臺灣博碩士論文加值系統

本論文採用合金成分分成兩部分：一為Pr2(Fe1-yTiy)23B3（y = 0.018-0.048）、PrxFe82.2-yTiyB17.8-x（x = 11.8-5；y = 2.5-5.5）及Pr9Fe88.5-xTi2.5Bx（x= 7-15）；另一部份則以C置換B於Pr9Febal.CoxTiyB11-zCz（x = 0及10；y = 0-4；z = 0-11）合金。針對上述合金所製作之快淬薄帶探討其磁性、相變化及顯微結構，並瞭解添加元素（Ti、C及Co）在PrFeB合金薄帶之效應。實驗結果如下：
1. 適量的Ti元素置換Fe 於Pr2(Fe1-yTiy)23B3合金薄帶可抑制2:23:3及Fe3B相形成且有細化晶粒的效果。在Pr9Febal.Ti2.5Bz合金薄帶中，隨B含量的增加，?Fe相有隨之減少而硬磁2:14:1相增加趨勢。另一方面，微量C（0.5 at％）置換硼於Pr9Febal.B11-zCz合金薄帶不但形成Pr2Fe14(B,C)相且有細化晶粒的效果。且在較高Ti含量（4 at％）之Pr9Febal.Ti4B11-zCz合金薄帶系列中，因為有足夠Ti用以抑制2:23:3及Fe3B相及微量C （0.5 at％）置換B於Pr9Febal.Ti2.5B10.5C0.5合金薄帶形成Pr2Fe14(B,C)相及細化晶粒之作用，致使合金薄帶之磁性值顯著提升。此外，10 at％Co置換Fe於Pr9Febal.Co10Ti4B11合金薄帶會造成晶粒粗化，不但侷限了磁性提升的幅度並且使iHc值降低。唯有以微量C （0.5~2.5 at％）置換B 於Pr9Febal.Co10Ti4B11-zCz合金薄帶，藉由TiC相形成於晶界以阻礙晶粒成長而可獲得細晶粒且均勻顯微結構及本研究中之最佳磁性值。最佳磁性之薄帶成分為具?(Fe, Co)/Pr2(Fe, Co)14(B, C)雙相複合奈米晶顯微組織之Pr9Febal.Co10Ti4B10C1，其磁性質為Br = 10.0 kG、iHc = 10.5 kOe及(BH)max值高達20.2 MGOe且?= -0.092 %/oC及β = -0.504 %/oC。
2. 在Pr9Febal.Co10Ti4B11-zCz合金薄帶中，隨著C含量的增加，矯頑機制由磁區壁拴固型轉向反向磁區孕核成長型主導。就磁化行為而言，Pr9Febal.B11-zCz（C＝0～11 at％）合金薄帶之磁化翻轉皆由軟磁相主導。而Pr9Febal.Ti4B11-zCz（C≦0.5 at％）及Pr9Febal.Co10Ti4B11-zCz（C≦2.5 at％）合金薄帶則由硬磁相主導磁化翻轉。

The phase evolution, microstructures and magnetic properties of Pr2(Fe1-yTiy)23B3（y = 0.018-0.048）, PrxFe82.2-yTiyB17.8-x （x = 11.8-5；y = 2.5-5.5）and Pr9Fe88.5-xTi2.5Bx （x= 7-15）melt-spun ribbons have been investigated. Because Pr2Fe14C compound is isostructural with Pr2Fe14B, its magnetocrystalline anisotropy field is even larger than that of Pr2Fe14B, the effect of C substitution for B in Pr9Febal.CoxTiyB11-zCz （x = 0及10；y = 0-4；z = 0-11）nanocomposites were also studied. The major results are summarized as follows.
1. The appropriate substitution of Ti element for Fe in Pr2(Fe1-yTiy)23B3 ribbons can suppress the formation of metastable Pr2Fe23B3 and Fe3B phases and result in the presence of large amount of Pr2Fe14B and ?Fe phases with fine grain size. In Pr9Fe88.5-xTi2.5Bx nanocomposites, the volume fraction of Pr2Fe14B phase increases and ?Fe phase decreases with increasing the boron content, giving rise to the increment of iHc and the decrement of Br. On the other hand, for Pr9Febal.TixB11-yCy series ribbons, the addition of 4 at% Ti suppresses the formation of metastable Pr2Fe23B3 phase and ensures the existence of large amount of magnetically hard Pr2Fe14B phase in the ribbons. Besides, a slight C addition can not only form Pr2Fe14(B, C) phase but also refine the grain size, resulting in the improvement of magnetic properties. However, Co substitution for Fe in Pr9Febal.Co10Ti4B11 ribbon merely results in coarser grain size to limit the enhancement of magnetic properties, and decreases the coercivity slightly. Only in the C-containing Pr9Febal.Co10Ti4B11-yCy (1≦y≦2.5) alloy ribbons is beneficial in obtaining a much finer and more homogeneous microstructure due to the formation of TiC to impede grain growth. As a result, ?(Fe, Co)/Pr2(Fe, Co)14(B, C)-type nanocomposites with excellent magnetic properties of Br = 10.0 kG, iHc = 10.5 kOe, (BH)max = 20.2 MGOe and ?= -0.092 %/oC, β = -0.504 %/ oC could be obtained in Pr9Febal.Co10Ti4B10C1 ribbons.
2. In Pr9Febal.Co10Ti4B11-zCz ribbons, the coercivity mechanism varies from domain wall pinning to reverse domain nucleation with increasing carbon content. For magnetization behavior, the magnetization reversal of Pr9Febal.B11-zCz (C= 0~11 at％) ribbons is mainly dominated by soft phase. However, the magnetization reversal of Pr9Febal.Ti4B11-zCz (C≦0.5 at％) and Pr9Febal.Co10Ti4B11-zCz (C≦2.5 at％) ribbons are dominated by hard phase.

目錄
中文摘要……………………………………………………………........I
英文摘要…………………………………………………………….......II
誌謝……………………………………………………………............III
目錄……………………………………………………………..............IV
表目錄……………………………………………………………............V
圖目錄…………………………………………………………….........VI
第一章 緒論……………………………………………………………..1
1-1 前言……………………………………………………………..1
1-2 磁性材料分類簡介…………………………………………..…4
1-3 稀土永久磁石之發展簡介………...………………...…………7
1-4 RFeB合金之顯微結構簡介……………………………16
1-5 雙相奈米複合永磁材料……………………………….18
1-6 雙相奈米晶複合永磁材料的特徵……………………20
1-7 雙相納米複合永磁材料的製造方式之一…………..22
1-8 新型複合奈米晶之磁特性比較………………………26
1-9 R2Fe14C相關文獻……………………………………….34
1-10 研究動機與目的……………………………………………..37

第二章 理論基礎………………………………………………………39
2-1 磁滯曲線………………………………………………………39
2-2 材料磁性起源…………………………………………………41
2-3 磁性體分類……………………………………………………43
2-4 磁異向性………………………………………………………46
2-5 稀土磁石之矯頑機制簡介……………………………48
2-6 矯頑機制之基本理論-反向磁區孕核模型………….52
2-7 交換藕合作用………………………………………….58
2-8 R2Fe14B化合物間的居里溫度與交換作用……………65
2-9 析出物與晶粒的成長………………………………….67

第三章 實驗方法………………………………………………………68
3-1實驗流程.....................................................................................68
3-2 合金成分………………………………………………………69
3-3 奈米晶材料樣品之製備………………………………………70
3-4 樣品量測與分析………………………………………………74

第四章 Pr(Fe,Ti)B複合奈米晶之磁性、相變化及顯微結構……..…78
4-1 Ti置換Fe對Pr2Fe23B3奈米晶薄帶影響……………………..78
4-2 由Pr2Fe14B 至Pr2Fe23B3區域合金薄帶之磁性、相變化及顯微結構探討……………………………..……………………...88
4-3 硼含量的變化對Pr9Febal.Ti2.5Bz合金薄帶之磁性、相變化及顯微結構探討…………………………………………………...99

第五章 PrFe(B, C)型複合奈米晶之磁性、相變化及顯微結構…….108
5-1 C元素置換B對Pr9Febal.B11 (at％)合金薄帶磁性、相變化及顯微結構的影響……………………………………………...109
5-2 C元素置換B對Pr9Febal.Ti2.5B11 (at％)合金薄帶磁性、相變化及顯微結構的影響………………………………………...119
5-3 C元素置換B對Pr9Febal.Ti4B11 (at％)合金薄帶磁性、相變化及顯微結構的影響…………………………………………...130
5-4 C元素置換B對Pr9Febal.Co10Ti4B11 (at％)合金薄帶磁性、相變化及顯微結構的影響……………………………………...141
5-5 綜合討論……………………………………………………..157
5-6 可逆與不可逆磁化…………………………………………..164
5-7 矯頑機制……………………………………………………..180

第六章 綜合分析與討論………………………………………..……185

第七章 結論……………………………………………………..……192

參考文獻………………………………………………………………195

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