低温烧结CoFe2O4-(PZN-PZT)多铁复合材料磁电性能研究

doi:10.15541/jim20150548

摘要/Abstract

摘要：

采用传统陶瓷工艺和低温烧结制备了CoFe₂O₄-(PZN-PZT)多铁复合陶瓷, 研究了混合方式、PZT包覆和成分变化对其结构、磁性能、磁电耦合性能的影响。XRD图谱和TEM照片显示, 采用溶胶-凝胶和包覆搅拌混合的方法获得了CoFe₂O₄/PZT核壳结构粉末, 在CoFe₂O₄表面形成了10~20 nm的钙钛矿PZT壳层。EDS结果显示, 低温烧结和阻挡层可以有效抑制两相间的元素扩散。SEM照片和磁电性能结果显示, 相对未包覆研磨混合工艺, 包覆搅拌混合可以提高磁性颗粒复合含量, 获得较好烧结匹配性, 有效提高材料的磁电耦合性能。研究结果表明, 包覆搅拌混合制备体积比为4:6的CoFe₂O₄-(PZN-PZT)样品, 经1000℃烧结, 在10 kHz下获得最大磁电耦合系数(18.3 mV/(cm·Oe))。

关键词: 多铁, 磁电耦合, 核壳结构, 磁性能

Abstract:

CoFe₂O₄-(PZN-PZT) multiferroic composite ceramics were prepared by low temperature sintering using traditional ceramic method. The influences of mixed mode, PZT shell and composition on structure, magnetic and magnetoelectric coupling properties were studied. XRD and TEM results show that CoFe₂O₄/PZT core-shell nanostructured particles are prepared by the Sol-Gel method. A 10-20 nm thick PZT shell formed on the surface of CoFe₂O₄ particle. EDS analyses show that low temperature sintering and barrier layer effectively inhibit the elements diffusion of the two phases. SEM images and magnetoelectric property measurement show that PZT shell coated on CoFe₂O₄ particles and the stirring process improve the magnetic particles content in com-position, match the sintering process perfectly, and improve the magnetoelectric coupling properties effectively. The coated and stirred sample CoFe₂O₄-(PZN-PZT) with volume ratio of 4:6 which sintered at 1000℃ show maximum magnetoelectric coupling coefficient of (18.3 mV/(cm·Oe)) at 10 kHz.

Key words: multiferroic, magnetoelectric coupling, core-shell structure, magnetic properties

中图分类号:

O469
O432

范桂芬, 徐星, 王凯, 吕文中, 梁飞, 金善龙. 低温烧结CoFe₂O₄-(PZN-PZT)多铁复合材料磁电性能研究[J]. 无机材料学报, 2016, 31(6): 561-566.

FAN Gui-Fen, XU Xing, WANG Kai, LV Wen-Zhong, LIANG Fei, JIN Shan-Long. Magnetoelectric Properties of Low Temperature Sintered CoFe₂O₄-(PZN-PZT) Multiferroic Composite Materials[J]. Journal of Inorganic Materials, 2016, 31(6): 561-566.

图/表 10

图1 CFO粉末和CFO/PZT粉末的XRD图谱

Fig. 1 XRD patterns of CFO powder and CFO/PZT powder. (a) Non-treated CFO; (b) Coated but non-calcined CFO/PZT; (c) Coated and calcined CFO/PZT

图2 包覆煅烧的CFO/PZT粉末的TEM照片

Fig. 2 TEM image of CFO/PZT powder coated after calcinations

图3 不同温度烧结,未包覆研磨混合体积比2:8的CFO- (PZN-PZT)复合陶瓷的d33

Fig. 3 d33 of non-coated and grinded CFO/PZN-PZT composite ceramics with volume ratio of 2:8 sintered at different temperatures

图4 未包覆搅拌混合不同体积比CFO-(PZN-PZT)复合陶瓷的XRD图谱

Fig. 4 XRD patterns of non-coated and stirred CFO-(PZN- PZT) composite ceramics with different volume ratios of CFO. (a) 10%; (b) 20%; (c) 30%; (d) 40%; (e) 50%

图5 体积比2:8的CFO-(PZN-PZT)复合多铁陶瓷断面SEM照片

Fig. 5 SEM imges of CFO-(PZN-PZT) composite ceramics section with volume ratio of 2:8. (a) Non-coated and grinded; (b) Non-coated and stirred; (c) Coated and stirred

表1 体积比2:8的CFO-(PZN-PZT)复合多铁陶瓷EDS成分分析

Table 1 EDS analyses of CFO-(PZN-PZT) composite ceramics with volume ratio of 2:8

Element	O	Ti	Fe	Co	Zn	Zr	Nb	Pb
Red cross section in Figure 5 (a)/at%	68.48	2.47	12.38	7.26	3.49	1.52	1.93	2.46
Red cross section in Figure 5 (c)/at%	74.88	2.63	7.07	3.42	2.15	2.10	4.46	3.28

图6 不同工艺制备CFO-(PZN-PZT)复合多铁陶瓷d33值随CFO成分的变化

Fig. 6 d33 value as functions of CFO volume ratio in CFO- (PZN-PZT) composite ceramics prepared with different processes

图7 不同工艺制备CFO-(PZN-PZT)复合多铁陶瓷的电滞回线

Fig. 7 Hysteresis loops of CFO-(PZN-PZT) composite ceramics prepared with different processes. (a) Non-coated and stirred; (b) Volume ratio of 2:8

图8 包覆搅拌混合制备CFO-(PZN-PZT)复合多铁陶瓷的磁滞回线

Fig. 8 Magnetic loops of CFO-(PZN-PZT) composite ceramics prepared with coating and stirring processes

图9 10 kHz下不同制备工艺CFO-(PZN-PZT)复合多铁陶瓷的磁电耦合系数变化曲线

Fig. 9 Magnetoelectric coupling coefficient curves of CFO- (PZN-PZT) composite multiferroic ceramics at 10 kHz with different process. (a) Coated and stirred; (b) Volume ratio of 2:8

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低温烧结CoFe₂O₄-(PZN-PZT)多铁复合材料磁电性能研究

Magnetoelectric Properties of Low Temperature Sintered CoFe₂O₄-(PZN-PZT) Multiferroic Composite Materials

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