稀土氧化物纳米结构的可控合成及性能研究
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摘要
本文采用负压抽滤法,以氧化铝(AAO)为模板,制备出NdCoxOy、LaNdxPy、 NdCoxOy:Eu、LaNdxOy:Eu稀土氧化物纳米阵列结构,并研究了它们的结构和性能。研究结果如下：
1.采用两步阳极氧化法分别在硫酸、草酸、磷酸溶液中,分别制备出孔径为50nm,80nm,130nm,200-250nm,350-400nmAAO模板。采用负压抽滤法,在AA0模板中制备了NdCoxOy纳米线阵列。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)、振动样品磁强计(VSM)等对NdCoxOy纳米线形貌、结构和化学组成及磁性能进行表征。结果表明：NdCoxOy纳米线是非晶结构；具有明显磁各向异性,且易磁化方向是外加磁场平行于纳米线方向。
2.在AAO模板中,制备了NdCoxOy:Eu、LaNdxOy:Eu纳米管阵列。对其形貌和晶相结构进行表征；并研究了它们的荧光性能。结果表明：NdCoxOy:Eu、 LaNdxOy:Eu纳米管都是非晶态结构；在波长394nm的光激发下,NdCoxOy:Eu、 LaNdxOy:Eu纳米管阵列,593nm处都出现一个宽的荧光发射峰,为Eu3+的5Do-7F1跃迁,这与发光基质无关。
3.制备了LaNdxOy纳米线及纳米管阵列,研究了热处理工艺对LaNdxOy纳米线阵列晶相结构和LaNdxOy:Eu纳米线阵列荧光性能的影响。结果表明：LaNdxOy纳米线阵列晶相结构与热处理温度无关,但LaNdxOy:Eu纳米线阵列的荧光强度随着热处理温度的升高而变强。LaNdxOy结构与性能测试的结果表明：LaNdxOy:Eu纳米线的荧光强度弱于LaNdxOy:Eu纳米管的；LaNdxOy:Eu纳米线的荧光强度随着纳米线直径的增大而变小。LaNdxOy纳米管阵列具有明显的磁各向异性,平行方向的矩形比比垂直方向高,LaNdxOy纳米管阵列具备明显的软磁体特征。
We have employed anodic aluminium (AAO) as template to prepare NdCoxOy、 LaNdxOy、NdCoxOy:Eu、LaNdxOy:Eu rare earth oxide nanoarrays nanostructure by suction filtration at subatmospheric pressure. The detailed researches of the thesis are as follows:
1. The different nanopores porous anodic aluminum oxide (AAO) template have been fabricated by two-step anodization using in sulfuric, oxalic acid and phosphoric acid. The NdCoxOy nanowire arrays have been successfully fabricated in AAO by suction filtration at subatmospheric pressure (SFSP). The morphology, structure, chemical composition and magnetic performance of NdCoxOy nanowires have been characterized by scanning electron microscope(SEM)、transmission electron microscope (TEM)、x-ray diffraction (XRD)、energy dispersive spectra (EDS) and vibrating sample magnetometer(VSM). The results show the NdCoxOy nanowires is amorphous in structure. There are obvious magnetic anisotropy for NdCoxOy nanowire arrays, and the easily magnetized direction is parallel to the nanowire arrays.
2. The NdCoxOy:Euand LaNdxOy:Eu nanotube arrays have been synthesized by the method of SFSP assisted AAO template. The morphology and the crystal structure have been investigated and luminescence Properties have been studied. The results show that the nanotubes are both amorphous in structure, the diameter of nanotube is homogeneous. The result of the fluorescence spectrum for the two nanotubes indicates that there are both a strong broad emission peak at593nm under394nm excitation characterized as transition5D0-7F1of the Eu3+ions, which is not related to the substrate.
3. LaNdxOy nanowire arrays and LaNdxOy nanotubes arrays have been prepared. We have researched heat treatment technology on the influence of the structure of LaNdxOy nanowire arrays, luminescence Property of LaNdxOy:Eu3+nanowire arrays, we find thermal treatment temperature do not influence the structure of LaNdxOy nanowire arrays, but luminescence intensity of LaNdxOy:Eu nanowire arrays increases with increasing the calcination temperature. The result reveals that the luminescence intensity of LaNdxOy:Eu nanowires is weaker than that of LaNdxOy:Eu nanotubes, and the luminescence intensity of LaNdxOy:Eu nanowires increases with decreasing the diameter of the nanowires. The magnetic property of LaNdxOy nanotube arrays shows that the squareness along the parallel direction is higher than that of the perpendicular direction, and it exhibits obvious soft ferromagnetism in both parallel and perpendicular directions.
1.采用两步阳极氧化法分别在硫酸、草酸、磷酸溶液中,分别制备出孔径为50nm,80nm,130nm,200-250nm,350-400nmAAO模板。采用负压抽滤法,在AA0模板中制备了NdCoxOy纳米线阵列。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)、振动样品磁强计(VSM)等对NdCoxOy纳米线形貌、结构和化学组成及磁性能进行表征。结果表明：NdCoxOy纳米线是非晶结构；具有明显磁各向异性,且易磁化方向是外加磁场平行于纳米线方向。
2.在AAO模板中,制备了NdCoxOy:Eu、LaNdxOy:Eu纳米管阵列。对其形貌和晶相结构进行表征；并研究了它们的荧光性能。结果表明：NdCoxOy:Eu、 LaNdxOy:Eu纳米管都是非晶态结构；在波长394nm的光激发下,NdCoxOy:Eu、 LaNdxOy:Eu纳米管阵列,593nm处都出现一个宽的荧光发射峰,为Eu3+的5Do-7F1跃迁,这与发光基质无关。
3.制备了LaNdxOy纳米线及纳米管阵列,研究了热处理工艺对LaNdxOy纳米线阵列晶相结构和LaNdxOy:Eu纳米线阵列荧光性能的影响。结果表明：LaNdxOy纳米线阵列晶相结构与热处理温度无关,但LaNdxOy:Eu纳米线阵列的荧光强度随着热处理温度的升高而变强。LaNdxOy结构与性能测试的结果表明：LaNdxOy:Eu纳米线的荧光强度弱于LaNdxOy:Eu纳米管的；LaNdxOy:Eu纳米线的荧光强度随着纳米线直径的增大而变小。LaNdxOy纳米管阵列具有明显的磁各向异性,平行方向的矩形比比垂直方向高,LaNdxOy纳米管阵列具备明显的软磁体特征。
We have employed anodic aluminium (AAO) as template to prepare NdCoxOy、 LaNdxOy、NdCoxOy:Eu、LaNdxOy:Eu rare earth oxide nanoarrays nanostructure by suction filtration at subatmospheric pressure. The detailed researches of the thesis are as follows:
1. The different nanopores porous anodic aluminum oxide (AAO) template have been fabricated by two-step anodization using in sulfuric, oxalic acid and phosphoric acid. The NdCoxOy nanowire arrays have been successfully fabricated in AAO by suction filtration at subatmospheric pressure (SFSP). The morphology, structure, chemical composition and magnetic performance of NdCoxOy nanowires have been characterized by scanning electron microscope(SEM)、transmission electron microscope (TEM)、x-ray diffraction (XRD)、energy dispersive spectra (EDS) and vibrating sample magnetometer(VSM). The results show the NdCoxOy nanowires is amorphous in structure. There are obvious magnetic anisotropy for NdCoxOy nanowire arrays, and the easily magnetized direction is parallel to the nanowire arrays.
2. The NdCoxOy:Euand LaNdxOy:Eu nanotube arrays have been synthesized by the method of SFSP assisted AAO template. The morphology and the crystal structure have been investigated and luminescence Properties have been studied. The results show that the nanotubes are both amorphous in structure, the diameter of nanotube is homogeneous. The result of the fluorescence spectrum for the two nanotubes indicates that there are both a strong broad emission peak at593nm under394nm excitation characterized as transition5D0-7F1of the Eu3+ions, which is not related to the substrate.
3. LaNdxOy nanowire arrays and LaNdxOy nanotubes arrays have been prepared. We have researched heat treatment technology on the influence of the structure of LaNdxOy nanowire arrays, luminescence Property of LaNdxOy:Eu3+nanowire arrays, we find thermal treatment temperature do not influence the structure of LaNdxOy nanowire arrays, but luminescence intensity of LaNdxOy:Eu nanowire arrays increases with increasing the calcination temperature. The result reveals that the luminescence intensity of LaNdxOy:Eu nanowires is weaker than that of LaNdxOy:Eu nanotubes, and the luminescence intensity of LaNdxOy:Eu nanowires increases with decreasing the diameter of the nanowires. The magnetic property of LaNdxOy nanotube arrays shows that the squareness along the parallel direction is higher than that of the perpendicular direction, and it exhibits obvious soft ferromagnetism in both parallel and perpendicular directions.
引文
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