臺灣博碩士論文加值系統

A(B'1/3B"2/3)O3-type (A= Ba+2, Ca+2; B' = Mg+2 , Zn+2; B" = Nb+5, Ta+5)複合鈣鈦礦型結構的化合物,具有B位置陽離子序化的結構,且在微波頻率下仍存在非常低的介電損耗,但是高成本的鉭氧化物使得應用上不具成本效益.因此,此研究針對複合鈣鈦礦型結構的鈮氧化物,探討其結構與微波介電性質之間的關係.
Ba(Zn1/3Nb2/3)O3 化合物在之前的研究已經被報導具優異的微波介電特性,且其品質因子和序化的晶體結構有顯著的關係,此研究以拉曼光譜儀;X光繞射儀及穿透式電子顯微鏡, 探討�y燒條件對序化結構的演變及品質因子的影響.目前的結果顯示,較低溫下的合成粉末,在燒結過程中,抑制了序化晶域的成長,相對地,以兩次�y燒合成的粉末,其1:2序化的晶域隨著燒結溫度及持溫時間的增加而顯著地成長,其原因是由於二次�y燒造成合成粉末具較高程度的1:2序化結構及良好的均質性,且當採用二次�y燒及1350˚C / 48小時的燒結條件時,燒結體的品質因子可獲得顯著地改善.此研究發現Ba(Zn1/3 Nb2/3)O3化合物的品質因子和序化晶域的大小; 1:2序化的程度及燒結體的相對理論密度有關.
另外, Ba1-xLax[Zn(1+x)/3Nb(2-x)/3]O3 (BLZN) 固溶體的介電及結構性質,亦被探討.其1:1序化的結構可以用隨機分佈的模型來解釋,當鑭元素取代進入結構時,其容忍因子降低,造成氧八面體的傾斜,鄰層間氧八面體的同相或反相傾斜造成共振頻率的溫度係數( )顯著變化.在氧八面體未傾斜成份區間t ≥ 1.01,其 隨著容忍因子下降呈線性上升.而在氧八面體反相傾斜的成份區間0.965 ≤ t < 1.01,其 快速下降,造成 由正值變為負值,進一步地,當容忍因子小於0.965,其同相傾斜造成 再次地緩慢的增加,因此, 可以由容忍因子的計算來預測之,而藉由鑭離子的添加,獲得 =0 ppm/˚C的組成.
另外,本研究進一步地探討CaZrO3 (CZ)添加所造成 Ca(Mg1/3Nb2/3)O3 (CMN) 化合物序化結構的變化,研究顯示,此(1-x)CMN-(x)CZ固溶體被氧八面體同相,異相傾斜及A位置陽離子偏移的出現而形成扭曲的1:2及1:1序化結構.同時,在序化結構的轉換及微波介電性質之間,具有明顯的相關性,當鋯離子取代CMN時,造成容忍因子的下降,而導致晶體結構的不穩定性,進一步造成品質因子的降低而介電常數的上升.此外,容忍因子下降造成 的上升,此乃由於氧八面體傾斜角度的增加而造成的.
本研究中,亦探討另一陽離子欠缺型鈣鈦礦結構的陶瓷系統A5B4O15 (A = Ba+2, Sr+2, Mg+2, Ca+2; B = Nb+5),其具有優異的微波介電特性,探討當以�k取代鋇時,其結構和微波介電特性的變化,在富含Ba離子的組成,拉曼光譜的分裂,顯示在固溶體系統中具不對稱晶體結構,且在富含Sr離子的組成,由X光繞射圖的Rietveld分析發現其對稱性由 轉換成 ,在固溶體中,富含Ba離子的成份區間內,介電常數和 隨著�k離子的增加而增加,但是在富含Sr離子的成份區間中呈現相反的趨勢.原因乃是其晶體結構對稱性的轉換,造成介電常數及 的變化,且變化的行為和NbO6八面體振動及晶格常數c/a比的變化,有顯著的相關性. Mg取代Ba的固溶體系統(Ba1-xMgx)5Nb4O15, 其微波介電性質被探討,研究發現 MgNb2O6第二相的出現,造成 下降,因而可獲得近乎為零的 之微波介電陶瓷的成份組成.

The A(B'1/3B" 2/3)O3-type (A= Ba+2, Ca+2; B' = Mg+2 , Zn+2; B" = Nb+5, Ta+5) complex perovskite compound shows ordering structure in B-site cations and exhibits a very low dielectric loss at microwave frequency. The high cost of Ta-based complex perovskite ceramics makes it less cost-effective for many applications. Therefore, this study aims to investigate the structure-microwave dielectric property relations in the Nb2O5-based complex perovskite ceramics.
Barium zinc niobate, Ba(Zn1/3Nb2/3)O3, complex perovskite has been reported to have excellent microwave dielectric properties with close relation of its ordered structure and quality factor. This study investigates the effect of calcination condition on the evolution of ordered structure and on quality factor with Raman spectroscopy, x-ray diffractometry, and transmission electron microscopy. The present results reveal that the low temperature of synthesis causes the inhibition of ordered domain growth during sintering. In contrast, the 1:2 ordered domain in double-calcined Ba(Zn1/3Nb2/3)O3 powder grows significantly with an increase of sintering temperature and soaking time. It is attributed that the relatively higher degree of 1:2 ordering and better homogeneity are achieved by double calcinations. The quality factor is highly promoted by using double-calcined Ba(Zn1/3Nb2/3)O3 powder and sintered at 1350˚C / 48 h. Certainly, the quality factor closely relates to the size of ordered domain, degree of 1:2 ordering and relative density in Ba(Zn1/3Nb2/3)O3ceramic.
Furthermore, the dielectric properties and microstructural characteristics in solid solutions of Ba1-xLax[Zn(1+x)/3Nb(2-x)/3]O3 (BLZN) are investigated by measuring and observing these properties respectively. The 1:1 ordered structure of BLZN is explained by the random-site model for the distribution of B-site cations. The decrease in the tolerance factor (t) by lanthanum substitution causes the tilting of oxygen octahedra. It appears that the onset of antiphase and inphase tilting causes the variation in the temperature coefficient of resonant frequency. In the untilted region where t ≥ 1.01, the TCF shows a linear increase with decreasing tolerance factor. The region of antiphase tilting where 0.965 ≤ t < 1.01 causes the rapid decrease in TCF , including the reverse sign. The TCF slowly increases where t < 0.965, which is due to the presence of inphase tilting of oxygen octahedra. The is predicted by using the tolerance factor, and the near zero of TCF is obtained with lanthanum substitution in the solid solution of the BLZN system.
Moreover, this study investigates the effect of CaZrO3 (CZ) substitution on the evolution of ordered structure in a Ca(Mg1/3Nb2/3)O3 (CMN) system. It indicates that a (1-x)CMN-(x)CZ solid solution has the 1:2 and 1:1 ordered structure distorted by the antiphase, the inphase tilting of oxygen octahedra and the antiparallel shift of A-site cation. A distinct correlation is noted between the transition of the ordered structure and microwave dielectric properties. The decrease in the tolerance factor by zirconium substitution causes the large anharmonicity, which decreases the quality factor and increases the relative permittivity. Furthermore, the reduction in the tolerance factor causes the increase in because of an increase in tilting amplitude.
The A5B4O15 (A = Ba+2, Sr+2, Mg+2, Ca+2; B = Nb+5) cation-deficient perovskites ceramics also have good microwave dielectric properties. The effects of strontium substitution for barium on the structure and microwave dielectric properties of Ba5Nb4O15 compounds are investigated. The symmetric stretching vibration of Ba-rich compounds splits into two narrow Raman-active modes and indicates the existence of a strong anharmonic lattice in (Ba1-xSrx)5Nb4O15 system. Nevertheless, the symmetry changes from P-3m1 to P-3c1 for the Sr-rich compounds by the Rietveld analysis of XRD patterns. The relative permittivity and temperature coefficient of resonant frequency increases linearly with an increase of strontium content in Ba-rich compounds, but decreases in Sr-rich compounds. The transition of symmetry influences the variation of TCF and K. The behavior of TCF and K is correlated to the variation of symmetric stretching vibrations of NbO6 octahedra and c/a ratio of lattice parameter in the unit cell.
Furthermore, the microwave dielectric properties of (Ba1-xMgx)5Nb4O15 ceramics are also investigated. The formation of second phase MgNb2O6 causes the TCF decrease, including reverse sign and near zero of TCF is obtained.

Chinese Abstract……………………………………………………………………I
English Abstract………………………………………………………………… IV
Thanks……………………………………………………………………………..VII
Contents……………………………………………………………………………VIII
Figure Captions……………………………………………………………………XII
Table Captions……………………………………………………………………XXII
Chapter 1 General Introduction
1-1Application of Microwave Dielectric Ceramics…………………………… 1
1-2Microwave Dielectric Characteristics……………………………………… 5
1-3Microwave Dielectric Ceramics……………………………………………. 11
1-4Structural and Microwave Dielectric Properties Relations………………….16
Chapter 2 Theory
2-1 Structure of Complex Perovskites A(B’1/3B”2/3)O3 (A = Ba, Ca; B’ = Mg, Zn; B” = Ta, Nb) System……………………………………………………….19
2-2 Ordering Phase Transition in Complex Perovskite…………………………26
2-3 Tilting of Oxygen Octahedra in Complex Perovskite………………………29
2-4 Tolerance Factor in Perovskite Ceramics…………………………………...40
2-5 Two Types of Domain Boundary in Complex Perovskite…………………..41
2-6 Structure -Quality Factor (Q) Relations…………………………………….46
2-7 Structure -Temperature Coefficient of Resonant Frequency ( ) Relations.49
2-8 Structure –Relative Permittivity (εr) Relations…………………………… 54
2-9 Raman Spectrum in Complex Perovskite………………………………….57
Chapter 3 Structure -Quality Factor (Q) Relation in Barium Zinc Niobate
3-1 Introduction………………………………………………………………..62
3-2 Experimental Procedure…………………………………………………...63
3-3 Results……………………………………………………………………..66
3-4 Discussion…………………………………………………………………94
3-5 Conclusion…………………………………………………………………95
Chapter 4 Structure - Temperature Coefficient of Resonant Frequency (τf) Relation in Barium Lanthanum Zinc Niobate
4-1 Introduction………………………………………………………………..96
4-2 Experimental Procedure…………………………………………………...101
4-3 Results…………………………………………………………………….104
4-4 Discussion…………………………………………………………………121
4-5 Conclusion…………………………………………………………………127
Chapter 5 Structure – Microwave Dielectric Property Relations in Calcium Magnesium Niobate – CaZrO3
5-1 Introduction………………………………………………………………..128
5-2 Experimental Procedure………………………………………………….. 129
5-3 Results……………………………………………………………………..130
5-4 Discussion…………………………………………………………………155
5-5 Conclusion…………………………………………………………………162
Chapter 6 Structure –Relative Permittivity (εr) Relations in Barium Strontium Niobate
6-1 Introduction………………………………………………………………..163
6-2 Experimental Procedure………………………………………………….. 167
6-3 Results……………………………………………………………………. 167
6-4 Discussion…………………………………………………………………191
6-5 Conclusion…………………………………………………………………197
Chapter 7 Microstructure and Microwave Dielectric Property Relations in Barium Magnesium Niobate
7-1 Introduction…………………………………………………………… …198
7-2 Experimental Procedure………………………………………………… .198
7-3 Results and Discussion……………………………………………………199
7-4 Conclusion………………………………………………………………...209
Chapter 8 Summary……………………………………………………………210
References……………………………………………………………………… 213
Paper List………………………………………………………………………..225
Resume………………………………………………………………………….227

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