摘要
随着纳米技术的迅速发展,纳米发光材料由于具有高的发光强度和高的量子效率等特性,已经成为人们关注和研究的热点。在众多纳米发光材料中,以稀土磷酸盐为基质的纳米发光材料在紫外光以及真空紫外光激发下具有很好的发光性质,而且在恶劣工作环境下具有很好的稳定性,因而在各种照明和显示仪器具有广泛的应用前景。
本文综述了纳米发光材料的研究现状,系统介绍了镧系离子的光谱理论及镧系掺杂发光纳米微粒的研究背景,概括和评述了近年来镧系掺杂发光磷酸盐纳米微粒的合成和表面修饰所取得的进展和面临的问题,并对其今后的研究方向进行了总结和展望。在此基础上,我们针对场发射显示器(FED)和等离子平板显示器(PDP)对发光材料的要求,以稀土磷酸盐纳米发光材料作为研究对象,采用共沉淀法,成功制备了多种具有不同光学性质的稀土磷酸盐纳米晶。应用X射线衍射(XRD)、场发射扫描电镜(SEM)、透射电镜(TEM)、光致发光光谱(PL)、傅立叶变换红外光谱(FT-IR)、发光衰减曲线和寿命等手段研究了合成条件和掺杂离子浓度等对稀土磷酸盐纳米微粒的晶体结构、形貌和尺寸、表面化学性质、掺杂离子的固溶度和掺杂格位以及发光性能的影响和控制规律,另外,对于不同基质中Eu~(3+)的发光性质进行了讨论,同时重点讨论了YPO_4基质中Ce~(3+)离子对Tb~(3+)离子的敏化作用机理,取得了一系列重要的结论和创新性成果,为稀土磷酸盐纳米发光材料成为一种极具发展前景的新型发光材料打下了坚实的基础。
采用水热法,通过控制水热条件分别可控合成了四方相,六方相和单斜相的LnPO_4纳米和纳米颗粒,分析了水热合成条件以及结构导向剂CTAB对于样品的结构以及形貌的影响以及热力学过程对于其成核的影响,比较了不同形貌以及不同相的Re~(3+)掺杂的LnPO_4的发光性质,并对发光机理进行了探讨。并证明这些纳米晶的光谱性质与基质材料的晶体结构和形貌密切相关,为通过结构设计实现对稀土纳米材料光学性能的调控提供了新思路。
With the technical development of FED and PDP, the requirement including crystal size distribution, stability, luminescence efficiency, brightness, and conductivity of the luminescent powder also has been improved. Meanwhile, with the development of nanotechnology, nanoscale luminescent materials are likely to be the next generation novel luminescent materials due to their numerous unique properties. Among many nano-materials, rare-earth phosphates are ideal to be the fluorescence host material for their good chemical and thermal stability. However, up to now, the investigation of the fluorescence properties of these materials is limited. In this paper, rare-earth phosphate fluorescence nano-materials were prepared through many different ways, and the fluorescence properties were also systematically investigated. These results are helpful for us to find a new type of high-powered fluorescence materials.
1. In the first chapter, we briefly expound the research condition of fluorescence nano-materials; systematically introduce the spectrum theory of rare earth ions and the research background of rare earth ions doped fluorescence nano-materials; besides that, we generalize and comment the improvement of the synthesis and surface modification of fluorescence nano-materials, as well as the problem which confronts; moreover, the research direction also be prospected and summarized.
2. In order to improve the properties for application of YPO_4:Re~(3+), We have synthesized a series of nano-scale YPO_4: Re~(3+) (Re = Eu, Dy)through the improved co-precipitation method with Li_2CO_3 as a flux. At the same time, we have investigated the best synthesis conditions: such as pH, the concentration of Re~(3+), the additional concentration of Li_2CO_3 and the anneal temperature. The optimum luminescent intensity could be achieved when the concentration of Eu~(3+) was 6%, the concentration of Li_2CO_3 is 10%, the annealed temperature is 950℃and the value of pH is 2. The nanoparticles we synthesized have a well crystalline morphology with nanometer dimension and the particle sizes of obtained nanocrystals were distributed in the range of 20-100 nm without Li_2CO_3 flux through XRD. Under the irradiation of UV, we studied the fluorescence properties of the powder, YPO_4: Eu、YPO_4: Dy nanocrystals imply orangish and white-emitting, which is corresponding to transitions of ~5D_0 - ~7F_1 and ~4F_(9/2)→~6H_(15/2). Furthermore, a small shift of the excitation bands could be observed for the YPO_4: Eu nanoparticles, duing to the small particle size of the sample. When the flux Li_2CO_3 is used, the crystallization of samples is improved, and the particle size is increased. Furthermore, the energy loss of non-radiative is descreased, and the activate ions are easy to enter the lattice to form the luminescence centers, which result in the strong luminescent intensity.
3. At the same time, we also prepared Eu~(3+) iron doped LaPO_4 nanocrystalline by co-precipitation method at 950℃, 3 h. The obtained LaPO_4 have nano-crystalline, particle size of about 70 nm, and the improvement of the calcination temperature can be increased the degree of crystallization of the samples. X-ray powder diffraction confirmed the structure of LaPO_4 monoclinic, cell parameters a = 6.84, b = 7.08, c = 6.46,β= 103.85°, is P2_1 / n (No·14) space group. The PL properties of the Eu~(3+)-doped LaPO_4 nanocrystals were discussed. Fluorescence spectra indicate that: the charge transfer excited states of LaPO_4 can effectively transfer energy to the Eu~(3+) ions. Four emission peaks, which are at 592, 612 nm emission peak near the two split both phenomena, description of the Eu~(3+) ion doped in the crystal LaPO_4 have not the same coordination environment, that Eu~(3+) ions exsite sites D_(2d) or C_3 symmetry. The optimum quantity of concentration Eu~(3+) is 5%. The concentration quenching is due to Eu~(3+) ions exchange interaction.
4. Ortherwise, the luminescence of Eu~(3+) in different host was deduced. Eu~(3+) -doped (Y_xLa_(1-x))_(0.95)Eu_(0.05)PO_4 and (La_xGd_(1-x))_(0.95_Eu_(0.05)PO_4 phosphors were prepared by a facile co-precipitation method. It is found that (La, Gd) PO_4:Eu~(3+) phosphors have the same crystal structure as LaPO_4:Eu~(3+), which is monoclinic with a little different lattice parameters. In the case of (La, Y) PO_4:Eu~(3+) phosphors, however, the gradual change from monoclinic to tetragonal structure of host lattice was observed as the amount of Y ion increased. Finally, we investigate (Y_xLa_(1-x))_(0.95)Eu_(0.05)PO_4 and (La_xGd_(1-x)) _(0.95)Eu_(0.05)PO_4 phosphor samples ~5D_0→~7F_1 under the source of excitation at different excitation and the emission intensity changes of X values, results showed that (Y_xLa_(1-x))_(0.95)Eu_(0.05)PO_4, with the addition of Y~(3+), the first increase in emission intensity in the X = 0.5 at the maximum, and then decrease. Then (La_xGd_(1-x)) 0.95Eu0.05PO_4 first emission intensity of samples with increasing concentrations of Gd3 + and enhanced in the X = 0.5 at maximum, and then with the Gd~(3+) concentration further increased, emission intensity started to decline, that is, quenching concentration of X = 0.5, show that the Gd~(3+) to Eu~(3+) has a significant energy transfer. Consequently, it was found that Gd or Y ions in orange-emitting LaPO_4:Eu~(3+) phosphor affected the site symmetry around Eu~(3+) ion, which influenced the PL intensity and PL spectra of Eu~(3+)-activated orthophosphate phosphors. The 5D0→7F1 emission intensity of (Y_xLa_(1-x)) _(0.95)Eu_(0.05)PO_4 phosphor samples is increased by 70% than LaPO_4: Eu intensity, while emission intensity of (LaxGd1-x) _(0.95)Eu_(0.05)PO_4 phosphor samples is increased 30% than LaPO_4: Eu.
5. In order to study the energy of Ce~(3+) to Tb~(3+) in YPO_4, co- precipitation was applied as the method to attain the nanosized luminescent grains YPO_4: Ce~(3+), YPO_4: Tb~(3+) and YPO_4: Ce / Tb, the doped Re~(3+) and the calcination temperature on the structure to determine the phase transition temperature was studied . The results show that with the increasing of heat treatment temperature, the crystallization of the product increased, but the particle size does not grow significantly, and the particles,non-aggregation and 20 -100 nm size. The luminescence properties of Ce~(3+)-doped YPO_4 samples with ~5d→~2F_(5/2) and ~5d→~2F_(7/2) transitions have broad band, its excitation and emission spectra are broad band spectrum; Tb~(3+)-doped YPO_4 samples under the UV excitation, the emissioon spectra of samples is is divided into two parts, represents the 4f–5d transition of Tb~(3+) and the 4f– 4f transition of Tb~(3+). The emissions from Tb doped YPO_4 mainly result from the transitions of ~5D_3 and ~5D_4 to ~7F_J (where J = 1- 6). With an increase of Tb concentration, the emissions from ~5D_3 to ~7F_J level are quenched gradually by the cross relaxation process; For Ce~(3+) and Tb~(3+) co-doped YPO_4 sample, as monitoring the emission of Tb~(3+) at 542 nm, the strong allowed f– d transitions in the 250 nm ~ 290 nm of Ce~(3+) and the weak forbidden f–f transitions of Tb~(3+) ions were observed, maximum excitation peak cemtered at 272 nm, demonstrated the phenomenon of blue shift of spectral peaks, which is more conducive to Ce~(3+)→Tb~(3+) energy transfer. Under 272 nm excitation, the emission spectrum has four emission peaks for 490 nm, 542 nm, 589 nm, 626 nm, attributed to Tb~(3+) the ~5D_4→~7F_J (J = 6, 5, 4, 3) transitions launch, which launched the strongest transition for the ~5D_4→~7F_5, there is no characteristic of Ce~(3+) emission peaks appeared, show that the Ce~(3+) ion effectively sensitized luminescence of Tb~(3+). With the increase in concentration, the ~5D_4→~7F_5 increase in luminous intensity, Ce~(3+) doping concentration of 4 percent of the time in the emission intensity of the strongest, Ce~(3+) to increase the amount of doping, the luminescence intensity decreased. The energy transfer process, energy transfer efficiency, and the dynamic process of Ce~(3+) and Tb~(3+). The results showed that the effective, energy transfer efficiency of codoping YPO_4 material exists in the Ce~(3+) to Tb~(3+) energy transfer is 70%.
6. Lanthanide orthophosphate 1D nanostructures with different crystalline phases and morphologies have been successfully synthesized using a hydrothermal method under mild conditions. It has been shown that the obtained LaPO_4 and GdPO_4 have a monoclinic and hexagonal structure, while YPO_4 exists in the tetragonal structure. When CTAB after accession, GdPO_4 the structure into a monoclinic structure, while YPO_4 the structure into a hexagonal structure。Irregularly LnPO_4 (Ln = La, Gd) nanorods with diameters of 50– 100 nm and lengths ranging from several hundreds of nanometres to several micrometres were obtained. The FE-SEM also indicates that the presence of CTAB can also promote oriented growth of the hexagonal and tetragonal structure. The possible growth mechanism of LnPO_4 (Ln = La, Gd, Y) with CTAB nanomaterial was explored. A study of the photoluminescence in Eu~(3+) and Tb~(3+)-doped lanthanide phosphates has shown that the optical properties of these nanophosphors are strongly dependent on their crystal structures and morphologies. It was indicating the possibility of modiyfing their optical properties by structural design. These Re~(3+)-doped rare-earth phosphate can also change the optical properties of other rare earth elements, and is expected to fluorescent light, UV excitation of the new plasma display devices, as well as other important biological fluorescent labeling technology has been applied.
引文
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[1]肖林久,孙彦彬,邱关明等,纳米稀土发光材料的研究进展[J].稀土, 2002, 23 (4) : 46.
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