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1、安徽大学 硕士学位论文 稀土氧化纳米管阵列制备及性能研究 姓名：刘桂林 申请学位级别：硕士 专业：物理化学 指导教师：袁孝友 2010-05 摘 要 I 摘摘 要要 制备纳米阵列结构材料，己成为当前纳米材料领域的研究热点。本论文以多 孔阳极氧化铝（AAM）为模板，结合减压抽滤法在 AAM 模板纳米孔道中构筑 一元、二元、三元稀土氧化物纳米管阵列，并对其各种性能进行了研究。其主要 研究内容如下： 1以 0.3M 草酸溶液为电解质溶液，采用直流电二次阳极氧化法制备纳米 阵列结构多孔阳极氧化铝（AAM）模板。系统地讨论了制备纳米阵列结构 AAM 模板的理论问题及影响因素。 2利用减压抽滤法，在 AA
2、M 模板孔道中构筑 Dy2O3纳米管阵列。以热重 分析仪（TGA）研究了前驱体的分解温度；利用场发射扫描电镜（SEM） 、透射 电子显微镜 （TEM） 、 x-射线衍射 （XRD） 、 能谱 （EDS） 、选区电子衍射 （SAED） 、 荧光分光光度计和振动样品磁强计（VSM）对 Dy2O3纳米管形貌、结构、化学 组成和性能进行表征。EDS 分析结果表明，Dy2O3纳米管的原子百分比 Dy:O 约 为 18.75:81.25，质量百分比 Dy:O 约为 97.78:2.22；荧光光谱分析表明，用波长 为 288nm 的光激发 Dy2O3纳米管，在 587nm 处有荧光发射峰；磁性测试结果表 明
3、， 室温时 Dy2O3纳米管阵列具有垂直各向异性，且易磁化方向是平行于纳米管 阵列方向。 3 采用减压抽滤 AAM 模板法组装了 DyCoxOy纳米管阵列。利用热重分析 仪（TGA）研究前驱体的分解温度；用 SEM、TEM 对所得样品的形貌进行表征； 纳米管的晶相结构利用 SAED 和 XRD 来表征；振动样品磁强计（VSM）用以测 试 DyCoxOy纳米管的磁性。结果表明，DyCoxOy纳米管为非晶态结构，每根纳 米管都是均匀、连续的，管与管之间相互平行；磁性测试结果表明，室温下 DyCoxOy纳米管阵列具备软磁体特征，易磁化方向是平行于纳米管阵列方向。 4以AAM为模板，结合减压抽滤法制备
4、了DyCoxZnyOz纳米管阵列。分别用 XRD、SEM、TEM、SAED和EDS对DyCoxZnyOz纳米管的形貌和晶相结构进行表 征。结果表明，DyCoxZnyOz纳米管阵列为非晶态结构，纳米管元素组成的原子 百分比Dy:Co:Zn:O约为4.86:1.67:1.70:91.77。利用振动样品磁强计（VSM）对纳 米管的磁性进行了研究。研究结果表明，DyCoxZnyOz纳米管阵列易磁化方向为 安徽大学硕士学位论文 稀土氧化物纳米管阵列制备及性能研究 II 平行于纳米管阵列方向。DyCoxZnyOz纳米管阵列具备软磁体特征。 5利用AAM模板的纳米孔道，在减压抽滤作用下制备出大面积，形状、尺
5、 寸均匀一致的SmNixOy纳米管阵列。 纳米管的形貌、 晶相结构和元素组成由SEM、 TEM、SAED、XRD和EDS来表征；SmNixOy纳米管阵列的荧光性能和磁性能分 别利用荧光分光光度计和振动样品磁强计来分析。SAED和XRD测试结果表明， SmNixOy纳米管为非晶态结构；EDS分析表明，SmNixOy纳米管中Sm、Ni和O元 素 的 原 子 百 分 比 Sm:Ni:O 约 为 5.85:1.62:92.53 ， 质 量 百 分 比 Sm:Ni:O 约 为 34.83:7.33:57.82；荧光光谱表明，用335nm 的光激发纳米管，在383nm处有较强 的荧光发射峰；VSM测试表明
6、，SmNixOy纳米管阵列具有垂直各向异性，易磁化 方向为平行于纳米管轴方向。 关键词关键词: AAM模板；减压抽滤法；纳米管阵列；荧光性能；磁性能 Abstract III Abstract Fbrication of nanostructure materials have become an hot topic in the field of nanomaterials during the recent years. In this paper, we employed porous anodic alumina membrane(AAM) as template with filte
7、ring at subatmospheric to fabricate a series of rare earth oxide nanotube arrays in the AAM template. The main research contents are as follows: 1. The AAM template has been fabricated via two-step anodization with direct current in 0.3 M oxalic solution. The theoretical and influencing about the na
8、no-array structure of AAM template are discussed. 2. The Dy2O3 nanotube arrays have been synthesized in the AAM template by filtering at subatmospheric. The decomposition temperature of the precursor has been studied by thermal gravimetric analysis (TGA).The morphology, structure, composition, fluor
9、escence and magnetism of the nanotubes have been investigated by using scanning electron microscopy (SEM)、 transmission electron microscopy (TEM), x-ray diffraction (XRD), energy dispersive spectra (EDS), selected area electron diffraction (SAED), fluoroscope and vibrating sample magnetometer (VSM),
10、 respectively. The result of EDS showed that the ratio of atomic percentage of Dy : O for Dy2O3 nanotube equals to 18.75 : 81.25, and the ratio of mass percentage of Dy : O for Dy2O3 nanotube is 97.78 : 2.22. Fluorescence spectrum indicated that there is a fluorescence emission peak for Dy2O3 nanotu
11、bes at 587nm with 288nm light excited. The result of VSM showed that there is perpendicular anisotropy for Dy2O3 nanotube arrays at room temperature, and the easy magnetization direction is parallel to the direction of nanotube axis. 3. The DyCoxOy nanotube arrays have been assembled in the pores of
12、 AAM template by the method of filtering at subatmospheric. The decomposition temperature of the precursor has been studied by TGA. The morphology of resulting samples has been characterized by SEM and TEM. The structure of the nanotubes has been characterized by SAED and XRD. The magnetism of DyCox
13、Oy nanotube arrays 安徽大学硕士学位论文 稀土氧化物纳米管阵列制备及性能研究 IV has been studied by VSM. The results showed that the DyCoxOy nanotubes are amorphous, and the nanotubes are homogeneous, continuous and parallel from each other. The magnetization curve indicated that DyCoxOy nanotube arrays exhibits soft magnetic c
14、haracteristics, and the easy magnetization direction is parallel to the direction of nanotube axis at room temperature. 4. DyCoxZnyOz nanotube arrays have been fabricated in AAM by filtering at subatmospheric. The morphology and the crystal structure of DyCoxZnyOz nanotubes have been characterized b
15、y SEM、TEM、XRD、SAED and EDS, respectively. The results indicated that the DyCoxZnyOz nanotubes are amorphous, and the ratio of atomic percentage of Dy:Co:Zn:O is 4.86:1.67:1.70:91.77. The hysteresis loops characterized by VSM indicated that the easily magnetized direction of DyCoxZnyOz is parallel to
16、 the nanotube arrays and that there is magnetic anisotropy as a result of the shape anisotropy. DyCoxZnyOz nanotube arrays exhibited soft magnetic characteristics. 5. SmNixOy nanotube arrays have been synthesized by the technique of filtering at subatmospheric assisted with AAM template. The morphology and the crystal structure of SmNixOy nanotubes are characterized by SEM、TEM、XRD、SAED and EDS, respectively. SAED and XRD indicated that the SmNixOy nanotu
