KNN基无铅压电陶瓷的改性与机理研究
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摘要
结合BF(BM)的铁电性与LS的取代改性等综合特性,以传统的陶瓷烧结技术为制备手段,对KNN-LS-BF与KNN-LS-BM两个体系的成分、结构、相变、烧结工艺与压电、介电性能间的关系进行了系统研究。主要研究内容和创新之处如下：
系统研究了(1-x)KNN-xBF陶瓷的成分与结构、显微组织、压电介电性能的关系,结果表明：陶瓷的准同型相界成分范围为：0.01≤x≤0.02。当x=0.008时,KNN-BF陶瓷具有最好的电性能：d33=125pC／N,kp=40％,Tc=405℃,To-t=185℃,εr=432,tanδ=2.93％。系统研究了烧结温度与保温时间对陶瓷的晶体结构与相转变、组织形貌、致密度及压电、介电性能的影响。结果表明,样品在1150℃保温2h烧结时表现较好的性能：ρ=4.50 g.cm-3,εr=513.86,d33=132 pC／N, kp=45%,Qm=333.73,tanδ=2.39％。
对比研究了氧化铝和氧化锆板承烧的(1-x)(0.95KNN-0.05LS)-xBF陶瓷的掺杂量、相结构、相转变、显微组织与压电介电性能。结果表明：采用氧化锆板承烧的陶瓷的压电性能明显高于氧化铝板承烧的,而后者的Tc则高于前者；并指出,承烧板中的元素有无扩散到陶瓷中是引起两者结构与性能差别的主要机制。另外,还指出：Al元素的引入可以明显提高陶瓷的居里温度。系统研究了该体系陶瓷的成分、烧结温度与时间、相结构、相转变、显微组织及压电介电性能的关系。随着BF含量的增加,陶瓷的相结构从正交与四方相共混结构转变为四方结构,转变起始点在x=0.004时。当BF含量为0.4at.%、在1100℃烧结3h时,陶瓷有较好的性能：d33=272pC／N,kp=53％,Tc=345℃,εr=1103,tanδ=1.89％。
系统研究了(0.996-y)KNN-0.004BF-yLS陶瓷的成分、烧结温度、相结构、相转变、显微组织及压电介电性能的关系。表明：陶瓷的准同型相界的成分范围为：0.02≤y≤0.04。随着LS含量的增加,d33和kp均先增加后减小；εr先显著升高后略有下降；tanδ降低后略有回升；To-t和Tc均向低温方向移动。随烧结温度的升高,压电性能先显著提高后降低,但Tc峰先向高温区移动后向低温区方向略有偏移,当烧结温度为1100℃时,陶瓷有最好的压电性能,d33=297pC/N,kp54%。未掺杂与BF掺杂的KNN-LS陶瓷的均有较高的退极化温度,但掺杂后陶瓷的退极化温度低于未掺杂陶瓷。BF掺杂KNN-LS陶瓷具有明显的热滞现象,热滞温区为310-380℃,对应陶瓷四方相与立方相共存的温区。
系统研究了(1-x(0.95KNN-0.05LS)-xM陶瓷的成分、相结构、相转变、显微组织及压电介电性能的关系。在0≤x≤0.008范围内,室温下陶瓷具有正交相与四方相混合结构；当x=0.01时,陶瓷的结构开始具有趋于向四方相结构转变的结构特征。随BM含量的增加,陶瓷的d33和kp先增加后降低,介电损耗则先降低后略有回升,Tc先向高温区移动然后又回落,当x=0.004时,d333和kp同时达到最大值：213pC／N和0.408；tanδ达最低,为2.6%；Tc=370℃。
系统研究了(0.996-y)KNN-0.004BM-yLS陶瓷的成分、烧结温度、相结构、相转变、显微组织及压电介电性能的关系。表明：陶瓷的准同型相界的成分范围为：0.03≤y≤0.05。随着LS含量的增加,陶瓷的d33和kp均先增加后减小,当x=0.05时,均达到最大值,分别为230pC/N和0.42；陶瓷的Tc向低温方向移动。
对比研究了BF与BM在KNN-LS陶瓷中的作用。研究表明,两者对KNN、LS陶瓷的晶体结构、相变、组织结构与压电介电性能影响既有相似之处也存在明显的差别。与BM相比,BF对KNN-LS陶瓷的压电性能的促进作用更加明显。另外,也对LS与BF(BM)对KNN陶瓷的影响进行了比较研究,表明,LS在KNN陶瓷中的作用占主导地位。首次对KNN-LS-BF(BM)陶瓷的阻抗特性研究表明,BF掺杂KNN陶瓷使陶瓷呈现“硬”掺杂特性,而LS掺杂KNN和KNN-BM(BF)使陶瓷呈现“软”掺杂特性。
Based on the ferroelectricity and high Curie temperature of the perovskite-type BiFeO3 (BF) and BiMnO3 (BM), and the substitute modifying effect of LiSbO3, the relationship among the composition, structure, phase transition, sintering process, piezoelectric and dielectric properties of KNN-LS-BF(BM) ceramic systems, which were prepared by using the traditional ceramic sintering process, was studied systematically. Several important conclusions can be summarized as follows:
The relation between composition and crystalline structure, microstructure, piezoelectric properties, dielectric properties of (1-x)KNN-xBF system ceramics was systemically investigated. It was found that the morphotropic phase boundary(MPB) with orthorhombic and tetragonal co-existence crystalline structure for the ceramics lies in the range of x=0.01-0.02. The best piezoelectric properties of d33= 125 pC/N, kp=40%, Tc=405℃, To-t=185℃,εr= 432, tanδ= 2.93% were obtained at x= 0.008 which is near the MPB composition. The effects of sintering temperature and holding time on the microstructure, phase transition, density and piezoelectric properties of BF doped KNN ceramics were investigated. The 0.8at.% BF-doped KNN ceramics sintered at 1150℃for 2h exhibit excellent properties of p= 4.50 g.cm-3, d33= 132 pC/N, kp= 45%, Qm= 333.73 and tanδ= 2.39%.
Studied on comparing the doping content, phase structure, phase transition, microstructure, piezoelectric and dielectric properties of (1-x)(0.95KNN-0.05LS)-xBF ceramics sintered on zirconia and alumina setter plate. Results showed that the piezoelectric properties of the ceramics sintered on the zirconia setter plate were higher than that of the ceramics sintered on the alumina setter plate. It was pointed out that the mechanism of this difference should attribute to whether the elements in the setter plate diffuse into (1-x)(0.95KNN-0.05LS)-xBF ceramics or not. What's more, the results also showed that the addition of Al element was useful for the enhance of the Curie temperature (Tc) of (1-x)(0.95KNN-0.05LS)-xBF ceramics. The relation between composition and crystalline structure, microstructure, piezoelectric properties, dielectric properties of (1-x)(0.95KNN-0.05LS)-xBF system ceramics was also systemically investigated. With increasing the content of BF, the phase structure of the ceramic changed from the co-existence phase structure including the orthorhombic and tetragonal phase to a single tetragonal phase, and the transition point was at x= 0.004. When the content of BF is 0.4at.%, the ceramics sintered at 1100℃for 3h showed good electrical properties:d33= 272 pC/N, kp= 53%, Tc= 345℃,εr= 1103, tanδ=1.89%.
The relation between composition and crystalline structure, microstructure, piezoelectric properties, dielectric properties of (0.996-y) KNN-0.004BF-yLS system ceramics was also systemically studied. It was found that the MPB for the ceramics lies in the range of 0.02≤y≤0.04. With increasing the content of LS, the d33, kp andεr of the ceramics firstly increased and then decreased, while the tanδfirstly decreased and then increased. At the same time, both of To-t and Tc of the ceramics shifted to the low temperature with the increasing of LS content. The effects of sintering temperature on the microstructure, phase transition, density and piezoelectric properties of (0.996-y) KNN-0.004BF-yLS ceramics were also investigated. With increasing the sintering temperature, the piezoelectric properties of the ceramics firstly increased and then decreased, while the Tc firstly increased and then decreased. The ceramics sintered at 1100℃had the best piezoelectric properties: d33=297pC/N, kp=54%. BiFeO3 doped and undoped KNN-LS ceramics had a higher depolarizing temperature. The depolarizing temperature of the doped and undoped KNN-LS ceramics was 370 and 390℃, respectively. BiFeO3 doped KNN-LS ceramic show a dielectric constant-temperature behavior with a thermal hysteresis upon heating/cooling from 310-380℃which was corresponding to the temperature range of the mixed phase between tetragonal and cubic phases.
The relation between composition and crystalline structure, microstructure, piezoelectric properties, dielectric properties of (1-x)(0.95KNN-0.05LS)-xBM system ceramics was systemically investigated. It was found that the MPB for the ceramics lies in the range of 0≤x≤0.008. When x= 0.01, the structure of the ceramics started to change from the co-existence structure to the tetragonal phase structure. With increasing the content of BM, the d33 and kp of the ceramics firstly increased and then decreased, while the tanδfirstly decreased and then increased. At the same time, Tc of the ceramics firstly increased and then decreased. The best piezoelectric properties of d33=213pC/N, kp= 40.8%, Tc= 370℃, tanδ= 2.6% were obtained at x= 0.004.
The relation between composition, phase structure, phase transition, microstructure, piezoelectric properties and dielectric properties of (0.996-y) KNN-0.004BM-yLS system ceramics was also systemically studied. It was found that the MPB for the ceramics lies in the range of 0.03≤y≤0.05. With increasing the content of LS, the d33 and kp of the ceramics firstly increased and then decreased, while Tc of the ceramics shifted to the low temperature. The ceramics at x= 0.05 had the best piezoelectric properties:d33=230 pC/N,kp=42%.
The mechanisms of BF(BM) in the KNN-LS ceramics were studied by contrast. The results showed that on the one hand, the effect of BF on the crystalline structure, phase transition, microstructure, piezoelectric and dielectric properties was similar with that of BM, and was differ from that of BM on the other hand. Comparing with BM-doping, the improving effect of BF-doping on the piezoelectric properties of KNN-LS ceramics was greater. The mechanisms of LS and BF(BM) in the pure KNN ceramics were also studied by contrast. The results showed that the effect of LS on KNN-LS-BF(BM) ceramics occupied the leading position. Studying on the frequency dependence of the impedance and phase angle for the ceramics showed that BF doped KNN ceramics showed the "hard" characteristics, while the LS doped KNN and KNN-BF(BM) ceramics showed "soft" characteristics.
系统研究了(1-x)KNN-xBF陶瓷的成分与结构、显微组织、压电介电性能的关系,结果表明：陶瓷的准同型相界成分范围为：0.01≤x≤0.02。当x=0.008时,KNN-BF陶瓷具有最好的电性能：d33=125pC／N,kp=40％,Tc=405℃,To-t=185℃,εr=432,tanδ=2.93％。系统研究了烧结温度与保温时间对陶瓷的晶体结构与相转变、组织形貌、致密度及压电、介电性能的影响。结果表明,样品在1150℃保温2h烧结时表现较好的性能：ρ=4.50 g.cm-3,εr=513.86,d33=132 pC／N, kp=45%,Qm=333.73,tanδ=2.39％。
对比研究了氧化铝和氧化锆板承烧的(1-x)(0.95KNN-0.05LS)-xBF陶瓷的掺杂量、相结构、相转变、显微组织与压电介电性能。结果表明：采用氧化锆板承烧的陶瓷的压电性能明显高于氧化铝板承烧的,而后者的Tc则高于前者；并指出,承烧板中的元素有无扩散到陶瓷中是引起两者结构与性能差别的主要机制。另外,还指出：Al元素的引入可以明显提高陶瓷的居里温度。系统研究了该体系陶瓷的成分、烧结温度与时间、相结构、相转变、显微组织及压电介电性能的关系。随着BF含量的增加,陶瓷的相结构从正交与四方相共混结构转变为四方结构,转变起始点在x=0.004时。当BF含量为0.4at.%、在1100℃烧结3h时,陶瓷有较好的性能：d33=272pC／N,kp=53％,Tc=345℃,εr=1103,tanδ=1.89％。
系统研究了(0.996-y)KNN-0.004BF-yLS陶瓷的成分、烧结温度、相结构、相转变、显微组织及压电介电性能的关系。表明：陶瓷的准同型相界的成分范围为：0.02≤y≤0.04。随着LS含量的增加,d33和kp均先增加后减小；εr先显著升高后略有下降；tanδ降低后略有回升；To-t和Tc均向低温方向移动。随烧结温度的升高,压电性能先显著提高后降低,但Tc峰先向高温区移动后向低温区方向略有偏移,当烧结温度为1100℃时,陶瓷有最好的压电性能,d33=297pC/N,kp54%。未掺杂与BF掺杂的KNN-LS陶瓷的均有较高的退极化温度,但掺杂后陶瓷的退极化温度低于未掺杂陶瓷。BF掺杂KNN-LS陶瓷具有明显的热滞现象,热滞温区为310-380℃,对应陶瓷四方相与立方相共存的温区。
系统研究了(1-x(0.95KNN-0.05LS)-xM陶瓷的成分、相结构、相转变、显微组织及压电介电性能的关系。在0≤x≤0.008范围内,室温下陶瓷具有正交相与四方相混合结构；当x=0.01时,陶瓷的结构开始具有趋于向四方相结构转变的结构特征。随BM含量的增加,陶瓷的d33和kp先增加后降低,介电损耗则先降低后略有回升,Tc先向高温区移动然后又回落,当x=0.004时,d333和kp同时达到最大值：213pC／N和0.408；tanδ达最低,为2.6%；Tc=370℃。
系统研究了(0.996-y)KNN-0.004BM-yLS陶瓷的成分、烧结温度、相结构、相转变、显微组织及压电介电性能的关系。表明：陶瓷的准同型相界的成分范围为：0.03≤y≤0.05。随着LS含量的增加,陶瓷的d33和kp均先增加后减小,当x=0.05时,均达到最大值,分别为230pC/N和0.42；陶瓷的Tc向低温方向移动。
对比研究了BF与BM在KNN-LS陶瓷中的作用。研究表明,两者对KNN、LS陶瓷的晶体结构、相变、组织结构与压电介电性能影响既有相似之处也存在明显的差别。与BM相比,BF对KNN-LS陶瓷的压电性能的促进作用更加明显。另外,也对LS与BF(BM)对KNN陶瓷的影响进行了比较研究,表明,LS在KNN陶瓷中的作用占主导地位。首次对KNN-LS-BF(BM)陶瓷的阻抗特性研究表明,BF掺杂KNN陶瓷使陶瓷呈现“硬”掺杂特性,而LS掺杂KNN和KNN-BM(BF)使陶瓷呈现“软”掺杂特性。
Based on the ferroelectricity and high Curie temperature of the perovskite-type BiFeO3 (BF) and BiMnO3 (BM), and the substitute modifying effect of LiSbO3, the relationship among the composition, structure, phase transition, sintering process, piezoelectric and dielectric properties of KNN-LS-BF(BM) ceramic systems, which were prepared by using the traditional ceramic sintering process, was studied systematically. Several important conclusions can be summarized as follows:
The relation between composition and crystalline structure, microstructure, piezoelectric properties, dielectric properties of (1-x)KNN-xBF system ceramics was systemically investigated. It was found that the morphotropic phase boundary(MPB) with orthorhombic and tetragonal co-existence crystalline structure for the ceramics lies in the range of x=0.01-0.02. The best piezoelectric properties of d33= 125 pC/N, kp=40%, Tc=405℃, To-t=185℃,εr= 432, tanδ= 2.93% were obtained at x= 0.008 which is near the MPB composition. The effects of sintering temperature and holding time on the microstructure, phase transition, density and piezoelectric properties of BF doped KNN ceramics were investigated. The 0.8at.% BF-doped KNN ceramics sintered at 1150℃for 2h exhibit excellent properties of p= 4.50 g.cm-3, d33= 132 pC/N, kp= 45%, Qm= 333.73 and tanδ= 2.39%.
Studied on comparing the doping content, phase structure, phase transition, microstructure, piezoelectric and dielectric properties of (1-x)(0.95KNN-0.05LS)-xBF ceramics sintered on zirconia and alumina setter plate. Results showed that the piezoelectric properties of the ceramics sintered on the zirconia setter plate were higher than that of the ceramics sintered on the alumina setter plate. It was pointed out that the mechanism of this difference should attribute to whether the elements in the setter plate diffuse into (1-x)(0.95KNN-0.05LS)-xBF ceramics or not. What's more, the results also showed that the addition of Al element was useful for the enhance of the Curie temperature (Tc) of (1-x)(0.95KNN-0.05LS)-xBF ceramics. The relation between composition and crystalline structure, microstructure, piezoelectric properties, dielectric properties of (1-x)(0.95KNN-0.05LS)-xBF system ceramics was also systemically investigated. With increasing the content of BF, the phase structure of the ceramic changed from the co-existence phase structure including the orthorhombic and tetragonal phase to a single tetragonal phase, and the transition point was at x= 0.004. When the content of BF is 0.4at.%, the ceramics sintered at 1100℃for 3h showed good electrical properties:d33= 272 pC/N, kp= 53%, Tc= 345℃,εr= 1103, tanδ=1.89%.
The relation between composition and crystalline structure, microstructure, piezoelectric properties, dielectric properties of (0.996-y) KNN-0.004BF-yLS system ceramics was also systemically studied. It was found that the MPB for the ceramics lies in the range of 0.02≤y≤0.04. With increasing the content of LS, the d33, kp andεr of the ceramics firstly increased and then decreased, while the tanδfirstly decreased and then increased. At the same time, both of To-t and Tc of the ceramics shifted to the low temperature with the increasing of LS content. The effects of sintering temperature on the microstructure, phase transition, density and piezoelectric properties of (0.996-y) KNN-0.004BF-yLS ceramics were also investigated. With increasing the sintering temperature, the piezoelectric properties of the ceramics firstly increased and then decreased, while the Tc firstly increased and then decreased. The ceramics sintered at 1100℃had the best piezoelectric properties: d33=297pC/N, kp=54%. BiFeO3 doped and undoped KNN-LS ceramics had a higher depolarizing temperature. The depolarizing temperature of the doped and undoped KNN-LS ceramics was 370 and 390℃, respectively. BiFeO3 doped KNN-LS ceramic show a dielectric constant-temperature behavior with a thermal hysteresis upon heating/cooling from 310-380℃which was corresponding to the temperature range of the mixed phase between tetragonal and cubic phases.
The relation between composition and crystalline structure, microstructure, piezoelectric properties, dielectric properties of (1-x)(0.95KNN-0.05LS)-xBM system ceramics was systemically investigated. It was found that the MPB for the ceramics lies in the range of 0≤x≤0.008. When x= 0.01, the structure of the ceramics started to change from the co-existence structure to the tetragonal phase structure. With increasing the content of BM, the d33 and kp of the ceramics firstly increased and then decreased, while the tanδfirstly decreased and then increased. At the same time, Tc of the ceramics firstly increased and then decreased. The best piezoelectric properties of d33=213pC/N, kp= 40.8%, Tc= 370℃, tanδ= 2.6% were obtained at x= 0.004.
The relation between composition, phase structure, phase transition, microstructure, piezoelectric properties and dielectric properties of (0.996-y) KNN-0.004BM-yLS system ceramics was also systemically studied. It was found that the MPB for the ceramics lies in the range of 0.03≤y≤0.05. With increasing the content of LS, the d33 and kp of the ceramics firstly increased and then decreased, while Tc of the ceramics shifted to the low temperature. The ceramics at x= 0.05 had the best piezoelectric properties:d33=230 pC/N,kp=42%.
The mechanisms of BF(BM) in the KNN-LS ceramics were studied by contrast. The results showed that on the one hand, the effect of BF on the crystalline structure, phase transition, microstructure, piezoelectric and dielectric properties was similar with that of BM, and was differ from that of BM on the other hand. Comparing with BM-doping, the improving effect of BF-doping on the piezoelectric properties of KNN-LS ceramics was greater. The mechanisms of LS and BF(BM) in the pure KNN ceramics were also studied by contrast. The results showed that the effect of LS on KNN-LS-BF(BM) ceramics occupied the leading position. Studying on the frequency dependence of the impedance and phase angle for the ceramics showed that BF doped KNN ceramics showed the "hard" characteristics, while the LS doped KNN and KNN-BF(BM) ceramics showed "soft" characteristics.
引文
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