的主要成果如下：
1.对当前NiCuZn铁氧体的稀土掺杂和复合掺杂现状进行了研究。
2.采用溶胶凝胶自蔓延法制备出Ni0.6Cu0.2Zn0.2CexFe2-xO4铁氧体,结合样品的XRD图、M-H图和穆斯堡尔谱图,分析研究了稀土铈掺杂对NiCuZn铁氧体微观结构和磁性能的影响。通过XRD分析可知该样品为典型的尖晶石结构,粉末晶粒尺寸在30nm左右。通过样品在T=300K时的磁滞回线表明,此铁氧体为典型的亚铁磁性,并且矫顽力(Hc)随着掺杂离子的增加而增加,饱和磁化强度(Ms)随着掺杂离子的增加而先增大后减小。通过Mossbauer谱分析可知,随着Ce3+掺杂量的增加,A位吸收面积和超精细场相对减小,B位吸收面积相对增加,超精细场变化不大。
3.采用溶胶凝胶自蔓延法制备出Ni0.6-xCu0.2Zn0.2CoxBiyFe2_yO4铁氧体,结合样品的XRD图、M-H图和穆斯堡尔谱图,分析研究了Co、Bi复合掺杂对NiCuZn铁氧体的微观结构和磁性能的影响。通过XRD分析表明,随着Bi离子掺杂量的增加,样品晶粒密度逐渐增大。样品在T=300K时的磁滞回线表明,此铁氧体为典型的亚铁磁性,并且矫顽力(Hc)随着掺杂离子的增加而增加,饱和磁化强度(Ms)随着掺杂离子的增加而先增大后减小。通过Mossbauer谱分析可知,随着掺杂量的增加,A位吸收面积相对减小,B位吸收面积相对增加。
最后,我们总结了本文的研究工作,并展望了NiCuZn铁氧体潜在的研究方向。
The soft magnetic ferrite material is a very wide range of functional material, the most common is NiZn ferrite and MnZn ferrite. The ferrite material has the advantages of high permeability, high resistivity and low loss, not only the gradual strengthening of applications in automatic control, computing technology, instrumentation and communication broadcasting of the electronics industry sector, and in astronauts, information display, satellite communications, and pollution treatment and other industries also have broad prospects. The MnZn ferrite is mainly used in high frequency field and the NiZn ferrite is mainly used in the low frequency field, MnZn ferrite resistivity lower5-6order of magnitude than the NiZn ferrite and need higher sintering temperature. In this paper, we use the different doping preparation of NiCuZn ferrite. There are many preparation methods to prepare ferrite, the Sol-Gel SHS is a production process simple, easy control of the process, high purity preparation ferrite method. This article is based on previous research, using the Sol-Gel SHS prepared different doping ratio NiCuZn ferrite, applies X-ray diffractiometer, vibrating sample magnetometer and Mossbauer spectrometer to research microstructure and magnetic properties of the sample.
The main results of this paper are given as follows:
1. We research rare earth doped and composite doped NiCuZn ferrite's present situation.
2. The Sol-Gel SHS were prepared Ni0.6Cu0.2Zn0.2CexFe2-xO.4ferrite, combined with the sample's XRD figure, M-H figure and Mossbauer spectra, and analysis the rare earth cerium doped influence to the microstructure and magnetic properties of the NiCuZn ferrite. We analysis the sample on the XRD can know it is typical spinel structure, the powder grain size is about30nm. The hysteresis loop at T=300K of the samples showed that, this ferrite is typical ferrimagnetic, and coercive force (He) increase with increase of the doped ion. and the saturation magnetization (Mv) first increase and then decrease with increase of the doped ion. We can know through carries on the Mossbauer spectrum measurement, with Ce3+doping content increases, A absorption area and hyperfine field relative reduction, but B absorption area increases and hyperfine field have little change.
3. The Sol-Gel SHS were prepared Ni06-xCu0.2Zn0.2CoxBiyFe2-yO4ferrite, combined with the sample's XRD figure, M-H figure and Mossbauer spectra, and analysis the composite doped influence to the microstructure and magnetic properties of the NiCuZn ferrite. The XRD analysis showed that, with doping amount increase of the Bi ion, sample grain density increases. The hysteresis loop at T=300K of the samples showed that, this ferrite is typical ferrimagnetic, and coercive force (He) increase with increase of the doped ion, and the saturation magnetization (Ms) first increase and then decrease with increase of the doped ion. Through its Mossbauer spectrum analysis, the absorption area of A site is relatively reduced and the absorption area of B site is relative increase with compound doped increase.
本论文的主要成果如下：
1.对当前NiCuZn铁氧体的稀土掺杂和复合掺杂现状进行了研究。
2.采用溶胶凝胶自蔓延法制备出Ni0.6Cu0.2Zn0.2CexFe2-xO4铁氧体,结合样品的XRD图、M-H图和穆斯堡尔谱图,分析研究了稀土铈掺杂对NiCuZn铁氧体微观结构和磁性能的影响。通过XRD分析可知该样品为典型的尖晶石结构,粉末晶粒尺寸在30nm左右。通过样品在T=300K时的磁滞回线表明,此铁氧体为典型的亚铁磁性,并且矫顽力(Hc)随着掺杂离子的增加而增加,饱和磁化强度(Ms)随着掺杂离子的增加而先增大后减小。通过Mossbauer谱分析可知,随着Ce3+掺杂量的增加,A位吸收面积和超精细场相对减小,B位吸收面积相对增加,超精细场变化不大。
3.采用溶胶凝胶自蔓延法制备出Ni0.6-xCu0.2Zn0.2CoxBiyFe2_yO4铁氧体,结合样品的XRD图、M-H图和穆斯堡尔谱图,分析研究了Co、Bi复合掺杂对NiCuZn铁氧体的微观结构和磁性能的影响。通过XRD分析表明,随着Bi离子掺杂量的增加,样品晶粒密度逐渐增大。样品在T=300K时的磁滞回线表明,此铁氧体为典型的亚铁磁性,并且矫顽力(Hc)随着掺杂离子的增加而增加,饱和磁化强度(Ms)随着掺杂离子的增加而先增大后减小。通过Mossbauer谱分析可知,随着掺杂量的增加,A位吸收面积相对减小,B位吸收面积相对增加。
最后,我们总结了本文的研究工作,并展望了NiCuZn铁氧体潜在的研究方向。
The soft magnetic ferrite material is a very wide range of functional material, the most common is NiZn ferrite and MnZn ferrite. The ferrite material has the advantages of high permeability, high resistivity and low loss, not only the gradual strengthening of applications in automatic control, computing technology, instrumentation and communication broadcasting of the electronics industry sector, and in astronauts, information display, satellite communications, and pollution treatment and other industries also have broad prospects. The MnZn ferrite is mainly used in high frequency field and the NiZn ferrite is mainly used in the low frequency field, MnZn ferrite resistivity lower5-6order of magnitude than the NiZn ferrite and need higher sintering temperature. In this paper, we use the different doping preparation of NiCuZn ferrite. There are many preparation methods to prepare ferrite, the Sol-Gel SHS is a production process simple, easy control of the process, high purity preparation ferrite method. This article is based on previous research, using the Sol-Gel SHS prepared different doping ratio NiCuZn ferrite, applies X-ray diffractiometer, vibrating sample magnetometer and Mossbauer spectrometer to research microstructure and magnetic properties of the sample.
The main results of this paper are given as follows:
1. We research rare earth doped and composite doped NiCuZn ferrite's present situation.
2. The Sol-Gel SHS were prepared Ni0.6Cu0.2Zn0.2CexFe2-xO.4ferrite, combined with the sample's XRD figure, M-H figure and Mossbauer spectra, and analysis the rare earth cerium doped influence to the microstructure and magnetic properties of the NiCuZn ferrite. We analysis the sample on the XRD can know it is typical spinel structure, the powder grain size is about30nm. The hysteresis loop at T=300K of the samples showed that, this ferrite is typical ferrimagnetic, and coercive force (He) increase with increase of the doped ion. and the saturation magnetization (Mv) first increase and then decrease with increase of the doped ion. We can know through carries on the Mossbauer spectrum measurement, with Ce3+doping content increases, A absorption area and hyperfine field relative reduction, but B absorption area increases and hyperfine field have little change.
3. The Sol-Gel SHS were prepared Ni06-xCu0.2Zn0.2CoxBiyFe2-yO4ferrite, combined with the sample's XRD figure, M-H figure and Mossbauer spectra, and analysis the composite doped influence to the microstructure and magnetic properties of the NiCuZn ferrite. The XRD analysis showed that, with doping amount increase of the Bi ion, sample grain density increases. The hysteresis loop at T=300K of the samples showed that, this ferrite is typical ferrimagnetic, and coercive force (He) increase with increase of the doped ion, and the saturation magnetization (Ms) first increase and then decrease with increase of the doped ion. Through its Mossbauer spectrum analysis, the absorption area of A site is relatively reduced and the absorption area of B site is relative increase with compound doped increase.
引文
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