本論文主要使用sol-gel製程與磁控濺鍍系統來製備不同型態的多鐵性材料，其中包括塊材樣品與薄膜樣品，分別表示如下(i)單相多鐵性BiFeO3 (BFO)；(ii) 多鐵性複合塊材(1-x) BFO+(x) Ni0.5Zn0.5Fe2O4 (NZFO)；(iii)多鐵性多晶複合薄膜BFO+NZFO / LaNiO3 (LNO)/ Si；(iv)多鐵性磊晶複合薄膜BFO+NZFO / LNO / (001) SrTiO3 (STO)。
單相多鐵性BFO的樣品使用sol-gel法製備粉末，並在溫度400 ~ 700˚C燒結合成。這些不同溫度燒結的樣品中，低溫(400˚C、500˚C)跟高溫(600˚C、700˚C) 燒結的樣品在介電響應與磁性質上都表現出不一樣的結果。雖然樣品在XRD繞射圖中沒有發現其它二次相，但是藉由樣品在磁性上呈現交換偏置以及TEM觀察，可以證明有磁性相Fe3O4的存在。兩組樣品介電響應的巨大差異可歸咎於晶界的導電度，低溫樣品晶粒表面析出的Fe3O4薄層大幅提升了晶界的導電度，而高溫樣品雖然晶粒大5~10倍之多，但其晶界對介電響應的影響更為顯著。多鐵性複合塊材(1-x)BFO+(x)NZFO亦使用sol-gel法製備粉末，並在600˚C下燒結。從樣品的結構上分析，可以知道兩者經過混合燒結後，不會生成二次相。為研究BFO/NZFO界面反應、交換作用等相關問題，亦在複合材料中加入玻璃相之B2O3。微結構及相分析顯示，加入B2O3後兩相材料依然可以維持原來的結構。磁性分析顯示，沒有加入B2O3的複合材料其矯頑力(HC)隨溫度變化有異常表現，而M-H曲線亦出現交換偏置現象。加入B2O3的複合材料既沒有出現HC異常也沒有出現交換偏置等現象。
多鐵性多晶複合薄膜BFO+ NZFO利用雙靶共濺鍍的方式，分別沉積在Si基板與LNO / Si上，LNO為底電極與緩衝層。成長在LNO/Si上的複合薄膜，其結構特徵為細小的NZFO顆粒鑲嵌在大顆粒BFO中，也就是典型的0-3 type的對接方式。磁性測量發現複合薄膜呈現出明顯的交換偏置，在2 K時約為37 Oe，室溫則下降至11 Oe。此交換偏置的出現亦證實BFO/NZFO界面確實無擴散或化學反應。透過XRD繞射圖中d-spacing的移動以及HC隨溫度變化行為可發現，BFO與NZFO的顆粒都存在殘留應變，此殘留應變使得樣品在沒有施加直流偏壓場時也具有很大的磁電係數。而在共振頻率10 kHz以及外加偏壓場6.5 kOe時，磁電係數達到最大值 869 mV·Oe-1·cm-1。
多鐵性磊晶複合薄膜BFO+ NZFO一樣利用雙靶共濺鍍的方式在STO (001)基板上成長，並透過1D與2D的XRD證實了薄膜間的磊晶關係。在STO基板上方亦鍍有一層磊晶LNO作為量測磁電係數的底電極，此層LNO是由垂直於基板的奈米柱構成，這樣的微結構將有效緩解基板對應力傳遞的鉗制效應。由於LNO的晶格常數比BFO跟NZFO來得小，因此要在LNO上成長磊晶薄膜一定會產生明顯的晶格變形，高精度XRD確實觀察到這一現象。橫截面TEM影像圖顯示BFO與LNO的對應晶面彼此對齊，但是NZFO因為與LNO晶格尺寸相差太大，導致對應晶面之間有7.5˚夾角。因為異質磊晶成長產生更大應變，使得磊晶複合薄膜在沒有直流偏壓磁場時有更大的磁電電壓係數，其值在8 kHz時達911 mV·Oe-1·cm-1。

Multiferroic BiFeO3 (BFO) and its composites with Ni0.5Zn0.5Fe2O4 (NZFO) were synthesized by the sol-gel and dual-target RF magnetron co-sputterring methods. Different forms of composites were prepared, including sintered polycrystalline bulks of BFO+NZFO, polycrystalline thin films of BFO+NZFO/LaNiO3 (LNO)/Si, and epitaxial thin films of BFO+NZFO/LNO/(001) SrTiO3 (STO). BFO samples sintered at 400~500 C showed a single phase in XRD, but a Fe3O4 coating at grain surface was revealed by TEM as well as the occurrence of an exchange bias. So, the samples exhibited very different dielectric and magnetic behaviors from the samples sintered at 600~700 C. Polycrystalline composite films grown on LNO buffered Si substrates showed a grain epitaxy relationship between the BFO and LNO grains, resulting in some residual strain in the films. This led to a large magnetoelectric voltage coefficient at zero magnetic bias. The composite films grown on LNO buffered (001) STO substrates were epitaxial as confirmed by both XRD and TEM. The LNO buffer, which was sputtered epitaxially on STO as the bottom electrode, was composed of nanocolumns vertical to the substrate. Such a nanostructure is desired because it minimizes the “substrate clamp” problem that limits the applications of this type of composite films. The tetragonal distortion in both NZFO and BFO was apparent due to the compressive in-plane strain imposed by the epitaxial growth of larger NZFO and BFO lattices on smaller LNO lattice. The heteroepitaxial growth resulted in an even larger strain in the obtained composite films and hence, a larger zero-bias magnetoelectric voltage coefficient was achieved, which reached 911 mVcm-1Oe-1 at the frequency of 8 kHz.

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