大长径比压电陶瓷管的制备及性能研究
发布时间:2018-05-17 08:26
本文选题:PZT5压电陶瓷管 + 大长径比 ; 参考:《济南大学》2015年硕士论文
【摘要】:相比于传统块状、片状压电陶瓷材料,大长径比压电陶瓷管不仅具有优良的压电、介电性能,还具有柔韧性好,体积小,易与基体结构集成,以及使用时电场损失小等特点。大长径比压电陶瓷管的制备可以有效的解决传统压电陶瓷材料集成时对结构强度和可靠性影响大的问题,进一步推动主动振动控制复合材料及压电储能复合材料的优化和应用。本文以PZT5压电陶瓷预烧粉为原料,采用塑性聚合物-挤制成型法制备固相含量不同的PZT5大长径比压电陶瓷管素坯;经排胶及不同条件下烧结,制得PZT5大长径比压电陶瓷管。分别采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和排水法测定陶瓷管的相组成、显微结构和体积密度。研究了陶瓷泥料配方、烧成温度、保温时间和烧成气氛对PZT5陶瓷管相组成、显微结构和体积密度的影响。结果表明,采用塑性聚合物-挤制成型法可成功制备出平直、表面光滑的长150mm,外径1.98 mm,内径0.8mm的PZT5大长径比压电陶瓷管;最佳陶瓷泥料配方为陶瓷预烧粉:聚乙烯醇水溶液(10%):丙三醇=26:3:1,此时陶瓷固相含量为87%;最佳烧成条件为1290℃下烧结,保温2h,同时采用ZrO2和Pb304的混合物作为埋烧粉;所得陶瓷管由单一钙钛矿相组成,无Zr02、烧绿石或其他杂相;晶粒大小均匀,晶界清晰,结构致密,晶粒尺寸为2-5μm,体积密度为7.70 g/cm3。采用化学镀镍法在PZT5大长径比压电陶瓷管内外壁镀覆电极。首先,以镀速和电阻率为指标,采用正交试验法确定出PZT5大长径比压电陶瓷管化学镀镍最佳粗化工艺参数;然后,采用单因素实验法研究各粗化参数对PZT5大长径比压电陶瓷管化学镀镍层性能的影响;最后,综合对比两组实验结果,确定PZT5大长径比压电陶瓷管化学镀镍最佳粗化方案。结果表明,PZT5大长径比压电陶瓷管内外壁化学镀镍最优粗化方案为:粗化液中氢氧化钠质量分数为20%、粗化温度为25℃、粗化时间为35 min、粗化液中乙二胺浓度为30 mL/L。选用此粗化方案对PZT5大长径比压电陶瓷管进行粗化处理,可在PZT5陶瓷管内外壁获得光亮、均匀、致密、结合力好、电阻率小的镍电极。采用真空极化法对PZT5大长径比压电陶瓷管进行极化处理。采用Agilent 4294A型精密阻抗分析仪测量极化后PZT5大长径比压电陶瓷管的谐振频率fr、反谐振频率fa、电容C和介电损耗tanδ,并通过谐振频率-反谐振频率法与电容法推算PZT5压电陶瓷管的横向机电耦合系数K31和相对介电常数εr。研究了极化电场、极化温度、极化时间对PZT5大长径比压电陶瓷管压电、介电性能的影响。结果表明,采用真空极化法可成功实现PZT5大长径比压电陶瓷管的有效极化;最佳极化参数为:极化电场为2.0 kV/mm,极化温度为25℃,极化时间为10 min。用ZJ-6A型准静态d33测量仪测量PZT5压电陶瓷管的压电应变常数d33。用Agilent4294A型精密阻抗分析仪测试陶瓷管在1 kHz时的电容C和介电损耗tanδ,并进一步推算PZT5压电陶瓷管的相对介电常数εr。用Agilent 4294A型精密阻抗分析仪测试陶瓷管的谐振频率fr、反谐振频率fa及最小阻抗Zmin,并通过谐振频率-反谐振频率法推算出PZT5大长径比压电陶瓷管的横向机电耦合系数K31和机械品质因素Qm。测试及计算结果如下:压电应变常数d33为579 pC/N,横向机电耦合系数K31为0.49,相对介电常数εr为1789,介电损耗tanδ为0.026,机械品质因素Qm为11。
[Abstract]:Compared with the traditional block - shaped piezoelectric ceramic tube , the piezoelectric ceramic tube not only has excellent piezoelectric and dielectric properties , but also has the characteristics of good flexibility , small volume , easy integration with the base structure , small electric field loss during use , and the like , and further promotes the optimization and application of the active vibration control composite material and the piezoelectric energy storage composite material .
The phase composition , microstructure and bulk density of PZT5 ceramic tube were measured by means of X - ray diffraction ( XRD ) , scanning electron microscope ( SEM ) and drainage method . The effects of the formula , firing temperature , holding time and firing atmosphere on the composition , microstructure and bulk density of PZT5 ceramic tube were studied .
The best ceramic paste formulation is ceramic pre - sintered powder : polyvinyl alcohol aqueous solution ( 10 % ) : glycerol = 26 : 3 : 1 , at this time the content of ceramic solid phase is 87 % ;
the best firing condition is sintering at 129.degree . C . for 2 h , and the mixture of ZrO2 and Pb304 is adopted as the embedded burning powder ;
The obtained ceramic tube is composed of a single perovskite phase , no Zr02 , pyrochlore or other impurities ;
The size of grain is uniform , the grain boundary is clear , the structure is compact , the grain size is 2 - 5 渭m , the volume density is 7.70 g / cm3 .
Then , the influence of roughening parameters on the properties of electroless nickel plating layer of PZT5 was studied by single factor experiment .
The results show that the optimal scheme for electroless nickel plating of PZT5 large - length - diameter piezoelectric ceramic tube is as follows : the mass fraction of sodium hydroxide in the coarse liquid is 20 % , the roughening temperature is 25 鈩,
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