稀土氧化物纳米管阵列的制备及其性能研究
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摘要
本文用负压抽滤法,在多孔氧化铝膜(AAO)中制备出多种稀土-过渡金属氧化物纳米管阵列,并对它们的结构组成,光、磁性能进行研究,研究结果如下：
1.利用孔径为80nm AAO模板,辅之负压抽滤法,在AAO模板纳米孔道中合成了LaxCoyOz纳米管阵列。利用扫描电镜(SEM)、透射电镜(TEM)、X-射线衍射仪(XRD)、选区电子衍射(SAED)、能量色散仪(EDS)、振动样品磁强计(VSM)等,对LaxCoyOz纳米管阵列的形貌结构、化学组成和性能进行表征。结果表明：在AAO中的LaxCoyOz纳米管阵列尺寸均匀一致、高填充率,LaxCoyOz纳米管阵列为非晶结构；具有磁各向异性,在水平方向(H//)和垂直方向(H⊥)的矫顽力分别为39240e和3450e,易磁化方向是平行于纳米管阵列的方向。
2.制备出Eu3+掺杂LaxCoyOz纳米管阵列,并用荧光光度计测试其荧光特性。结果表明：在394nm的光激发下,LaxCoyOz:Eu纳米管阵列在592nm和616nm处有两个宽的发射峰,分别归属于Eu3+的5Do→7F1和5D0→7F2的跃迁。当Eu3+掺杂浓度为2%时,LaxCoyOz:Eu纳米管阵列的荧光强度最强；随着Eu3+掺杂浓度的增加,荧光强度逐渐减弱；当Eu3+掺杂浓度为10%,出现荧光猝灭现象。
3.分别制备出非晶态的LaxOy、LaxCoyOz、LaxFeyOz、LaxNiyOz的纳米管阵列。用VSM表征它们的磁性能,实验结果表明：上述纳米管均具有磁各向异性,且易磁化方向都是平行于纳米管阵列方向；在H//和H⊥方向,LaxOy纳米管阵列掺Co以后,H//和H⊥方向的矫顽力都增大；LaxOy纳米管阵列掺入Fe、Ni后,H//方向矫顽力减小,H⊥方向矫顽力增大。
4.制备并研究了不同孔径和不同过渡金属掺杂的稀土氧化物纳米管阵列,并研究了其红外光吸收性能。实验结果表明：大孔径的LaxCoyOz纳米管阵列红外吸收性能最强,吸收率达到97%；比较在LaxOy纳米管阵列中掺过渡金属Co、Ni、Zn、Fe后的红外光吸收性能发现：LaxCoyOz纳米管阵列的红外吸收能力最强。
In this paper, synthesized several rare earth-transition metal oxide nanotube array materials in AAO using the suction filtration at subatmospheric pressure (S FSP) method.The optical and magnetic properties of the nano-materials were studi ed and the results were shown below:
1.Using the SFSP method, LaxCoyOz nanotube arrays were prepared in th e nano-channels of AAO. The morphology, structure, chemical composition and prop erties of the LaxCoyOz nanotube array were researched by scanning electron micros cope(SEM), transmission electron microscope(TEM), X-ray diffraction(XRD), energ y dispersive spectrometer(EDS), selected area electron diffraction(SAED), vibratin g sample magnetometer(VSM).The results showed that LaxCoyOz nanotube arrays s ynthetized by SFSP are amorphous structure.The hysteresis loop showed that the co ercivity of LaxCoyOz nanotube arrays obvious magnetic anisotropy in the parall el direction and the perpendicular direction.The coercivity of LaxCoyOz nanotube arrays in paralled and vertical direction are3924Oe and345Oe, the easily magne tized direction is parallel to the nanotube array.
2.LaxCoyOz:Eu nanotube arrays have been synthesized in AAO template by suction filtration at subatmospheric pressure.The results show that:The LaxCoy Oz:Eu nanotube arrays exhibited two fluorescence emission bands around592n m and616nm under theexcitation of394nm, which recorresponding to5D0→7F1and5D0→7F2transitions of the Eu3+and the optimum doping concentration of Eu3+is2%.
3.Using the suction filtration at subatmospheric pressure and AAO template, amorphous nanotube arrays were prepared including LaxOy, LaxCoyOz, LaxFey Oz, and LaxNiyOz.Hysteresis loop shows that the LaxOy nanotube arrays are al1soft ferromagnetic performance, the parallel direction coercivity. Whereas, the easy magnetizationability was enhanced obviously because of the Co element doped.The nanotube arrays show a strong shape anisotropy and the easily m agnetized direction isparallel to the nanotube arrays.
4.The nanotube arrays with different diameter and transition metal were prepa red with SPSF and AAO, the capabilities of them to absorb the infrared light wer e tested with FTIR.The FTIR Spectra result showed that the infrared light absorbin g capabilities of the nanotube arrays was about97%were best at about200nm by th e test of different aperture of LaxCoyOz nanotube arrays,The nano-material with Fe, Ni,Zn,Co had the strongest infrared light absorbing ability.
1.利用孔径为80nm AAO模板,辅之负压抽滤法,在AAO模板纳米孔道中合成了LaxCoyOz纳米管阵列。利用扫描电镜(SEM)、透射电镜(TEM)、X-射线衍射仪(XRD)、选区电子衍射(SAED)、能量色散仪(EDS)、振动样品磁强计(VSM)等,对LaxCoyOz纳米管阵列的形貌结构、化学组成和性能进行表征。结果表明：在AAO中的LaxCoyOz纳米管阵列尺寸均匀一致、高填充率,LaxCoyOz纳米管阵列为非晶结构；具有磁各向异性,在水平方向(H//)和垂直方向(H⊥)的矫顽力分别为39240e和3450e,易磁化方向是平行于纳米管阵列的方向。
2.制备出Eu3+掺杂LaxCoyOz纳米管阵列,并用荧光光度计测试其荧光特性。结果表明：在394nm的光激发下,LaxCoyOz:Eu纳米管阵列在592nm和616nm处有两个宽的发射峰,分别归属于Eu3+的5Do→7F1和5D0→7F2的跃迁。当Eu3+掺杂浓度为2%时,LaxCoyOz:Eu纳米管阵列的荧光强度最强；随着Eu3+掺杂浓度的增加,荧光强度逐渐减弱；当Eu3+掺杂浓度为10%,出现荧光猝灭现象。
3.分别制备出非晶态的LaxOy、LaxCoyOz、LaxFeyOz、LaxNiyOz的纳米管阵列。用VSM表征它们的磁性能,实验结果表明：上述纳米管均具有磁各向异性,且易磁化方向都是平行于纳米管阵列方向；在H//和H⊥方向,LaxOy纳米管阵列掺Co以后,H//和H⊥方向的矫顽力都增大；LaxOy纳米管阵列掺入Fe、Ni后,H//方向矫顽力减小,H⊥方向矫顽力增大。
4.制备并研究了不同孔径和不同过渡金属掺杂的稀土氧化物纳米管阵列,并研究了其红外光吸收性能。实验结果表明：大孔径的LaxCoyOz纳米管阵列红外吸收性能最强,吸收率达到97%；比较在LaxOy纳米管阵列中掺过渡金属Co、Ni、Zn、Fe后的红外光吸收性能发现：LaxCoyOz纳米管阵列的红外吸收能力最强。
In this paper, synthesized several rare earth-transition metal oxide nanotube array materials in AAO using the suction filtration at subatmospheric pressure (S FSP) method.The optical and magnetic properties of the nano-materials were studi ed and the results were shown below:
1.Using the SFSP method, LaxCoyOz nanotube arrays were prepared in th e nano-channels of AAO. The morphology, structure, chemical composition and prop erties of the LaxCoyOz nanotube array were researched by scanning electron micros cope(SEM), transmission electron microscope(TEM), X-ray diffraction(XRD), energ y dispersive spectrometer(EDS), selected area electron diffraction(SAED), vibratin g sample magnetometer(VSM).The results showed that LaxCoyOz nanotube arrays s ynthetized by SFSP are amorphous structure.The hysteresis loop showed that the co ercivity of LaxCoyOz nanotube arrays obvious magnetic anisotropy in the parall el direction and the perpendicular direction.The coercivity of LaxCoyOz nanotube arrays in paralled and vertical direction are3924Oe and345Oe, the easily magne tized direction is parallel to the nanotube array.
2.LaxCoyOz:Eu nanotube arrays have been synthesized in AAO template by suction filtration at subatmospheric pressure.The results show that:The LaxCoy Oz:Eu nanotube arrays exhibited two fluorescence emission bands around592n m and616nm under theexcitation of394nm, which recorresponding to5D0→7F1and5D0→7F2transitions of the Eu3+and the optimum doping concentration of Eu3+is2%.
3.Using the suction filtration at subatmospheric pressure and AAO template, amorphous nanotube arrays were prepared including LaxOy, LaxCoyOz, LaxFey Oz, and LaxNiyOz.Hysteresis loop shows that the LaxOy nanotube arrays are al1soft ferromagnetic performance, the parallel direction coercivity. Whereas, the easy magnetizationability was enhanced obviously because of the Co element doped.The nanotube arrays show a strong shape anisotropy and the easily m agnetized direction isparallel to the nanotube arrays.
4.The nanotube arrays with different diameter and transition metal were prepa red with SPSF and AAO, the capabilities of them to absorb the infrared light wer e tested with FTIR.The FTIR Spectra result showed that the infrared light absorbin g capabilities of the nanotube arrays was about97%were best at about200nm by th e test of different aperture of LaxCoyOz nanotube arrays,The nano-material with Fe, Ni,Zn,Co had the strongest infrared light absorbing ability.
引文
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