类鱼骨结构CoFe2O4纳米纤维的制备与性能

doi:10.15541/jim20190581

摘要/Abstract

摘要：

采用静电纺丝与高温煅烧相结合的方法, 以聚乙烯吡咯烷酮(PVP)、九水合硝酸铁(Fe(NO₃)₃·9H₂O)和六水合硝酸钴(Co(NO₃)₂·6H₂O)为原料, 制备出了类鱼骨结构的CoFe₂O₄纳米纤维, 并研究了煅烧温度对CoFe₂O₄纳米纤维形貌、磁性能以及微波吸收性能的影响。结果表明: 随着煅烧温度的升高, CoFe₂O₄纤维的结晶度和晶粒尺寸逐渐增大, 纳米纤维的表面形貌由光滑发展为粗糙多孔, 煅烧温度超过800 ℃时, 纳米纤维呈现类鱼骨结构; 随着煅烧温度增加纤维直径逐渐减小, 900 ℃煅烧的纤维平均直径为80.3 nm。所制备的纳米纤维经振动样品磁强计(VSM)测试结果表明, 饱和磁化强度(M_s)随着煅烧温度的升高而增加, 在900 ℃煅烧条件下纤维的M_s达87.13 A·m²/kg。矢量网络分析仪测试结果表明, 不同煅烧温度下纤维的微波吸收性能差异明显, 800 ℃下煅烧的纤维具有最佳的吸波性能。CoFe₂O₄纳米纤维通过磁滞损耗和涡流损耗机制吸收电磁波, 煅烧产生的孔洞和类鱼骨形貌有利于电磁波在孔道表面多次反射从而增加反射损耗。

关键词: 静电纺丝, CoFe₂O₄, 纳米纤维, 磁性能, 微波吸收

Abstract:

CoFe₂O₄ nanofibers with fishbone-like structure were prepared by a electrospinning method followed with high temperature calcination, using polyvinylpyrrolidone (PVP), iron nitrate nonahydrate (Fe(NO₃)₃·9H₂O) and cobalt nitrate hexahydrate (Co(NO₃)₂·6H₂O) as raw materials. Results show that the crystallinity and grain size of nanofibers become larger with increasing calcination temperature. Meanwhile, the surface morphology of CoFe₂O₄ nanofibers changes from smooth to rough and porous. The morphology of CoFe₂O₄ nanofibers exhibits a fishbone-like structure with calcination temperature exceeding 800 ℃. The diameter of the fiber is gradually decreased with the increase of calcination temperature, and the average diameter of CoFe₂O₄ nanofibers calcined at 900 ℃ reaches 80.3 nm. By vibration sample magnetometer (VSM) test, the saturation magnetization (M_s) of CoFe₂O₄ nanofibers increases with the increase of calcination temperature, and the M_s of CoFe₂O₄ nanofibers calcined at 900 ℃ is 87.13 A·m²/kg. In a result of vector network analyzer (VNA) analysis, the microwave absorption performance is significantly different with calcination temperature changing. Among them the fibers calcined at 800 ℃ have the highest wave absorption ability. The microwave absorption mechanism of CoFe₂O₄ nanofibers mainly includes hysteresis loss and eddy current loss. The morphology of porous and fishbone-like generated by calcination can increase the reflection loss, for the reason that this morphology is beneficial for microwave reflection multiple times on the fiber surface.

Key words: electrospinning, CoFe₂O₄, nanofibers, magnetic performance, microwave absorption

中图分类号:

TQ343

朱正旺,冯锐,柳扬,张扬,谢文翰,董丽杰. 类鱼骨结构CoFe₂O₄纳米纤维的制备与性能[J]. 无机材料学报, 2020, 35(9): 1011-1016.

ZHU Zhengwang,FENG Rui,LIU Yang,ZHANG Yang,XIE Wenhan,DONG Lijie. Preparation and Property of CoFe₂O₄ Nanofibers with Fishbone-like Structure[J]. Journal of Inorganic Materials, 2020, 35(9): 1011-1016.

图/表 10

图1 CoFe2O4纳米纤维制备的实验流程图

Fig. 1 Experimental flow chart for preparation of CoFe2O4 nanofibers

图2 前驱体纤维(未烧)(a), 不同温度下煅烧的CoFe2O4纳米纤维(b~f)的SEM照片

Fig. 2 SEM images of precursor fiber (unsintered) (a) and CoFe2O4 nanofibers calcined at different temperatures (b-f)

图3 前驱体纤维(未烧)和不同温度下煅烧的CoFe2O4纳米纤维的平均直径

Fig. 3 Average diameter of precursor fiber (unsintered) and CoFe2O4 nanofibers calcined at different temperatures

图4 不同温度煅烧的CoFe2O4纳米纤维XRD图谱

Fig. 4 XRD patterns of CoFe2O4 nanofibers calcined at different temperatures

图5 不同温度煅烧的CoFe2O4纤维的平均晶粒尺寸

Fig. 5 Average grain size of CoFe2O4 fibers calcined at different temperatures

图6 不同温度煅烧的CoFe2O4纳米纤维和前驱体纤维的红外图谱

Fig. 6 Infrared spectra of CoFe2O4 nanofibers and precursor fibers calcined at different temperatures

图7 CoFe2O4前驱体纤维的TG曲线

Fig. 7 TG curve of CoFe2O4 precursor fiber

图8 不同温度煅烧的CoFe2O4纳米纤维的磁滞回线

Fig. 8 Hysteresis loops of CoFe2O4 nanofibers calcined at different temperatures

图9 不同温度煅烧的CoFe2O4纳米纤维的反射损耗曲线

Fig. 9 Reflection loss curves of CoFe2O4 nanofibers calcined at different temperatures

图10 不同温度煅烧的CoFe2O4纳米纤维的C0-f曲线

Fig. 10 C0-f curves of CoFe2O4 nanofibers calcined at different temperatures

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类鱼骨结构CoFe₂O₄纳米纤维的制备与性能

Preparation and Property of CoFe₂O₄ Nanofibers with Fishbone-like Structure

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