Fe-Ni合金/Ni铁氧体复合纳米纤维的制备、表征与磁性能研究

doi:10.6023/A12080587

摘要/Abstract

采用静电纺丝结合氢气热还原法制备了一系列平均直径约为60～70 nm的Fe-Ni合金/Ni铁氧体复合纳米纤维. 使用热重-差热分析、X射线衍射、扫描电镜、透射电镜、选区电子衍射和振动样品磁强计等技术对前驱体纤维的热分解行为以及目标产物的晶体结构、相组成、形貌和磁性能进行了表征. 结果显示, Ni铁氧体纳米纤维的制备温度及其还原温度对相应还原产物的相组成和磁性能有着显著的影响; 所得Fe-Ni合金/Ni铁氧体复合纳米纤维由于Fe-Ni合金的引入表现出更为优良的磁性能, 且各磁性相间存在良好的交换耦合, 其整体磁行为如同一个单相磁性材料. 在复合纳米纤维磁性能上所观察的变化可根据Fe-Ni合金和Ni铁氧体内禀磁特性的不同以及晶粒尺寸、相组成和磁相互作用的变化来进行解释.

关键词: Ni铁氧体, Fe-Ni合金, 复合纳米纤维, 磁性能, 静电纺丝, 氢气热还原

A series of Fe-Ni alloy/Ni-ferrite composite nanofibers with average diameters of 60～70 nm were successfully fabricated using electrospinning combined with the hydrogen-thermal reduction method. The thermal decomposition behavior of electrospun precursor nanofibers and crystal structures, phase compositions, morphologies and magnetic properties of the resultant products were characterized by means of thermogravimetric and differential thermal analysis, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, selected area electron diffraction, and vibrating sample magnetometer. It is found that both the preparation temperature of the pristine Ni-ferrite nanofibers and the reduction temperature have considerable influences on the phase compositions and magnetic properties of the corresponding reduction products. With increasing reduction temperature from 270 to 400 ℃ for the Ni-ferrite nanofibers prepared at 550 ℃, the content of Fe-Ni alloy in the reduction products increases gradually, the saturation magnetizations, remanences and coercivities increase initially, respectively reaching a maximum value of 203.0 emu·g^-1, 54.9 emu·g^-1 and 42.7 kA·m^-1 for the composite obtained after reduction at 320 ℃, with a mass fraction of about 82% for Fe-Ni alloy, and then decrease with a further increase in reduction temperature. As the preparation temperature of the pristine Ni-ferrite nanofibers decreases from 700 to 400 ℃, the saturation magnetizations of the corresponding products obtained at the same reduction condition (i.e., reduction at 300 ℃ for 1 h) increase gradually, while their remanences and coercivities show a trend of first increase and then decrease, and the reduction product of Ni-ferrite nanofibers synthesized at 500 ℃ has a maximum remanence and coercivity of 62.2 emu·g^-1 and 47.8 kA·m^-1, respectively. Compared to the pristine Ni-ferrite nanofibers, the prepared Fe-Ni alloy/Ni-ferrite composite nanofibers exhibit more excellent soft magnetic properties with much enhanced saturation magnetization due to introduction of Fe-Ni alloy phase. Furthermore, the composite nanofibers composed of three magnetic phases in crystallography show a good single-phase magnetic behavior, implying that these magnetic phases in composites are well exchange- coupled with each other. The observed changes in magnetic properties for the prepared composite nanofibers can be explained on the basis of the differences in intrinsic magnetic properties between Fe-Ni alloy and Ni-ferrite phases and the changes in grain size, phase composition and magnetic interactions. These novel magnetic composite nanofibers have potential application prospects in flexible magnets, sensing devices, catalysis, microwave absorption and electromagnetic interference (EMI) shielding.

Key words: Ni-ferrite, Fe-Ni alloy, composite nanofibers, magnetic properties, electrospinning, hydrogen-thermal reduction

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向军, 张雄辉, 褚艳秋, 沈湘黔. Fe-Ni合金/Ni铁氧体复合纳米纤维的制备、表征与磁性能研究[J]. 化学学报, 2012, 70(21): 2265-2272.

Xiang Jun, Zhang Xionghui, Chu Yanqiu, Shen Xiangqian. Preparation, Characterization and Magnetic Properties of Fe-Ni Alloy/Ni-Ferrite Composite Nanofibers[J]. Acta Chimica Sinica, 2012, 70(21): 2265-2272.

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