臺灣博碩士論文加值系統

本研究主要係利用一維電導模型(one-dimensional barrier model)，模擬經由固態反應法(solid state reaction)製作出的BiFeO3 (BFO)、(1-x)BiFeO3-(x)BaTiO3 (BFO-BT)以及(Bi1-xBax)(Fe1-xTix)O3 [BFO-(Ba,Ti)]等陶瓷，在溫度與頻率的相依下，電導與介電實數的行為並且與實驗結果相比較。BFO陶瓷在one-dimension barrier model分析中，顯示出其電導實數的轉折點溫度範圍約在600-700 K，此溫度區間正好與介電極大值的溫度非常相近，可能受反鐵磁轉變成順磁結構所影響。而BFO-BT與BFO-(Ba,Ti)陶瓷的電導也隨著其摻雜量的增加，電導實數的轉折點溫度愈往低溫移動。(Ba,Ti)含量的增加同時提升了材料中barriers (B)值，BFO-BT與BFO-(Ba,Ti)陶瓷的barrier (B=11000 K)值遠高於BFO (B=8200 K)。而barrier的提升可以降低電子躍遷至其它晶格與晶域之間的機率，有效地改善BFO陶瓷在高溫下電導過大的情形，此一結果也與介電損耗相呼應。BFO陶瓷的結構相變過程為rhombohedral (R)-orthorhombic (O)-cubic (C)，相變溫度分別為820 ℃與850 ℃；BFO-BT與BFO-(Ba,Ti)陶瓷的結構相變過程則直接為rhombohedral-cubic，相變溫度則隨著摻雜(Ba,Ti)之含量提高而下降。BFO陶瓷室溫下的晶格大小約為3.9699 Å。伴隨著(Ba,Ti)之含量增加，BFO-BT與BFO-(Ba,Ti) 陶瓷之晶格大小變化更為明顯。BFO、BFO-BT與BFO-(Ba,Ti) 陶瓷的晶軸極小值(αR)發生的溫度約為300-500 ℃，此溫度也與尼爾溫度(TN)發生範圍相近。BFO陶瓷於室溫下的介電常數約為33 (f = 1 MHz)，(Ba,Ti)的摻雜可以有效地提升介電常數至321 (BFO-30%BT)，並且能抑制高溫的介電色散現象。BFO、BFO-BT以及BFO-(Ba,Ti)陶瓷的介電常數隨著溫度升高皆有一明顯的介電極大值(Tm)，Tm發生的溫度範圍同時對應到晶軸極小值αR的產生，顯示出該現象與磁電效應有密切關係。此外，(Ba,Ti)的摻雜可以降低BFO陶瓷的介電損耗及提升介電性質，BFO-BT與BFO-(Ba,Ti)陶瓷的介電損耗皆低於0.1。磁性觀察上，BFO與BFO-BT陶瓷室溫下仍維持著反鐵磁的性質。BFO-5%(Ba,Ti)陶瓷呈現弱鐵磁的特性，BFO-10%(Ba,Ti)則因過高的燒結溫度，導致過多的Fe3+存在晶格內，導致磁滯曲線量測到氧化鐵的磁性行為。

A one-dimensional conductivity barrier model with intrinsic barrier B every lattice constant a and extrinsic barrier B+Δ is introduced to describe the dielectric response and conductivity as functions of temperature and frequency. Temperature- and frequency-dependent dielectric permittivity (ε′) and conductivity (σ′) have been studied on multiferroic BiFeO3 (BFO), (1-x)BiFeO3-(x)BaTiO3 (BFO-BT), and (Bi1-xBax)(Fe1-xTix)O3 [BFO-(Ba,Ti)] ceramics, which were synthesized by the solid state reaction method. A frequency-dependent dispersion of dielectric maximum appears in the lower temperature region. This phenomenon is likely activated by the antiferromagnetic (AFM)-paramagnetic (PM) transition. Good qualitative fits of dielectric permittivity and conductivity are obtained with the interior grain sizes d of 20-40 nm. BFO-BT and BFO-(Ba,Ti) ceramics show higher intrinsic barriers B about 11000 K than B=8200 K in BiFeO3. The phase transition of BFO is rhombohedral (R)-orthorhombic (O)-cubic (C) and the Curie temperature (Tc) is near 850 ℃. The structure transition sequence of BFO-BT and BFO-(Ba,Ti) ceramics is R to C upon heating. The Curie temperatures in BFO-BT and BFO-(Ba,Ti) ceramics shift toward lower temperatures due to the contents of (Ba,Ti). The lattice constant in BFO is about 3.9699 Å and increases with increasing the (Ba,Ti) contents. The local minima of R distortion angle (αR) in BFO, BFO-BT, and BFO-(Ba,Ti) occur in the region of 300-500 ℃, implying ionic displacements. The temperature regions also associate with Nèel temperature (TN). This anomaly is likely resulted from the antiferromagnetic (AFM)–paramagnetic (PM) transition and is responsible for the broad frequency-dependent dielectric maximum. The dielectric permittivities are about 33 in BFO and 321 in BFO-30%BT for 1 MHz at room temperature. The dielectric loss decreases as BT increases. The real part of conductivity in BFO shows a deviation from the linear relation near Tm and αR. The deviation temperature shifts to lower temperature with increasing BT contents. BFO and BFO-BT ceramics exhibit a similar antiferromagnetic (AFM) behavior. BFO-5%(Ba,Ti) shows the weak ferromagnetic behavior. The magnetic hysteresis loop of possible iron oxide in BFO-10%(Ba,Ti) was observed due to higher sintering temperature.

中文摘要 i
英文摘要 iii
誌謝 v
目錄 vii
圖目錄 x
表目錄 xiii
第一章　緒論 1
1.1 研究背景 1
1.2 研究方法 2
1.3 研究使用材料之特性 3
1.4 複鐵性材料歷史回顧 7
1.4.1　鐵酸鉍介紹 7
1.4.2　鐵酸鉍的相圖(phase diagram) 10
1.4.3　鐵酸鉍的電導與能隙 14
1.4.4　鐵酸鉍的鐵電特性 15
1.4.5　鐵酸鉍的介電特性 16
1.4.6　鐵酸鉍的磁性 17
1.5 鐵酸鉍相關文獻探討 18
第二章　實驗方法與理論計算 26
2.1　樣品製備 26
2.1.1　BiFeO3之調配與球磨 26
2.1.2　鍛燒(calcine) 29
2.1.3　高能球磨(high-energy ball milling) 30
2.1.4　造粒與成型 30
2.1.5　燒結(sinter) 31
2.1.6　(1-x)BiFeO3-(x)BaTiO3陶瓷製備 32
2.1.7　(Bi1-xBax)(Fe1-xTix)FeO3陶瓷製備 33
2.2　X-ray diffraction 結構量測 35
2.3　介電常數量測 37
2.3.1　介電陶瓷 37
2.3.2　介電特性 39
2.3.3　介電性質參數 42
2.4　磁性量測 45
2.5　One-dimensional barrier model 46
第三章　實驗結果與討論 58
3.1　結構相變 58
3.1.1　BiFeO3結構相變 58
3.1.2　(1-x)BiFeO3-(x)BaTiO3結構相變 56
3.1.3　(Bi1-xBax)(Fe1-xTix)FeO3結構相變 66
3.2　晶格常數分析 67
3.2.1　BiFeO3晶格常數 67
3.2.2　(1-x)BiFeO3-(x)BaTiO3晶格常數 69
3.2.3　(Bi1-xBax)(Fe1-xTix)FeO3晶格常數 71
3.3　介電常數分析 72
3.3.1　BiFeO3介電常數 72
3.3.2　(1-x)BiFeO3-(x)BaTiO3介電常數 74
3.3.3　(Bi1-xBax)(Fe1-xTix)FeO3介電常數 76
3.4 One-dimensional barrier model 77
3.5 磁性量測結果與分析 81
第四章　結論 83
參考文獻 86

圖目錄

圖1-1　複鐵性材料的鐵電性、鐵磁性、與鐵彈性相互關係示意圖 9
圖1-2　複鐵性材料的五種鐵性有序參數相互與衍生關係的示意圖 10
圖1-3 鐵酸鉍的相圖 11
圖1-4 鐵酸鉍薄膜之剩餘磁化率與雜相比例關係 11
圖1-5 鐵酸鉍之溫度與結構變化關係圖 14
圖1-6 鐵酸鉍單晶之電阻變化Arrhenius plot 15
圖1-7 鐵酸鉍單晶(上圖)與薄膜(下圖)之鐵電極化大小 16
圖1-8 鐵酸鉍單晶(左圖)與陶瓷(右圖)之溫度與介電圖 17
圖1-9 鐵酸鉍之(左圖)G型反鐵磁與(右圖)鐵原子磁矩示意圖 18
圖1-10 燒結溫度(a)600、(b)750、(c)880 ℃之鐵酸鉍陶瓷XRD圖 19
圖1-11 燒結溫度880 ℃之鐵酸鉍陶瓷電滯曲線與電流密度 20
圖1-12 燒結溫度880 ℃之鐵酸鉍陶瓷磁滯曲線 20
圖1-13 鐵酸鉍陶瓷之介電常數與介電損耗 22
圖1-14 BiFeO3-BaTiO3陶瓷之結構相圖 23
圖2-1 BiFeO3樣品製備流程圖 27
圖2-2 鍛燒前後BiFeO3粉末之XRD比較圖 30
圖2-3 燒結前後BiFeO3陶瓷之XRD比較圖 31
圖2-4 (1-x)BiFeO3-(x)BaTiO3陶瓷之XRD比較圖 33
圖2-5 (Bi1-xBax)(Fe1-xTix)FeO3陶瓷之XRD比較圖 34
圖2-6 (a)BFO、(b)BFO-5%(Ba,Ti)、(c)BFO-10%(Ba,Ti)、
(d)BFO-5%BT、(e)BFO-10%BT、(f)BFO-20%BT、
(g)BFO-30%BT之SEM比較圖 35
圖2-7 布拉格繞射示意圖 36
圖2-8 極化的產生機制 40
圖2-9 極化機制對頻率反應快慢 41
圖2-10 介電實驗下陶瓷樣品準備示意圖 45
圖2-11 VSM簡易構造示意圖 46
圖2-12 One-dimensional barrier model示意圖 47
圖3-1 BiFeO3 (110)晶格面之同步輻射XRD圖 59
圖3-2 0.95BiFeO3-0.05BaTO3 (110)晶格面之同步輻射XRD圖 61
圖3-3 0.9BiFeO3-0.1BaTO3 (110)晶格面之同步輻射XRD圖 63
圖3-4 0.8BiFeO3-0.2BaTO3 (110)晶格面之同步輻射XRD圖 64
圖3-5 0.7BiFeO3-0.3BaTO3 (110)晶格面之同步輻射XRD圖 65
圖3-6 BFO-BT之結構相圖 65
圖3-7 (Bi0.95Ba0.05)(Fe0.95Ti0.05)O3(110)晶格面之同步輻射XRD圖 66
圖3-8 (Bi0.9Ba0.1)(Fe0.9Ti0.1)O3(110)晶格面之同步輻射XRD圖 67
圖3-9 晶格常數與其對應晶格夾角隨溫度之變化 68
圖3-10 BFO-5~30%BT之晶格常數與晶軸夾角隨溫度變化圖 70
圖3-11 BFO-5~10%(Ba,Ti)之晶格常數與晶軸夾角隨溫度變化圖 71
圖3-12變溫變頻下BFO之介電常數與介電損耗圖 73
圖3-13變溫變頻下BFO-5~30%BT之介電常數與介電損耗圖 75
圖3-14變溫變頻下BFO-5~10%(Ba,Ti)之介電常數與介電損耗圖 76
圖3-15 One-dimensional barrier model模擬BFO之(a)介電常數與(b)電導
實部關係圖 78
圖3-16 One-dimensional barrier model模擬BFO-5%BT之(a)電導與(b)
介電常數實部關係圖 80
圖3-17 One-dimensional barrier model模擬BFO-10%BT之(a)電導與
(b)介電常數實部關係圖 80
圖3-18 One-dimensional barrier model模擬BFO-5%(Ba,Ti)之(a)電導與
(b)介電常數實部關係圖 81
圖3-19 One-dimensional barrier model模擬BFO-10%(Ba,Ti)之(a)電導與
(b)介電常數實部關係圖 81
圖3-20 BFO、BFO-BT與BFO-(Ba,Ti)之VSM量測圖 82

表目錄

表1-1　 氧化鉍的基本特性 4
表1-2　 氧化鐵的基本特性 4
表1-3　 碳酸鋇的基本特性 5
表1-4　 二氧化鈦的基本特性 5
表1-5　 鈦酸鋇的基本特性 6
表1-6　 不同原子的電子組態、價電子及氧化價數 6
表2-1　 七大晶系與32點群 38
表3-1　 BFO-BT晶格參數大小與其BT含量多寡之影響 69
表3-2　 測量頻率1 MHz下BFO-BT之室溫介電常數 75
表3-3　 BFO、BFO-BT以及BFO-(Ba,Ti)陶瓷之one-dimensional barrier model模擬參數 79

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