纯金属及合金磁性纳米线的制备及微结构研究
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摘要
随着电子信息科学与技术的发展，一维纳米材料因具有许多独特的光学、电学、磁学、化学等方面的性能，而成为近些年来纳米材料领域的研究热点之一。本文利用多孔阳极氧化铝为模板，通过直流电化学沉积方法，在多孔阳极氧化铝模板中获得了Pt、Fe、Co Fe_7Co_3、Fe_3Co_7及Sm-Co合金纳米线。利用X射线衍射仪（XRD）、扫描电子显微镜（SEM）、振动样品磁强计（VSM）对纳米线阵列的形貌、晶体结构和磁性进行了研究。并且研究了热处理对其结构和磁性的影响。具体工作如下：
1.采用两步阳极氧化法，分别在硫酸、草酸和磷酸电解液中制备了不同孔径的阳极氧化铝模板，并借助扫描电子显微镜（SEM）观察了膜的微观形貌，研究了电压、电解液种类等对膜的影响，最终获得了制备多孔氧化铝模板的最佳工艺条件，并对模板的形成机理进行了讨论。
2.由FE—SEM的观察可知：所制备的各种成分的纳米线均具有良好的线性结构，其线壁光滑、线径一致，具有大的长径比，纳米线直径与模板孔径相当。Pt纳米线的直流电沉积模板法制备少见文献报道。我们首次利用恒电压沉积法，以氧化铝膜为模板制备了Pt纳米线阵列。Pt原子是在模板孔洞的导向作用下沿（111）方向择优生长，并具有多晶结构。Fe、Co、Fe_3Co_7及Fe_7Co_3纳米线阵列都表现出明显的磁各向异性，易磁化方向是纳米线的长轴方向。这主要起源于纳米线的形状各向异性。
3.在AAO模板中，直流沉积工艺制备了Sm-Co合金纳米线阵列。XRD分析则表明该纳米线为非晶态结构，热处理后有SmCo_5与Co相析出。由TEM的观察显示，该纳米线同样具有良好的线性结构，线径约为40 nm。能谱分析仪（EDS）显示：稀土Sm在过渡族元素Co的诱导下，在水溶液中发生共沉积。
As electronic information science and technology development, one-dimensionalnanometerials have attracted increasing attention due to their novel optical, electronic, magneticand chemical properties. In this work, Pt, Fe, Co and Fe-Co, Sm-Co alloy nanowires wereformed in the pores of porous anodic aluminum oxide template (AAO) by dc electrochemicaldeposition. The morphology, structure and magnetic properties of the nanowires were studied byfield emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD) and vibratingsample magnetometer (VSM). And the influence of heat treatment on the structure and magneticproperties of the Fe-Co, Sm-Co alloy nanowires were also studied. This thesis presents thefollowing work:
1. AAO templates with different pores were prepared by two-step anodization method insulphuric acid, oxalic acid and phosphoric acid respectively. The morphology of AAO wasinvestigated by field emission scanning electron microscope (FE-SEM). The affecting factorsinvolved in the templates were concluded from votage, the kind of electrolytes and reaming time.At last, the suitable processing conditions have been obtained to prepare high quality AAOtemplates and the formation mechanism of AAO was also discussed.
2. The nanowire arrays were observed by FE-SEM.The Photos showed that the nanowirearrays had a good linear structure, the same diameters, large aspect ratio and the diameter of thenanowires is equal to the pore size of the template. Direct voltage electrodeposion was appliedfor the first time to fabiricate Pt nanowire arrays within the pores of AAO templates. The XRDresults showed Pt nanowires have fcc polycrystalline structure with (111) preferred orientation.Fe, Co, Fe_3Co_7 and Fe_7Co_3 alloy nanowire arrays show clearly magnetic anisotropy, easymagnetization direction is along nanowires’long axis direction. This is mainly due to shapeanisotropy.
3. The ordered Sm-Co alloy nanowires were electrodeposited in the AAO templates by dc electrochemical deposition. The wires Proved to be amorphous structure by the XRD technology.While after heat treatment, they would be turned into SmCo_5 and Co nanowires. The TEMobservations indicated that the Sm-Co alloy nanowires had the same good linear structure, thediameter of the wires were about 40 nm. The Energy Dispersive Spectroscopy (EDS) analysisdisPlayed: The rare earth element Sm was induced by the transitional metal Co, and theyco-deposited from the aqueous solution together.
1.采用两步阳极氧化法，分别在硫酸、草酸和磷酸电解液中制备了不同孔径的阳极氧化铝模板，并借助扫描电子显微镜（SEM）观察了膜的微观形貌，研究了电压、电解液种类等对膜的影响，最终获得了制备多孔氧化铝模板的最佳工艺条件，并对模板的形成机理进行了讨论。
2.由FE—SEM的观察可知：所制备的各种成分的纳米线均具有良好的线性结构，其线壁光滑、线径一致，具有大的长径比，纳米线直径与模板孔径相当。Pt纳米线的直流电沉积模板法制备少见文献报道。我们首次利用恒电压沉积法，以氧化铝膜为模板制备了Pt纳米线阵列。Pt原子是在模板孔洞的导向作用下沿（111）方向择优生长，并具有多晶结构。Fe、Co、Fe_3Co_7及Fe_7Co_3纳米线阵列都表现出明显的磁各向异性，易磁化方向是纳米线的长轴方向。这主要起源于纳米线的形状各向异性。
3.在AAO模板中，直流沉积工艺制备了Sm-Co合金纳米线阵列。XRD分析则表明该纳米线为非晶态结构，热处理后有SmCo_5与Co相析出。由TEM的观察显示，该纳米线同样具有良好的线性结构，线径约为40 nm。能谱分析仪（EDS）显示：稀土Sm在过渡族元素Co的诱导下，在水溶液中发生共沉积。
As electronic information science and technology development, one-dimensionalnanometerials have attracted increasing attention due to their novel optical, electronic, magneticand chemical properties. In this work, Pt, Fe, Co and Fe-Co, Sm-Co alloy nanowires wereformed in the pores of porous anodic aluminum oxide template (AAO) by dc electrochemicaldeposition. The morphology, structure and magnetic properties of the nanowires were studied byfield emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD) and vibratingsample magnetometer (VSM). And the influence of heat treatment on the structure and magneticproperties of the Fe-Co, Sm-Co alloy nanowires were also studied. This thesis presents thefollowing work:
1. AAO templates with different pores were prepared by two-step anodization method insulphuric acid, oxalic acid and phosphoric acid respectively. The morphology of AAO wasinvestigated by field emission scanning electron microscope (FE-SEM). The affecting factorsinvolved in the templates were concluded from votage, the kind of electrolytes and reaming time.At last, the suitable processing conditions have been obtained to prepare high quality AAOtemplates and the formation mechanism of AAO was also discussed.
2. The nanowire arrays were observed by FE-SEM.The Photos showed that the nanowirearrays had a good linear structure, the same diameters, large aspect ratio and the diameter of thenanowires is equal to the pore size of the template. Direct voltage electrodeposion was appliedfor the first time to fabiricate Pt nanowire arrays within the pores of AAO templates. The XRDresults showed Pt nanowires have fcc polycrystalline structure with (111) preferred orientation.Fe, Co, Fe_3Co_7 and Fe_7Co_3 alloy nanowire arrays show clearly magnetic anisotropy, easymagnetization direction is along nanowires’long axis direction. This is mainly due to shapeanisotropy.
3. The ordered Sm-Co alloy nanowires were electrodeposited in the AAO templates by dc electrochemical deposition. The wires Proved to be amorphous structure by the XRD technology.While after heat treatment, they would be turned into SmCo_5 and Co nanowires. The TEMobservations indicated that the Sm-Co alloy nanowires had the same good linear structure, thediameter of the wires were about 40 nm. The Energy Dispersive Spectroscopy (EDS) analysisdisPlayed: The rare earth element Sm was induced by the transitional metal Co, and theyco-deposited from the aqueous solution together.
引文
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