近年來，由於國際上對於環保問題的日漸重視，使得許多有毒元素及材料已逐漸被禁止，由於壓電陶瓷目前是以含鉛材料為主(如PZT陶瓷)，所以尋找可替代之材料是現今刻不容緩的研究方向。本論文針對無鉛壓電陶瓷材料中較具發展潛力的鈦酸鉍鉀鈉(Bi0.5Na0.5-xKx)TiO3 [BNKT]二元固溶系統，探討材料缺陷評估，微觀特徵與材料燒結環境對電性行為的影響。另外，利用電子顯微鏡和Impedance spectroscopy進行導電率的量測與分析去探討BNT-based和PZN-based壓電陶瓷之晶粒與晶界微觀結構與電性之關聯性。同時微波燒結之製程技術被運用於燒結鉛系壓電陶瓷0.5 (0.94PbZn1/3Nb2/3O3 + 0.06BaTiO3) + 0.5 PbZr0.52Ti0.48O3 (PBZNZT)材料與非鉛壓電陶瓷(BNKT)材料，去瞭解微波能量對不同材料作用之差異性及探討材料吸收微波之機制。
實驗結果顯示：BNKT陶瓷具有二次相之存在，二次相之形成可能起因於鈦離子與鉀離子基於燒結期間熱力學反應能量較穩定，因而形成二次相，此結果形成了材料內化學計量比之偏離導致鈦空缺、氧空缺、鈦價數轉移，並影響了鐵電與介電特性，而非僅是文獻所提因為元素揮發造成之缺陷並影響電性。試片經由高氧氣氛下燒結或經由退火處理，能夠改善鈦價數轉移並且有效地降低漏電流，提升鐵電與介電特性。鋰之添加抑制二次相與鈦價數轉移缺陷之形成，結果降低漏電流並且提升了鐵電與介電特性，這可能歸因於鋰加強了A，B-site離子與氧之鍵結強度進而穩定perovskite 結構和抑制二次相生成。
交流阻抗圖譜技術分析BNKT 和 PBZNZT壓電陶瓷探討微觀結構和導電率之間的關聯性，結果顯示在BNKT 和 PBZNZT材料上由於不同的微觀結構展現不同的導電行為，BNKT陶瓷的晶界呈現較完整的原子排列和薄的晶界，同時試片破斷面之SEM影像展現穿晶破裂。交流阻抗分析之複數阻抗圖譜顯現偏向只有一個半圓弧出現在複數阻抗圖譜上，並且在高溫量測時晶界之半圓貢獻不明顯，同時晶界導電率活化能高於晶粒導電率活化能，意含著BNKT陶瓷晶粒內Bi2O3 的揮發導致晶粒內誘發一個比較容易的導電路徑。另一方面，PBZNZT陶瓷在晶界處展現一個比較厚的非晶相層，而且試片破斷面之SEM影像展現沿晶破裂。交流阻抗分析之複數阻抗圖譜呈現了二個較明顯半圓弧圖形，而導電率活化能分析指出晶界導電率活化能低於晶粒導電率活化能，這可能歸因於高溫下處於晶界之非晶相層電荷載子參與了導電行為。一種導電模式基於晶粒與晶界之間之傳導行為被提出，晶界厚度藉由AC impedance數據被計算，並比較於電子顯微鏡之微觀研究，結果發現AC impedance之結果與微觀結構之間有一致的關聯性，建議阻抗圖譜能作為鐵電陶瓷晶界微觀結構之評估手法。
微波燒結製程使用於鉛基PBZNZT與非鉛BNKT壓電陶瓷，實驗結果顯示PBZNZT與BNKT壓電陶瓷展現不同的微波吸收效率，在相同密度下PBZNZT與BNKT陶瓷微波製程試片之晶粒尺寸較傳統製程試片之晶粒尺寸小，同時PBZNZT陶瓷之微波製程燒結溫度明顯展現較傳統製程之燒結溫度低，意謂著PBZNZT陶瓷擁有較佳之微波吸收能力，這可能歸因於介電常數與偶極損失(dipole loss)的貢獻，因此介電特性可能是導致鐵電/壓電陶瓷材料能否有效吸收微波能量之重要依據。HRTEM與EDS研究指出PBZNZT陶瓷之微波燒結製程較傳統製程在相同密度下比較展現少的PbO 與 ZnO元素之偏析，另一方面，BNKT陶瓷微波與傳統燒結試片晶界處並未有明顯之成份偏析，然而PBZNZT與BNKT陶瓷之微波製程試片展現較均勻之成份與結晶性，這結果改善了材料之電性。

In recent years, lead-based Pb(ZrTi)O3 materials have been restricted to use by legislation in some countries. The toxicity of lead oxide jeopardize human's health and pollute the environment. Recently, many scientists are devoted to investigating lead-free piezoelectric ceramics. (Bi0.5Na0.5)TiO3 [BNT] ceramics is thought to be the candidates as the alternative system. Therefore, the aims of this dissertation are attempted to investigate (Bi0.5(Na1-xKx)0.5)TiO3 ceramics with the effects of defects on electrical properties. On the other hand, the microstructural difference at grain and grain boundary between BNKT and PBZNZT ceramics using electron microscopy and correlated with measurements of electrical conductivity by complex impedance analysis. At the same time, comparative study was also carried out to understand microstructures and electrical properties of PBZNZT and BNKT ceramics by microwave heating technology.
According to our investigations, the second phase formation in BNKT ceramics might arise from thermodynamic stability of potassium titanate during sintering. The results produce compositional inhomogeneity and generate more oxygen and titanium vacancies in defective perovskite lattice, which obviously affects electrical properties in BNKT ceramics. The specimens sintered under higher oxygen atmosphere and post-oxidation annealing treatment could improve Ti valence transition and effectively decreases the leakage current. On the other hand, Li addition to BNKT ceramics can suppress formation of second phase and Ti valence transition, which decreased leakage current and promoted ferroelectric and dielectric properties. This might be attributed to that Li addition contributes to the binding energy among A, B-site cations with oxygen to stabilize the structure.
Impedance spectroscopy studies have been successfully performed in BNKT and PBZNZT piezoelectric ceramics to correlate microstructures with electrical conduction behavior. The results indicate that different microstructures between BNKT and PBZNZT ceramics display distinct differences in conductivity behavior. BNKT ceramics exhibit clean and thin grain boundaries and transgranular fracture surface. Impedance analysis shows only one semicircle in complex impedance plots and the contribution of grain boundaries is not obvious at higher temperatures. The activation energy of grain boundary conductivity is higher than that of grains for BNKT system, indicating Bi2O3 evaporation of grains induces an easy conduction path through grains in BNKT ceramics. On the other hand, PBZNZT ceramics exhibit a thick amorphous layer at grain boundaries and intergranular type fracture. Impedance analysis shows obvious two semicircles in complex impedance plots and activation energy of grain boundary conductivity is lower than that of grains for PBZNZT. This might be attributed to the charged particles in the amorphous phase at the grain boundaries, participating in the conduction process at high temperatures. A conduction model based upon microstructures considering both grain and grain boundary conductivities was proposed. The grain boundary thickness was calculated through AC impedance data and compared with the electron microscopic investigations. It was found that microstructural characteristics and AC impedance data of the ferroelectric ceramics can be correlated fairly well, suggesting that impedance spectroscopy can be employed in grain boundary engineering for ferroelectric ceramics.
Microwave sintering process had been successfully performed in PBZNZT and BNKT piezoelectric ceramics. The results indicate that PBZNZT and BNKT specimens displayed the different absorption efficiency of microwave energy. The grain size of MWS process for PBZNZT and BNKT specimens was smaller than that of CS process under the same densification and PBZNZT samples could achieve a significantly lower sintering temperature in MWS process, which implied that PBZNZT specimens displayed more efficient adsorption ability of microwave energy. It might be attributed to the contribution of dielectric constant and dipole loss. Therefore, the dielectric properties might dominant the adsorption ability of microwave energy for ferroelectric and pizeoelctric materials. HRTEM and energy dispersive spectroscopic investigations show that the grain boundaries of MW samples contain less PbO and ZnO segregation than those of the CS samples for PBZNZT specimens. On the other hand, BNKT specimens display no compositional segregation at grain boundaries for CS and MWS process. However, MWS process could efficiently achieve more uniform composition for PBZNZT and BNKT ceramics, and the result improved the electrical properties.

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