静电纺丝法制备一维纳米稀土氧化物和钒酸盐发光材料及其性质研究
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摘要
近年来,一维新型纳米结构材料以其独特的荧光特性在纳米级别的电子学、光学、显示器和先进生物分析上的广泛应用而受到研究者极大的重视。因此,寻找出制备完美形貌的纳米荧光材料的简单方法是非常重要的。而溶胶凝胶过程和电纺丝技术相结合的方法是制备一维和准一维纳米材料的有效方法。本论文采取了这种新颖方法制备出了具有完美形貌的一维纳米纤维。
本文利用静电纺丝法制备出一系列的一维纳米发光材料,例如:稀土氧化物纳米纤维和钒酸盐纳米纤维。利用X-射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、红外光谱(FT-IR)、差热-热重分析(TG-DTA)等技术对合成材料的结构、形貌、组成进行表征,用荧光光谱、低压阴极射线光谱等手段来评价所制备的材料的发光性质。同时就离子掺杂浓度对发光强度的影响做了进一步的讨论。
采用静电纺丝法制备了具有一维结构的Lu_2O_3:Eu~(3+)纳米纤维荧光粉。X-射线衍射(XRD)、红外光谱(FT-IR)和差热热重(TG-DTA)研究结果表明,Lu_2O_3:Eu~(3+)样品在900℃结晶,通过FESEM可以看出所制备的样品都是均匀的纤维状。TEM进一步表明了所制备的样品是由许多纳米粒子堆积而成的。在紫外光和低压电子束的激发下,样品发出强的红光。
采用简单、方便的静电纺丝方法成功制备了一维GdVO4:Ln~(3+)(Ln=Eu,Dy,Sm)纳米纤维。所得到的GdVO_4:Ln~(3+)(Ln=Eu,Dy,Sm)纳米纤维在700℃结晶完好。从扫描电镜结果可知,所制备的前驱纤维比较均匀且表面平滑,经过700℃煅烧4个小时后,纤维直径大幅减小并且仍然保持原来的纤维状,但表面变得粗糙了。光致发光和阴极射线发光光谱表明,GdVO_4:Ln~(3+)纳米纤维由于钒酸根向其掺杂离子的有效能量传递都表现出这些离子典型的特征发光。
In recent years, there is growing interest on exploring new luminescent materials onone-dimensional (1D) nanostructures, since they exhibit specific and fascinatingluminescent properties, which possess diverse potential applications in nanoscaleelectronics, photonics, display and advanced bioanalysis. So it is important to developsome facile synthesis methods to directly prepare luminescent materials innano-/microscale with defined morphologies. A combination method of sol-gel processand electrospinning technique is a good approach to obtain excellent 1D and Q-1Dnano- /microstructures. In this paper, we focus our attention on the preparation of 1Dnanofibers by the novel and facile sol-gel/electrospinning process.
A series of luminescent materials, such as one-dimensional (1D) nanostructuralrare earth oxides and vanadates phosphors, have been prepared by a simple andcost-effective electrospinning process. These obtained samples were characterized byX-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM),transmission electron microscopy (TEM), Fourier transform infrared spectra (FT-IR),thermogravimetric and differential thermal analysis (TG-DTA), photoluminescence(PL), cathodoluminescence (CL) spectra and so on. The effects of the concentration ofdoping ions on the luminescent properties of the samples were investigated in detail.
One-dimensional Lu_2O_3:Eu~(3+) nanofibers have been prepared by means ofelectrospinning technique in conjunction with sol-gel process. The XRD, FT-IR andTG-DTA results show that Lu2O3:Eu~(3+) samples crystallize at 900℃. SEM imagesindicate that as prepared precursor samples and those annealed at 900℃presentuniform fiberlike morphology. TEM image further manifests that the as formedLu_2O_3:Eu~(3+) nanofibers consist of nanoparticles. Under the short wavelength ultravioletirradiation and the low-voltage electron beam excitation, Lu2O3:Eu~(3+) nanofibers allexhibit typical red (5D0–7FJ) emission.
One-dimensional GdVO_4:Ln~(3+) (Ln = Eu, Dy, Sm) nanofibers have beensuccessfully prepared by a simple and versatile elcetrospinning method and sol-gelprocess. The obtained samples crystallized well at 700℃. SEM images indicate that theas prepared precursor fibers are smooth. After being calcined at 700℃for 4 h, the fibersstill maintain their fiberlike morphology with rough surface. Under ultraviolet excitationand low-voltage electron beam excitation, GdVO4:Ln~(3+) phosphors showed their strong characteristic emission due to an efficient energy transfer from vanadate groups todopants.
本文利用静电纺丝法制备出一系列的一维纳米发光材料,例如:稀土氧化物纳米纤维和钒酸盐纳米纤维。利用X-射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、红外光谱(FT-IR)、差热-热重分析(TG-DTA)等技术对合成材料的结构、形貌、组成进行表征,用荧光光谱、低压阴极射线光谱等手段来评价所制备的材料的发光性质。同时就离子掺杂浓度对发光强度的影响做了进一步的讨论。
采用静电纺丝法制备了具有一维结构的Lu_2O_3:Eu~(3+)纳米纤维荧光粉。X-射线衍射(XRD)、红外光谱(FT-IR)和差热热重(TG-DTA)研究结果表明,Lu_2O_3:Eu~(3+)样品在900℃结晶,通过FESEM可以看出所制备的样品都是均匀的纤维状。TEM进一步表明了所制备的样品是由许多纳米粒子堆积而成的。在紫外光和低压电子束的激发下,样品发出强的红光。
采用简单、方便的静电纺丝方法成功制备了一维GdVO4:Ln~(3+)(Ln=Eu,Dy,Sm)纳米纤维。所得到的GdVO_4:Ln~(3+)(Ln=Eu,Dy,Sm)纳米纤维在700℃结晶完好。从扫描电镜结果可知,所制备的前驱纤维比较均匀且表面平滑,经过700℃煅烧4个小时后,纤维直径大幅减小并且仍然保持原来的纤维状,但表面变得粗糙了。光致发光和阴极射线发光光谱表明,GdVO_4:Ln~(3+)纳米纤维由于钒酸根向其掺杂离子的有效能量传递都表现出这些离子典型的特征发光。
In recent years, there is growing interest on exploring new luminescent materials onone-dimensional (1D) nanostructures, since they exhibit specific and fascinatingluminescent properties, which possess diverse potential applications in nanoscaleelectronics, photonics, display and advanced bioanalysis. So it is important to developsome facile synthesis methods to directly prepare luminescent materials innano-/microscale with defined morphologies. A combination method of sol-gel processand electrospinning technique is a good approach to obtain excellent 1D and Q-1Dnano- /microstructures. In this paper, we focus our attention on the preparation of 1Dnanofibers by the novel and facile sol-gel/electrospinning process.
A series of luminescent materials, such as one-dimensional (1D) nanostructuralrare earth oxides and vanadates phosphors, have been prepared by a simple andcost-effective electrospinning process. These obtained samples were characterized byX-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM),transmission electron microscopy (TEM), Fourier transform infrared spectra (FT-IR),thermogravimetric and differential thermal analysis (TG-DTA), photoluminescence(PL), cathodoluminescence (CL) spectra and so on. The effects of the concentration ofdoping ions on the luminescent properties of the samples were investigated in detail.
One-dimensional Lu_2O_3:Eu~(3+) nanofibers have been prepared by means ofelectrospinning technique in conjunction with sol-gel process. The XRD, FT-IR andTG-DTA results show that Lu2O3:Eu~(3+) samples crystallize at 900℃. SEM imagesindicate that as prepared precursor samples and those annealed at 900℃presentuniform fiberlike morphology. TEM image further manifests that the as formedLu_2O_3:Eu~(3+) nanofibers consist of nanoparticles. Under the short wavelength ultravioletirradiation and the low-voltage electron beam excitation, Lu2O3:Eu~(3+) nanofibers allexhibit typical red (5D0–7FJ) emission.
One-dimensional GdVO_4:Ln~(3+) (Ln = Eu, Dy, Sm) nanofibers have beensuccessfully prepared by a simple and versatile elcetrospinning method and sol-gelprocess. The obtained samples crystallized well at 700℃. SEM images indicate that theas prepared precursor fibers are smooth. After being calcined at 700℃for 4 h, the fibersstill maintain their fiberlike morphology with rough surface. Under ultraviolet excitationand low-voltage electron beam excitation, GdVO4:Ln~(3+) phosphors showed their strong characteristic emission due to an efficient energy transfer from vanadate groups todopants.
引文
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