静电纺丝技术制备La_2M_2O_7（M=Ti，Zr，Sn）：RE~(3+)纳米带与发光性质研究
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摘要
低维纳米材料作为器件和材料的基本构成单元对集成电路和功能性元件的构筑,将起到十分重要的作用,其制备和加工是纳米技术领域的重要组成部分。静电纺丝技术因其高效、操作简单等优点,近年来已成为制备无机氧化物低维纳米材料的重要方法之一。La2M2O7(M=Ti, Zr, Sn)本身具有的光学透明性,稀土离子掺杂La2M2O7(M=Ti,Zr, Sn)的纳米发光材料也受到人们的广泛关注。因此,采用静电纺丝技术制备稀土离子掺杂La2M2O7(M=Ti, Zr, Sn)低维纳米发光材料将是一个有意义、重要的研究课题。
本文中以聚乙烯吡咯烷酮和无机盐为原料,通过溶胶-凝胶过程制备出具有一定粘度的前驱体溶胶,并采用静电纺丝技术制备了PVP/无机盐复合纤维及复合纳米带,经过热处理得到了La2Ti2O7：Eu3+纳米纤维、纳米带,La2Zr2O7纳米纤维,La2Zr207:RE3+(RE=Er, Yb/Er)纳米带、纳米纤维,La2Zr207:RE3+(RE=Eu,Tb)纳米纤维,La2Sn2O7纳米纤维,采用TG-DTA、XRD、FTIR、FESEM、TEM、UV-Vis和荧光光谱等技术对样品进行了表征。结果表明,所制备的稀土离子掺杂的La2M2O7(M=Ti, Zr)纳米带为纳米短棒或粒子组成,宽厚比大,平均带宽3-5μm,厚度约90-140nm。所制备的稀土离子掺杂的La2M2O7(M=Zr, Sn)纳米纤维尺寸均一,彼此没有交联,没有断裂,纤维直径平均为140-180 nm。获得了一些有意义的研究结果,为进一步深入研究稀土离子掺杂的La2M2O7(M=Ti, Zr, Sn)发光或者上转换发光低维纳米材料的性质奠定了一定的基础。
Low-dimensional nanomaterials are the basic component unit of devices and materials, which will play an important role in building integrated circuits and functional devices. The preparation and processing of low-dimensional nanomaterials have become key components in the field of nanotechnology. In recent years, electrospinning technology has been proved to be one of the effective methods to prepare inorganic oxides low-dimensional nanomaterials owing to its high efficiency, simple operation and so on. La2M2O7(M=Ti, Zr, Sn) are important matrixes for luminescence due to its optical transparency. Recently, Low-dimensional La2M2O7(M=Ti, Zr, Sn) luminescent nanomaterials have also aroused a lot of concern from scientists. Therefore, fabrication of rare earth ions-doped La2M2O7(M=Ti, Zr, Sn) low-dimensional luminescent nanomaterials via electrospinning will be a meaningful subject of significance.
In this dissertation, sol-gel process was applied to prepare the precursor sol of certain viscosity using PVP and various inorganic salts as starting materials, and electrospinning technique was used to fabricate PVP/inorganic salts composite nanofibers and composite nanobelts. La2Ti2O7:Eu3+nanobelts and nanofibers, La2Zr2O7 nanofibers, La2Zr207:RE3+(RE=Er, Yb/Er) nanobelts and nanofibers, La2Zr207:RE3+(RE=Eu, Tb) nanofibers, La2Zr2O7 nanofibers were fabricated by calcination of the as-prepared composite nanofibers and composite nanobelts. The samples were characterized by thermogravimetric-differential thermal analysis (TG-DTA), x-ray diffractometry (XRD), Fourier transform infrared spectrometry (FTIR), field emission scanning electron microscope (FESEM), transmission electron microscope (TEM), UV-Vis absorption spectroscopy (UV-Vis) and fluorescence spectroscopy. The results showed that as-prepared rare earth ions-doped La2M2O7(M=Ti, Zr) nanobelts with large width-to-thickness ratios were composed of nanorods or nanoparticles, the width of nanobelts were 0.45-5μm, and the thickness were ca.90-140 nm. The diameters of as-prepared rare earth ions-doped La2M2O7(M=Zr, Sn) nanofibers were in narrow range, and there is no cross-linking among nanofibers, and the diameter was about 140-180 nm. Some meaningful results were obtained, and laid solid foundation for the future study of luminescence or up-conversion luminescence of rare earth ions-doped La2M2O7(M=Ti, Zr, Sn) low-dimensional nanomaterials.
本文中以聚乙烯吡咯烷酮和无机盐为原料,通过溶胶-凝胶过程制备出具有一定粘度的前驱体溶胶,并采用静电纺丝技术制备了PVP/无机盐复合纤维及复合纳米带,经过热处理得到了La2Ti2O7：Eu3+纳米纤维、纳米带,La2Zr2O7纳米纤维,La2Zr207:RE3+(RE=Er, Yb/Er)纳米带、纳米纤维,La2Zr207:RE3+(RE=Eu,Tb)纳米纤维,La2Sn2O7纳米纤维,采用TG-DTA、XRD、FTIR、FESEM、TEM、UV-Vis和荧光光谱等技术对样品进行了表征。结果表明,所制备的稀土离子掺杂的La2M2O7(M=Ti, Zr)纳米带为纳米短棒或粒子组成,宽厚比大,平均带宽3-5μm,厚度约90-140nm。所制备的稀土离子掺杂的La2M2O7(M=Zr, Sn)纳米纤维尺寸均一,彼此没有交联,没有断裂,纤维直径平均为140-180 nm。获得了一些有意义的研究结果,为进一步深入研究稀土离子掺杂的La2M2O7(M=Ti, Zr, Sn)发光或者上转换发光低维纳米材料的性质奠定了一定的基础。
Low-dimensional nanomaterials are the basic component unit of devices and materials, which will play an important role in building integrated circuits and functional devices. The preparation and processing of low-dimensional nanomaterials have become key components in the field of nanotechnology. In recent years, electrospinning technology has been proved to be one of the effective methods to prepare inorganic oxides low-dimensional nanomaterials owing to its high efficiency, simple operation and so on. La2M2O7(M=Ti, Zr, Sn) are important matrixes for luminescence due to its optical transparency. Recently, Low-dimensional La2M2O7(M=Ti, Zr, Sn) luminescent nanomaterials have also aroused a lot of concern from scientists. Therefore, fabrication of rare earth ions-doped La2M2O7(M=Ti, Zr, Sn) low-dimensional luminescent nanomaterials via electrospinning will be a meaningful subject of significance.
In this dissertation, sol-gel process was applied to prepare the precursor sol of certain viscosity using PVP and various inorganic salts as starting materials, and electrospinning technique was used to fabricate PVP/inorganic salts composite nanofibers and composite nanobelts. La2Ti2O7:Eu3+nanobelts and nanofibers, La2Zr2O7 nanofibers, La2Zr207:RE3+(RE=Er, Yb/Er) nanobelts and nanofibers, La2Zr207:RE3+(RE=Eu, Tb) nanofibers, La2Zr2O7 nanofibers were fabricated by calcination of the as-prepared composite nanofibers and composite nanobelts. The samples were characterized by thermogravimetric-differential thermal analysis (TG-DTA), x-ray diffractometry (XRD), Fourier transform infrared spectrometry (FTIR), field emission scanning electron microscope (FESEM), transmission electron microscope (TEM), UV-Vis absorption spectroscopy (UV-Vis) and fluorescence spectroscopy. The results showed that as-prepared rare earth ions-doped La2M2O7(M=Ti, Zr) nanobelts with large width-to-thickness ratios were composed of nanorods or nanoparticles, the width of nanobelts were 0.45-5μm, and the thickness were ca.90-140 nm. The diameters of as-prepared rare earth ions-doped La2M2O7(M=Zr, Sn) nanofibers were in narrow range, and there is no cross-linking among nanofibers, and the diameter was about 140-180 nm. Some meaningful results were obtained, and laid solid foundation for the future study of luminescence or up-conversion luminescence of rare earth ions-doped La2M2O7(M=Ti, Zr, Sn) low-dimensional nanomaterials.
引文
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