稀土氧化物纳米管阵列制备及性能研究
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摘要
制备纳米阵列结构材料,已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AAM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；利用扫描电子显微镜(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,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铁特征,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,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。
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 (AAM) as template with filtering 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 nano-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, fluorescence 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), 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 nanotubes 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 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 DyCoxOy nanotube arrays 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 characteristics, 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 by 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 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 nanotubes are amorphous in structure. EDS showed that each SmNixOy nanotube contains three elements Sm, Ni and O, the ratio of atomic percentage of Sm:Ni:O is 5.85:1.62:92.53, and the ratio of mass percentage of Sm:Ni:O is 34.83:7.33:57.82, and there is a strong fluorescence emission peak for SmNixOy nanotubes at 383nm with 335nm light excited. VSM indicated that SmNixOy nanotube arrays with perpendicular anisotropy at room temperature, and the easy magnetization direction is parallel to the nanotube arrays.
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AAM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；利用扫描电子显微镜(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,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铁特征,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,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。
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 (AAM) as template with filtering 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 nano-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, fluorescence 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), 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 nanotubes 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 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 DyCoxOy nanotube arrays 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 characteristics, 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 by 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 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 nanotubes are amorphous in structure. EDS showed that each SmNixOy nanotube contains three elements Sm, Ni and O, the ratio of atomic percentage of Sm:Ni:O is 5.85:1.62:92.53, and the ratio of mass percentage of Sm:Ni:O is 34.83:7.33:57.82, and there is a strong fluorescence emission peak for SmNixOy nanotubes at 383nm with 335nm light excited. VSM indicated that SmNixOy nanotube arrays with perpendicular anisotropy at room temperature, and the easy magnetization direction is parallel to the nanotube arrays.
引文
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