稀土掺杂微纳发光材料的生长机制与光谱学性质研究
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摘要
稀土掺杂发光材料在照明、显示、激光、生物传感及防伪等诸多领域都有着广泛的应用前景。特别是固态照明光源在船只、舰艇及潜艇等载运工具上的应用可以大大减少能源消耗,提高载运工具的续航能力。随着纳米技术的发展,低维纳米结构材料呈现出特殊的光、电、磁和机械性能。因此,低维纳米结构材料在纳米器件和功能材料等诸多领域具有潜在的应用前景。众所周知,这些性质受纳米材料的结构、形貌和尺寸影响很大。纳米结构材料的形貌和尺寸对其物理及化学性质的影响成为了当前热门研究课题。因此,实现这类材料的可控合成具有十分重要的理论和现实意义。本文采用不同的化学方法合成了不同体系的稀土掺杂微纳米荧光材料,并对其形成过程与发光机理进行了详细地研究。主要研究内容如下。
(1)采用超声化学法合成了3D结构的CaWO4:Tb3+微米球。XRD与SEM结果表明,每个微米球的表面非常粗糙,包含了许多小的纳米粒子。我们对微球生长过程进行了研究,结果发现3D结构的CaWO4:Tb3+微米球是由纺锤粒子组装而成的,而且在组装过程中PEG-600对微球的形成发挥着重要的作用。在紫外光激发下,CaWO4:Tb3+微米球展现出较强的绿光发射,并且观察到了CaWO4:Tb3+微米球中W042-与Tb3+之间及Tb3+的5D3及5D4能级间的能量传递过程。通过发光动力学研究证明了Tb3+的5D3能级间能量传递的机理为电偶极-电偶极相互租用。
(2)采用微波水热法合成了NaY(WO4)2:Eu3+微米花,样品的XRD及SEM结果证实所得到的产物为纯相NaY(WO4)2:Eu3+。另外,实验发现一定温度的退火处理对产物的形貌基本上不产生影响。我们对NaY(WO4)2:Eu3+微米花的生长过程进行了研究,发现这种微米花是由许多纳米片组装而成的。详细研究了NaY(WO4)2:Eu3+微米花的光谱性质及温度猝灭发光机理,结果证实Crossover过程是Eu3+温度猝灭的主要机理。
(3)通过一步水热法直接合成了柿饼状NaLa(WO4)2:Eu3+,Tb3+微晶。XRD与SEM结果表明Na3Cit在柿饼状NaLa(WO4)2:Eu3+,Tb3+形成过程中起着重要的作用。在柿饼状NaLa(WO4)2:Eu3+,Tb3+微晶中,观察到Tb3+到Eu3+的能量传递过程,并且随着Eu3+离子浓度的增加,这种能量传递效率随之增加,并且样品的发光颜色也随之能够被有效地调节。
(4)采用共沉淀法合成了Eu3+及Dy3+掺杂的Y2(MoO4)3微米花。SEM结果表明Y2(MoO4)3微米花是由许多纳米片组装而成的,而且在合成过程中β-环糊精能够有效调节Y2(MoO4)3微米花的尺寸及形貌均匀性。因此,这个实验也建立了一种无机微纳米材料形貌可控的合成方法。最后,对上述两个样品中Dy3+及Eu3+发光性质进行了研究,并发现Dy3+离子间及Eu3+离子间能量传递分别为电偶极-电偶极相互作用及交换相互作用类型。
(5)采用共沉淀法合成了La2(MoO4)3:Eu3+纳米粒子。XRD与SEM结果证实我们制备的La2(MoO4)3:Eu3+纳米粒子晶体结构为四方相,且平均粒径约为88.5nm。我们研究了La2(MoO4)3:Eu3+;纳米粒子的电-声子耦合性质,发现La2(MoO4)3的最大声子能量约为1900cm-1,而且Eu3+与La2(MoO4)3基质电-声子相互作用为弱耦合体系。通过对Eu3+浓度猝灭的分析,证明Eu3+浓度猝灭机理为自猝灭过程。我们建立了一种粉体样品中稀土离子光学跃迁计算的方法。在这个方法中,我们不仅能够获得稀土离子Eu3+的J-O参数,也能够估计出基质材料的折射率。
(6)采用溶剂热法合成了YF3:Tb3+,Eu3+微纳米晶。通过控制反应条件,能够得到均匀的三明治结构的YF3:Tb3+,Eu3+亚微米晶。通过对其生长过程的研究,发现EG在三明治结构的YF3:Tb3+,Eu3+亚微米晶的生长过程中起到溶剂与结构导向双重作用。最后,我们详细研究了三明治结构的YF3:Tb3+,Eu3+亚微米晶的发光性质,结果证实YF3:Tb3+,Eu3+亚微米晶Tb3+到Eu3+的能量传递机理为电偶极-电偶极相互作用。
(7)采用水热法合成了正交相EuF3亚微米球。通过在合成过程中引入离子半径较大的稀土离子,观察到EuF3晶体发生了由正交相到六方相的相变过程。而且在相变的过程中,导致产物形貌组装程度及粒径均随着稀土离子半径的增大或浓度的增加而显著降低。我们认为导致EuF3相变的原因是由于半径较大的稀土离子能够有效降低正交相到六方相相变所需克服的势垒。另外,相变也导致了EuF3荧光发射的增强。因此,这也将提供一种新的纳米晶材料制备及改性的方法。
(8)以YF3:Er3+,Yb3+亚微米纺锤为前驱体,采用水热法合成了NaYF4:Er3+,Yb3+微米管。通过改变反应时间,我们观察到了NaYF4由立方相到六方相的相变过程。在980nm红外激光激发下六方相NaYF4:Er3+,Yb3+微米管的上转换强度约是其立方相的10倍,并且所有的上转换过程均是双光子过程。
(9)以Na3Cit为金属离子络合试剂,采用水热法合成了六方相NaEuF4微纳米晶。通过改变反应体系的pH值及Na3Cit/Eu3+的摩尔比,获得了不同形貌的NaEuF4微纳米晶,并对不同反应条件下六方相NaEuF4微纳米晶形成过程也进行了详细的分析。在394nm激发下,观察到了六方相NaEuF4亚微米球随粒径的减小而荧光增强现象。造成这种现象的原因可能是由于Eu3+间或Eu3+到其它猝灭中心的能量传递被阻断。
(10)通过共沉淀法合成了不同粒径的GdVO4:Dy3+微/纳米粒子。XRD结果表明GdVO4:Dy3+;纳米粒子具有更加扭曲的晶体结构。通过对其浓度猝灭机理的分析,发现Dy3+在纳米粒子中具有较高的掺杂浓度,而且此时Dy3+之间长程相互作用被阻断。除此之外,Dy3+在纳米粒子中具有较长的荧光寿命,导致这种现象的原因可能是由于纳米粒子空间填充率不同所致。
(11)采用离子液体辅助水热法合成了轮胎状YBO3:Eu3+纳米结构微球。通过改变体系的pH值,实现了YBO3:Eu3+微纳米晶的定向生长及形貌的控制。研究发现[MOIM]Cl离子液体在YBO3:Eu3+纳米结构微球的生长过程中起到溶剂及软模板的作用。通过比较YBO3:Eu3+纳米结构微球与相应体材料中Eu3+的光谱,发现YBO3:Eu3+纳米结构微球中Eu-O电荷迁移带发生移动,而且改变激发波长,YBO3:Eu3+纳米结构微球中Eu3+的5Do→7F2跃迁几率增加。
Rare earth doped luminescent materials have wide potential applications in the fields of lighting, display, laser, biosensor, anti-counterfeiting, etc. Especially, the solid state lighting resource employed in the vehicles of ships, naval vessels and submarines can reduce the consumption of energy and improve the self-supportability of vehicles efficiently. With the development of nanotechnology, low-dimensional nanostructured materials have sparked a worldwide interest due to their unique electronic, optical, and mechanical properties and their potential applications in nanodevices and functional materials. It is well known that these properties can be influenced greatly by the structure, morphology and size of nanomaterials. Therefore, the controlled syntheses of nanomaterials are very important for both fundamental research and practical applications. In this thesis, we synthesized different rare earth ions doped micro-/nano-materials through various chemical methods and studied their growth process and luminescent mechanism. The main contents in this thesis are as follows.
(1)3D structured CaWO4:Tb3+microspheres were prepared via a sonochemical route. XRD and SEM results displayed that the surface of each microsphere is very rough and contains a lot of small nanoparticles. The formation mechanism of3D structured CaWO4:Tb3+microspheres were studied. It was found that3D structured CaWO4:Tb3+microspheres are assembled by spindles. Moreover, PEG-600plays an important role in the formation of microsphere. Under UV excitation,3D structured CaWO4:Tb3+microspheres exhibit intense green emission. The energy transfer processes from WO42-to Tb3+and between5D3and5D4levels of Tb3+ions were observed in the3D structured CaWO4:Tb3+microspheres. It was also proved that electric dipole-dipole interation is the main mechanism for energy transfer between5D3and5D4levels of Tb3+.
(2) NaY(WO4)2:Eu3+microflowers were prepared via microwave-assisted hydrothermal process. XRD and SEM results showed that the product is pure NaY(WO4)2:Eu3+. Moreover, the final morphology of product was influenced slightly by calcination process. The growth process of NaY(WO4)2:Eu3+microflowers were studied. It was found that the NaY(WO4)2:Eu3+microflowers are assembled by many nanoflakes. The luminescent properties of NaY(WO4)2:Eu3+microflowers were studied in details. The crossover process is responsible for fluorescent quenching induced by high temperature.
(3) Persimmon-like NaLa(WO4)2:Eu3+,Tb3+microcrystals were prepared via one-pot hydrothermal process. XRD and SEM results showed that Na3Cit plays an important role in the formation of persimmon-like NaLa(WO4)2:Eu3+,Tb3+microcrystals. The energy transfer from Tb3+to Eu3+can be observed in the persimmon-like NaLa(WO4)2:Eu3+,Tb3+microcrystals. Moreover, with the increase of Eu3+concentration, the energy transfer efficiency increases and the luminescent color can be tuned efficiently.
(4) Eu3+and Dy3+doped Y2(MoO4)3microflowers were prepared by co-precipitation method. SEM results revealed that Y2(MoO4)3microflowers are assembled by many nanoflakes. Moreover,β-cyclodextrin can control the size and morphology of the products in the synthesis process. Therefore, β-cyclodextrin assisted co-precipitation reaction may be an efficient approach for preparation of inorganic micro-/nano-materials with special morphologies. Finally, it was confirmed that the energy transfer mechanisms in Eu3+and Dy3+single doped molybdate phosphors are exchange and electric dipole-dipole interaction, respectively.
(5) La2(MoO4)3:Eu3+nanoparticles were prepared via co-precipitation method. XRD and SEM results showed the crystal structure of the resultant La2(MoO4)3:Eu3+nanoparticles is tetragonal phase. Moreover, the average size of La2(MoO4)3:Eu3+nanoparticles is about88.5nm. The electron-phonon coupling properties were studied. It is found that the maximum phonon energy of La2(MoO4)3:Eu3+nanoparticles is about1900cm-1. It was also confirmed that the mechanism of concentration quenching for Eu3+is a self-quenching process. Additionally, a new route for J-O parameters calculation was developed, in which the refractive index of host might be estimated.
(6) YF3:Tb3+,Eu3+micro-/nano-crystals were prepared through a solvothermal process, and the uniform sandwich-structural rhombus-like YF3:Tb3+,Eu3+particles could be obtained by well controling the reaction parameters. The growth mechanism of sandwich-structural rhombus-like YF3:Tb3+,Eu3+particles were studied. It was found that EG plays double functions in the formation of sandwich-structural rhombus-like YF3:Tb3+,Eu3+particles. Finally, the luminescent properties of sandwich-structural rhombus-like YF3+:Tb3+,Eu3+were studied. The energy transfer from Tb3+to Eu3+in the sandwich-structural rhombus-like YF3:Tb3+,Eu3+particles was conformed to be electric dipole-dipole interaction.
(7) Orthorhombic EuF.3submicrospheres were prepared via a hydrothermal process. The phase transition of EuF3phosphor from orthorhombic phase to hexagonal one was observed when rare earth ions with larger ionic radius were introduced into the reaction system. Moreover, in the phase transition process it was found that the size and assembling degree of the product decreased with the increase of rare earth ions concentration or radius. The rare earth ions-induced phase transition was attributed to the decrease of energy from orthorhombic phase to hexagonal one. Meanwhile, the luminescent enhancement can be observed.
(8) NaYF4:Er3+,Yb3+microtubes were prepared through a hydrothermal process with YF3:Er3+,Yb3+submicrotubes as precursor. The phase transition process of NaYF4from cubic to hexagonal was observed with the increase of reaction time. Under980nm exaction, the uponversion luminescent intensities of hexagonal NaYF4:Er3+,Yb3+microtubes is10times as that of the cubic sample. It was confirmed that both the green and red upconversion emissions are two-photon process.
(9) Hexagonal NaEuF4micro-/nano-crystals were prepared via a hydrothermal process in the presence of Na3Cit. Different morphologies of hexagonal NaEuF4micro-/nano-crystals were obtained by changing the pH value and Na3Cit/Eu3+molar ratio. The formation mechanism of hexagonal NaEuF4micro-/nano-crystals was studied. Under394nm excitation, it was found that the luminescent intensity of hexagonal NaEuF4micro-/nano-crystals increased with the decrease of size of product, which was attributed to the fact that the energy transfer from Eu3+to quenching center was hindered.
(10) Bulk and nanosized GdVO4:Dy3+phosphors were prepared via a simple co-precipitation process. The characteristic emissions from4F9/2level of Dy3+in the bulk and nanosized samples were observed. It was found that electric dipole-dipole interaction is hindered in the nanosized samples based on the analysis of the dependence of luminescent intensity on concentration. The decay time of the4F9/2level in the nanosized GdVO4:2mol%Dy3+sample is determined to be longer than that in the0.3mol%Dy3+doped bulk sample. Moreover, the fluorescent lifetime of this level in the nanosized sample is strongly dependent on the index of refraction of the medium surrounding the nanoparticles and a0.68filling factor is obtained. The intrinsic radiative lifetimes and internal quantum efficiencies of the4F9/2level of Dy3+in the nanosized and bulk samples were obtained, which indicated that the internal quantum efficiency of nanosized sample was higher than that of the bulk sample.
(11) Three dimensional (3D) architectures YBO3phosphors were prepared via an ionic liquid assisted hydrothermal process and characterized by XRD, FE-SEM and photoluminescence (PL). It was found that the pH value and ionic liquid played an important role on the morphology of products. Self-assembly evolution of microblocks and Ostwald ripening process were assigned to the possible formation mechanism for the tyre-like YBO3microspheres based on the analysis of time-dependent experiments. Compared with corresponding bulk, the tyre-like YBO3:5mol%Eu3+microspheres demonstrated a red shift of the charge transfer band (CTB) with a long excitation tail at the long wavelength side of the CTB, and high improved chromaticity in the spectra. Two kinds Eu3+environments in the tyre-like sample, namely, interior and outside Eu3+, were found by exciting the samples at different excitation wavelengths. Finally, fluorescent decays and Judd-Ofelt (J-O) theory were utilized for analysis of local crystal environments around Eu3+ions in the tyre-like and bulk phosphors.
(1)采用超声化学法合成了3D结构的CaWO4:Tb3+微米球。XRD与SEM结果表明,每个微米球的表面非常粗糙,包含了许多小的纳米粒子。我们对微球生长过程进行了研究,结果发现3D结构的CaWO4:Tb3+微米球是由纺锤粒子组装而成的,而且在组装过程中PEG-600对微球的形成发挥着重要的作用。在紫外光激发下,CaWO4:Tb3+微米球展现出较强的绿光发射,并且观察到了CaWO4:Tb3+微米球中W042-与Tb3+之间及Tb3+的5D3及5D4能级间的能量传递过程。通过发光动力学研究证明了Tb3+的5D3能级间能量传递的机理为电偶极-电偶极相互租用。
(2)采用微波水热法合成了NaY(WO4)2:Eu3+微米花,样品的XRD及SEM结果证实所得到的产物为纯相NaY(WO4)2:Eu3+。另外,实验发现一定温度的退火处理对产物的形貌基本上不产生影响。我们对NaY(WO4)2:Eu3+微米花的生长过程进行了研究,发现这种微米花是由许多纳米片组装而成的。详细研究了NaY(WO4)2:Eu3+微米花的光谱性质及温度猝灭发光机理,结果证实Crossover过程是Eu3+温度猝灭的主要机理。
(3)通过一步水热法直接合成了柿饼状NaLa(WO4)2:Eu3+,Tb3+微晶。XRD与SEM结果表明Na3Cit在柿饼状NaLa(WO4)2:Eu3+,Tb3+形成过程中起着重要的作用。在柿饼状NaLa(WO4)2:Eu3+,Tb3+微晶中,观察到Tb3+到Eu3+的能量传递过程,并且随着Eu3+离子浓度的增加,这种能量传递效率随之增加,并且样品的发光颜色也随之能够被有效地调节。
(4)采用共沉淀法合成了Eu3+及Dy3+掺杂的Y2(MoO4)3微米花。SEM结果表明Y2(MoO4)3微米花是由许多纳米片组装而成的,而且在合成过程中β-环糊精能够有效调节Y2(MoO4)3微米花的尺寸及形貌均匀性。因此,这个实验也建立了一种无机微纳米材料形貌可控的合成方法。最后,对上述两个样品中Dy3+及Eu3+发光性质进行了研究,并发现Dy3+离子间及Eu3+离子间能量传递分别为电偶极-电偶极相互作用及交换相互作用类型。
(5)采用共沉淀法合成了La2(MoO4)3:Eu3+纳米粒子。XRD与SEM结果证实我们制备的La2(MoO4)3:Eu3+纳米粒子晶体结构为四方相,且平均粒径约为88.5nm。我们研究了La2(MoO4)3:Eu3+;纳米粒子的电-声子耦合性质,发现La2(MoO4)3的最大声子能量约为1900cm-1,而且Eu3+与La2(MoO4)3基质电-声子相互作用为弱耦合体系。通过对Eu3+浓度猝灭的分析,证明Eu3+浓度猝灭机理为自猝灭过程。我们建立了一种粉体样品中稀土离子光学跃迁计算的方法。在这个方法中,我们不仅能够获得稀土离子Eu3+的J-O参数,也能够估计出基质材料的折射率。
(6)采用溶剂热法合成了YF3:Tb3+,Eu3+微纳米晶。通过控制反应条件,能够得到均匀的三明治结构的YF3:Tb3+,Eu3+亚微米晶。通过对其生长过程的研究,发现EG在三明治结构的YF3:Tb3+,Eu3+亚微米晶的生长过程中起到溶剂与结构导向双重作用。最后,我们详细研究了三明治结构的YF3:Tb3+,Eu3+亚微米晶的发光性质,结果证实YF3:Tb3+,Eu3+亚微米晶Tb3+到Eu3+的能量传递机理为电偶极-电偶极相互作用。
(7)采用水热法合成了正交相EuF3亚微米球。通过在合成过程中引入离子半径较大的稀土离子,观察到EuF3晶体发生了由正交相到六方相的相变过程。而且在相变的过程中,导致产物形貌组装程度及粒径均随着稀土离子半径的增大或浓度的增加而显著降低。我们认为导致EuF3相变的原因是由于半径较大的稀土离子能够有效降低正交相到六方相相变所需克服的势垒。另外,相变也导致了EuF3荧光发射的增强。因此,这也将提供一种新的纳米晶材料制备及改性的方法。
(8)以YF3:Er3+,Yb3+亚微米纺锤为前驱体,采用水热法合成了NaYF4:Er3+,Yb3+微米管。通过改变反应时间,我们观察到了NaYF4由立方相到六方相的相变过程。在980nm红外激光激发下六方相NaYF4:Er3+,Yb3+微米管的上转换强度约是其立方相的10倍,并且所有的上转换过程均是双光子过程。
(9)以Na3Cit为金属离子络合试剂,采用水热法合成了六方相NaEuF4微纳米晶。通过改变反应体系的pH值及Na3Cit/Eu3+的摩尔比,获得了不同形貌的NaEuF4微纳米晶,并对不同反应条件下六方相NaEuF4微纳米晶形成过程也进行了详细的分析。在394nm激发下,观察到了六方相NaEuF4亚微米球随粒径的减小而荧光增强现象。造成这种现象的原因可能是由于Eu3+间或Eu3+到其它猝灭中心的能量传递被阻断。
(10)通过共沉淀法合成了不同粒径的GdVO4:Dy3+微/纳米粒子。XRD结果表明GdVO4:Dy3+;纳米粒子具有更加扭曲的晶体结构。通过对其浓度猝灭机理的分析,发现Dy3+在纳米粒子中具有较高的掺杂浓度,而且此时Dy3+之间长程相互作用被阻断。除此之外,Dy3+在纳米粒子中具有较长的荧光寿命,导致这种现象的原因可能是由于纳米粒子空间填充率不同所致。
(11)采用离子液体辅助水热法合成了轮胎状YBO3:Eu3+纳米结构微球。通过改变体系的pH值,实现了YBO3:Eu3+微纳米晶的定向生长及形貌的控制。研究发现[MOIM]Cl离子液体在YBO3:Eu3+纳米结构微球的生长过程中起到溶剂及软模板的作用。通过比较YBO3:Eu3+纳米结构微球与相应体材料中Eu3+的光谱,发现YBO3:Eu3+纳米结构微球中Eu-O电荷迁移带发生移动,而且改变激发波长,YBO3:Eu3+纳米结构微球中Eu3+的5Do→7F2跃迁几率增加。
Rare earth doped luminescent materials have wide potential applications in the fields of lighting, display, laser, biosensor, anti-counterfeiting, etc. Especially, the solid state lighting resource employed in the vehicles of ships, naval vessels and submarines can reduce the consumption of energy and improve the self-supportability of vehicles efficiently. With the development of nanotechnology, low-dimensional nanostructured materials have sparked a worldwide interest due to their unique electronic, optical, and mechanical properties and their potential applications in nanodevices and functional materials. It is well known that these properties can be influenced greatly by the structure, morphology and size of nanomaterials. Therefore, the controlled syntheses of nanomaterials are very important for both fundamental research and practical applications. In this thesis, we synthesized different rare earth ions doped micro-/nano-materials through various chemical methods and studied their growth process and luminescent mechanism. The main contents in this thesis are as follows.
(1)3D structured CaWO4:Tb3+microspheres were prepared via a sonochemical route. XRD and SEM results displayed that the surface of each microsphere is very rough and contains a lot of small nanoparticles. The formation mechanism of3D structured CaWO4:Tb3+microspheres were studied. It was found that3D structured CaWO4:Tb3+microspheres are assembled by spindles. Moreover, PEG-600plays an important role in the formation of microsphere. Under UV excitation,3D structured CaWO4:Tb3+microspheres exhibit intense green emission. The energy transfer processes from WO42-to Tb3+and between5D3and5D4levels of Tb3+ions were observed in the3D structured CaWO4:Tb3+microspheres. It was also proved that electric dipole-dipole interation is the main mechanism for energy transfer between5D3and5D4levels of Tb3+.
(2) NaY(WO4)2:Eu3+microflowers were prepared via microwave-assisted hydrothermal process. XRD and SEM results showed that the product is pure NaY(WO4)2:Eu3+. Moreover, the final morphology of product was influenced slightly by calcination process. The growth process of NaY(WO4)2:Eu3+microflowers were studied. It was found that the NaY(WO4)2:Eu3+microflowers are assembled by many nanoflakes. The luminescent properties of NaY(WO4)2:Eu3+microflowers were studied in details. The crossover process is responsible for fluorescent quenching induced by high temperature.
(3) Persimmon-like NaLa(WO4)2:Eu3+,Tb3+microcrystals were prepared via one-pot hydrothermal process. XRD and SEM results showed that Na3Cit plays an important role in the formation of persimmon-like NaLa(WO4)2:Eu3+,Tb3+microcrystals. The energy transfer from Tb3+to Eu3+can be observed in the persimmon-like NaLa(WO4)2:Eu3+,Tb3+microcrystals. Moreover, with the increase of Eu3+concentration, the energy transfer efficiency increases and the luminescent color can be tuned efficiently.
(4) Eu3+and Dy3+doped Y2(MoO4)3microflowers were prepared by co-precipitation method. SEM results revealed that Y2(MoO4)3microflowers are assembled by many nanoflakes. Moreover,β-cyclodextrin can control the size and morphology of the products in the synthesis process. Therefore, β-cyclodextrin assisted co-precipitation reaction may be an efficient approach for preparation of inorganic micro-/nano-materials with special morphologies. Finally, it was confirmed that the energy transfer mechanisms in Eu3+and Dy3+single doped molybdate phosphors are exchange and electric dipole-dipole interaction, respectively.
(5) La2(MoO4)3:Eu3+nanoparticles were prepared via co-precipitation method. XRD and SEM results showed the crystal structure of the resultant La2(MoO4)3:Eu3+nanoparticles is tetragonal phase. Moreover, the average size of La2(MoO4)3:Eu3+nanoparticles is about88.5nm. The electron-phonon coupling properties were studied. It is found that the maximum phonon energy of La2(MoO4)3:Eu3+nanoparticles is about1900cm-1. It was also confirmed that the mechanism of concentration quenching for Eu3+is a self-quenching process. Additionally, a new route for J-O parameters calculation was developed, in which the refractive index of host might be estimated.
(6) YF3:Tb3+,Eu3+micro-/nano-crystals were prepared through a solvothermal process, and the uniform sandwich-structural rhombus-like YF3:Tb3+,Eu3+particles could be obtained by well controling the reaction parameters. The growth mechanism of sandwich-structural rhombus-like YF3:Tb3+,Eu3+particles were studied. It was found that EG plays double functions in the formation of sandwich-structural rhombus-like YF3:Tb3+,Eu3+particles. Finally, the luminescent properties of sandwich-structural rhombus-like YF3+:Tb3+,Eu3+were studied. The energy transfer from Tb3+to Eu3+in the sandwich-structural rhombus-like YF3:Tb3+,Eu3+particles was conformed to be electric dipole-dipole interaction.
(7) Orthorhombic EuF.3submicrospheres were prepared via a hydrothermal process. The phase transition of EuF3phosphor from orthorhombic phase to hexagonal one was observed when rare earth ions with larger ionic radius were introduced into the reaction system. Moreover, in the phase transition process it was found that the size and assembling degree of the product decreased with the increase of rare earth ions concentration or radius. The rare earth ions-induced phase transition was attributed to the decrease of energy from orthorhombic phase to hexagonal one. Meanwhile, the luminescent enhancement can be observed.
(8) NaYF4:Er3+,Yb3+microtubes were prepared through a hydrothermal process with YF3:Er3+,Yb3+submicrotubes as precursor. The phase transition process of NaYF4from cubic to hexagonal was observed with the increase of reaction time. Under980nm exaction, the uponversion luminescent intensities of hexagonal NaYF4:Er3+,Yb3+microtubes is10times as that of the cubic sample. It was confirmed that both the green and red upconversion emissions are two-photon process.
(9) Hexagonal NaEuF4micro-/nano-crystals were prepared via a hydrothermal process in the presence of Na3Cit. Different morphologies of hexagonal NaEuF4micro-/nano-crystals were obtained by changing the pH value and Na3Cit/Eu3+molar ratio. The formation mechanism of hexagonal NaEuF4micro-/nano-crystals was studied. Under394nm excitation, it was found that the luminescent intensity of hexagonal NaEuF4micro-/nano-crystals increased with the decrease of size of product, which was attributed to the fact that the energy transfer from Eu3+to quenching center was hindered.
(10) Bulk and nanosized GdVO4:Dy3+phosphors were prepared via a simple co-precipitation process. The characteristic emissions from4F9/2level of Dy3+in the bulk and nanosized samples were observed. It was found that electric dipole-dipole interaction is hindered in the nanosized samples based on the analysis of the dependence of luminescent intensity on concentration. The decay time of the4F9/2level in the nanosized GdVO4:2mol%Dy3+sample is determined to be longer than that in the0.3mol%Dy3+doped bulk sample. Moreover, the fluorescent lifetime of this level in the nanosized sample is strongly dependent on the index of refraction of the medium surrounding the nanoparticles and a0.68filling factor is obtained. The intrinsic radiative lifetimes and internal quantum efficiencies of the4F9/2level of Dy3+in the nanosized and bulk samples were obtained, which indicated that the internal quantum efficiency of nanosized sample was higher than that of the bulk sample.
(11) Three dimensional (3D) architectures YBO3phosphors were prepared via an ionic liquid assisted hydrothermal process and characterized by XRD, FE-SEM and photoluminescence (PL). It was found that the pH value and ionic liquid played an important role on the morphology of products. Self-assembly evolution of microblocks and Ostwald ripening process were assigned to the possible formation mechanism for the tyre-like YBO3microspheres based on the analysis of time-dependent experiments. Compared with corresponding bulk, the tyre-like YBO3:5mol%Eu3+microspheres demonstrated a red shift of the charge transfer band (CTB) with a long excitation tail at the long wavelength side of the CTB, and high improved chromaticity in the spectra. Two kinds Eu3+environments in the tyre-like sample, namely, interior and outside Eu3+, were found by exciting the samples at different excitation wavelengths. Finally, fluorescent decays and Judd-Ofelt (J-O) theory were utilized for analysis of local crystal environments around Eu3+ions in the tyre-like and bulk phosphors.
引文
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