稀土—过渡金属氧化物纳米线阵列的制备及性能研究
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摘要
本文以有序多孔阳极氧化铝膜(AAO)为模板,用化学共沉积法,辅之负压抽滤技术,在AAO模板纳米孔道内制备出LaxZnyOz、LaxMnyOz、LaxFeyOz、 LaxCuyOz、CexFeyOz和TbxOy纳米线阵列。以扫描电镜(SEM)、透射电镜(TEM)、X-射线衍射仪(XRD)、能量散射光谱仪(EDS)表征了它们的形貌、结构及其化学组成。以振动样品磁强计(VSM)测定了LaxZnyOz、LaxMnyO2、LaxFeyOz、 LaxCuyOz、CexFeyOz、TbxOy纳米线阵列的磁性能。以荧光光谱仪(F--4500)研究了Tb, Eu, Sm掺杂浓度对LaxCuyOz、CexFeyOz纳米线阵列荧光强度的影响,探究了激发光波长和Eu, Sm掺杂浓度与TbxOy纳米线阵列荧光强度的对应关系。
主要研究结果如下：
1、本文制备的稀土-过渡金属氧化物及稀土氧化物纳米线均为非晶态结构。改变反应物浓度、反应时间、抽滤负压、热分解温度以及AAO模板纳米孔径等参数,可以对稀土-过渡金属氧化物纳米线形貌、化学组成及结构进行调控。
2、LaxZnyOz、LaxMnyOz、LaxFeyOz、LaxCuyOz、CexFeyOz纳米线阵列在外加磁场下,都具有磁各向异性。除LaxCuyOz外,它们的易磁化方向都是平行于纳米线阵列轴向且磁各向异性来自形状各向异性的贡献。TbxOy纳米线在外加磁场下,表现为顺磁性特征。
3、Tb, Eu, Sm掺杂浓度在2-30mo1%范围内,LaxCuyOz、CexFeyOz纳米线阵列的荧光强度与掺杂浓度相关。当Tb, Eu掺杂浓度为5mo1%或Sm掺杂浓度为30mo1%时,LaxCuyOz荧光强度最强。当Eu, Sm掺杂浓度分别为10mo1%或Tb掺杂浓度为5mo1%时,CexFeyOz荧光强度最强。Tb, Eu, Sm掺杂超过上述最佳掺杂浓度时,LaxCuyOz、CexFeyOz出现荧光猝灭现象。
4、TbxOy纳米线阵列荧光强度受激发光波长和Eu, Sm掺杂浓度共同影响。Eu, Sm掺杂浓度在2-20mol%范围内,当激发光波长分别为221nm,394nm, Eu掺杂浓度为2mol%时,Eu掺杂TbxOy纳米线阵列荧光强度最强。当激发光波长分别为221nm,405nm, Sm掺杂浓度分别为5mol%,20mol%时,Sm掺杂TbxOy纳米线阵列荧光强度最强。
In this thesis, LaxZnyOz、LaxMnyOz、LaxFeyOz、LaxCuyOz、CexFeyOz and TbxOy nanowire arrays have been fabricated in the anodic aluminum oxide (AAO) template with chemical deposition reaction via suction filteration at subatmospheric. The SEM、TEM、XRD and EDS were employed to characterize their crystal structure, morphology and chemical composition, respectively. The vibrating sample magnetometer (VSM) was used to study the magnetic performances of LaxZnyOz、 LaxMnyOz、LaxFeyOz、LaxCuyOz、CexFeyOz and TbxOy nanowire arrays, and the fluorescence spectrophotometer (F-4500) was employed to study the fluorescence intensity of LaxCuyOz、CexFeyOz、TbxOy nanowire arrays doped with Tb, Eu or Sm.
The mainly research results are as follow:
1. The above nanowire arrays are all amorphous in structure, and their structure, morphology and chemical composition could be adjusted by reactant concentration, reaction time, subatmospheric of suction filtration, thermal decomposition temperature and the pore size of AAO template.
2. There are obvious magnetic anisotropy of LaxZnyOz、LaxMnyOz、LaxFeyOz、 LaxCuyOz、CexFeyOz nanowire arrays with the applied magnetic field and their easy magnetized direction is parallel to the axis of nanowire except for LaxCuyOz, which is from the shape anistropy of nanowire arrays. The TbxOy nanowire array is paramagnetic with the applied magnetic field.
3. The fluorescence intensities of LaxCuyOz、CexFeyOz nanowire arrays are related with the doped Tb, Eu or Sm within2-30mol%. The results indicated that there is the strongest fluorescence for LaxCuyOz nanowire arrays, when the optimum doping concentration of Tb, Eu is5mol%and that of Sm is30mol%. When the optimum doping concentration of Eu or Sm is10mol%and Tb is5mol%, the fluorescence of CexFeyOz nanowire arrays is the strongest. The LaxCuyOz or CexFeyOz nanowire array is fluorescence quenching, when Eu or Sm is respectively over the optimum doping concentration.
4. The fluorescence intensity of TbxOy nanowire array is both influenced by the exciting light and the doping concentrations of Eu·or Sm. there are the strongest fluorescence peaks of TbxOy nanowire arrays, when the doping concentrations of Eu is2mol%, and the exciting light is respectively221nm,394nm. When the doping concentration of Sm is10mol%or20mol%, the exciting light is respectively221nm,405nm, there are the strongest fluorescence peaks of TbxOy nanowire array.
主要研究结果如下：
1、本文制备的稀土-过渡金属氧化物及稀土氧化物纳米线均为非晶态结构。改变反应物浓度、反应时间、抽滤负压、热分解温度以及AAO模板纳米孔径等参数,可以对稀土-过渡金属氧化物纳米线形貌、化学组成及结构进行调控。
2、LaxZnyOz、LaxMnyOz、LaxFeyOz、LaxCuyOz、CexFeyOz纳米线阵列在外加磁场下,都具有磁各向异性。除LaxCuyOz外,它们的易磁化方向都是平行于纳米线阵列轴向且磁各向异性来自形状各向异性的贡献。TbxOy纳米线在外加磁场下,表现为顺磁性特征。
3、Tb, Eu, Sm掺杂浓度在2-30mo1%范围内,LaxCuyOz、CexFeyOz纳米线阵列的荧光强度与掺杂浓度相关。当Tb, Eu掺杂浓度为5mo1%或Sm掺杂浓度为30mo1%时,LaxCuyOz荧光强度最强。当Eu, Sm掺杂浓度分别为10mo1%或Tb掺杂浓度为5mo1%时,CexFeyOz荧光强度最强。Tb, Eu, Sm掺杂超过上述最佳掺杂浓度时,LaxCuyOz、CexFeyOz出现荧光猝灭现象。
4、TbxOy纳米线阵列荧光强度受激发光波长和Eu, Sm掺杂浓度共同影响。Eu, Sm掺杂浓度在2-20mol%范围内,当激发光波长分别为221nm,394nm, Eu掺杂浓度为2mol%时,Eu掺杂TbxOy纳米线阵列荧光强度最强。当激发光波长分别为221nm,405nm, Sm掺杂浓度分别为5mol%,20mol%时,Sm掺杂TbxOy纳米线阵列荧光强度最强。
In this thesis, LaxZnyOz、LaxMnyOz、LaxFeyOz、LaxCuyOz、CexFeyOz and TbxOy nanowire arrays have been fabricated in the anodic aluminum oxide (AAO) template with chemical deposition reaction via suction filteration at subatmospheric. The SEM、TEM、XRD and EDS were employed to characterize their crystal structure, morphology and chemical composition, respectively. The vibrating sample magnetometer (VSM) was used to study the magnetic performances of LaxZnyOz、 LaxMnyOz、LaxFeyOz、LaxCuyOz、CexFeyOz and TbxOy nanowire arrays, and the fluorescence spectrophotometer (F-4500) was employed to study the fluorescence intensity of LaxCuyOz、CexFeyOz、TbxOy nanowire arrays doped with Tb, Eu or Sm.
The mainly research results are as follow:
1. The above nanowire arrays are all amorphous in structure, and their structure, morphology and chemical composition could be adjusted by reactant concentration, reaction time, subatmospheric of suction filtration, thermal decomposition temperature and the pore size of AAO template.
2. There are obvious magnetic anisotropy of LaxZnyOz、LaxMnyOz、LaxFeyOz、 LaxCuyOz、CexFeyOz nanowire arrays with the applied magnetic field and their easy magnetized direction is parallel to the axis of nanowire except for LaxCuyOz, which is from the shape anistropy of nanowire arrays. The TbxOy nanowire array is paramagnetic with the applied magnetic field.
3. The fluorescence intensities of LaxCuyOz、CexFeyOz nanowire arrays are related with the doped Tb, Eu or Sm within2-30mol%. The results indicated that there is the strongest fluorescence for LaxCuyOz nanowire arrays, when the optimum doping concentration of Tb, Eu is5mol%and that of Sm is30mol%. When the optimum doping concentration of Eu or Sm is10mol%and Tb is5mol%, the fluorescence of CexFeyOz nanowire arrays is the strongest. The LaxCuyOz or CexFeyOz nanowire array is fluorescence quenching, when Eu or Sm is respectively over the optimum doping concentration.
4. The fluorescence intensity of TbxOy nanowire array is both influenced by the exciting light and the doping concentrations of Eu·or Sm. there are the strongest fluorescence peaks of TbxOy nanowire arrays, when the doping concentrations of Eu is2mol%, and the exciting light is respectively221nm,394nm. When the doping concentration of Sm is10mol%or20mol%, the exciting light is respectively221nm,405nm, there are the strongest fluorescence peaks of TbxOy nanowire array.
引文
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