电泳沉积法制备PNN-PZT厚膜的研究

doi:10.3724/SP.J.1077.2012.00379

摘要/Abstract

摘要：

利用电泳沉积法在φ50 μm的铂金丝上制备了厚度约50 μm的0.2Pb(Ni_1/3Nb_2/3)O₃-(0.8-x)PbTiO₃-xPbZrO₃ (PNN-PZT)致密压电陶瓷厚膜. 研究了不同聚合度的分散剂聚乙二醇(PEG)对悬浮液的Zeta电势和厚膜表面形貌的影响.结果显示, 加入高聚合度的分散剂PEG10000所制得的悬浮液比加入低聚合度的分散剂PEG6000制得的悬浮液更稳定, 并且电泳沉积得到的厚膜也更加致密. 本研究解释了不同聚合度的PEG对悬浮液稳定的可能原因, 并比较了连续电泳沉积法与分步电泳沉积法对厚膜表面形貌的影响, 结果表明采用分步电泳沉积法制备的厚膜更加致密. 研究了不同的烧结温度对PNN-PZT厚膜形貌和介电性能的影响, 结果显示烧结温度为1180℃时, 厚膜的介电性能最好, 介电常数达988, 介电损耗为3.7%. 测试了1180℃烧结的PNN-PZT厚膜的电压位移曲线和电滞回线, 结果表明厚膜的有效压电常数为90 pm/V,剩余极化为6.00 kV/cm.

关键词: 电泳沉积, PNN-PZT厚膜, 聚乙二醇

Abstract:

0.2Pb(Ni_1/3Nb_2/3)O₃-(0.8-x)PbTiO₃-xPbZrO₃ (PNN-PZT) dense piezoelectric thick films with the thickness of about 50 μm were fabricated by electrophoretic deposition(EPD) on Pt wire. Effects of different dispersants to the Zeta potential of the suspension and the microstructures of the PNN-PZT thick films were evaluated. The results shows that suspension with polyethyleneglycol 10000 is more stable than the suspension with polyethyleneglycol 6000, and the thick films deposited from suspension with polyethyleneglycol 10000 is more denser. The effects of different dispersants on the stability of the suspension and the influences of different deposition methods on the microstructures of the thick films were discussed. The result shows that dense thick films can be fabricated by stepwise deposition. The effect of different sintering temperatures to the dielectric constant and the dielectric loss of PNN-PZT thick films at room temperature were investigated. The dielectric constant and the dielectric loss at room temperature of the PNN-PZT thick film sintered at 1180℃ for 30 min are 988 and 3.7% respectively. The electric induced displacement (E-D) curve and hysteresis loop of the PNN-PZT thick films were measured. The effective piezoelectric constant and the residual polarization of the PNN-PZT films are 90 pm/V and 6.00 kV/cm, respectively.

Key words: electrophoretic deposition, PNN-PZT thick films, polyethylene glycol

中图分类号:

卢剑萍, 李国荣, 郑嘹赢, 曾江涛, 曾华荣, 卞建江. 电泳沉积法制备PNN-PZT厚膜的研究[J]. 无机材料学报, 2012, 27(4): 379-384.

LU Jian-Ping, LI Guo-Rong, ZHENG Liao-Ying, ZENG Jiang-Tao, ZENG Hua-Rong, BIAN Jian-Jiang. Investigation of PNN-PZT Thick Films Fabricated by Electrophoretic Deposition[J]. Journal of Inorganic Materials, 2012, 27(4): 379-384.

图/表 9

图1 为加入分散剂聚乙二醇6000(PEG6000)和聚乙二醇10000 (PEG10000)时悬浮液的Zeta电势随pH值的变化情况. 悬浮液的稳定性可以通过Zeta电势的大小来表征: Zeta电势越大, 颗粒之间斥力越大, 颗粒越不容易团聚, 悬浮液越稳定. 通常25?mV是阻止团聚的最小值[14]. 图1中, 加入PEG6000悬浮液的Zeta电位最大值出现在pH=5.2, 此时Zeta电位为40?mV. 加入PEG10000的悬浮液的Zeta电位最大值出现在pH=4.5, 此时Zeta电位为56?mV.在酸性条件下, 加入PEG10000悬浮液在较宽的pH值(2.5~7)范围内Zeta电势都大于25?mV; 而加入PEG6000悬浮液的Zeta电势大于25?mV的pH值(3.7~7)范围比加入PEG10000悬浮液的小. 在pH值相同时, 加入PEG10000悬浮液的Zeta电势比加入PEG6000悬浮液的Zeta电势大, 表明在酸性条件下, 加入PEG10000的悬浮液更加稳定, 适合用于电泳沉积. 在碱性条件下, pH值相同时, 加入PEG6000的Zeta电势比加入PEG10000的悬浮液的Zeta电势略大一点, 但是, 分别加入这两种分散剂时悬浮液的Zeta电势都比较小, 当pH值达到11时, 两者的Zeta电势仍然小于25?mV, 这表明在碱性条件下, 悬浮液不够稳定, 不适合于电泳沉积.

图1 PEG10000和PEG6000对PNN-PZT乙醇悬浮液Zeta电位的影响

Fig. 1 Effects of PEG10000 and PEG6000 on the Zeta potential of PNN-PZT ethanol suspension

图2 (a)酸性和(b)碱性悬浮液中PNN-PZT颗粒表面聚合物高分子链的吸附模型

Fig. 2 Adsorption models of the polymer chain on PNN-PZT particle surface in (a) acidic and (b) basic suspensions

图3 添加不同分散剂的厚膜在1180℃保温30 min后的SEM照片

Fig. 3 SEM images of the thick films with different dispersants deposited by continuous deposition and then sintered at 1180℃ for 30 min (a) PEG6000; (b) PEG10000

图4 连续沉积方法(a)和分步沉积法(b)并在1180℃保温30 min制得的厚膜的表面SEM照片

Fig. 4 SEM images of the thick films deposited by continuous deposition (a) and stepwise deposition (b) and then sintered at 1180℃ for 30 min

图5 不同温度烧结PNN-PZT厚膜表面的SEM照片

Fig. 5 Surface SEM images of PNN-PZT thick films sintered at different temperatures

图6 烧结温度对PNN-PZT厚膜室温下的介电常数和介电损耗的影响

Fig. 6 Effects of sintering temperatures on the dielectric constant and dielectric loss of PNN-PZT thick films measured at room temperature

图7 1180℃烧结30?min的PNN-PZT厚膜的电压位移(E-D)曲线

Fig. 7 Electric ﬁeld induced displacement (E-D) of the PNN-PZT thick film sintered at 1180℃ for 30 min

图8 1180℃烧结30?min的PNN-PZT厚膜的电滞回线

Fig. 8 Hysteresis loop of PNN-PZT thick film sintered at 1180℃ for 30 min

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