稀土掺杂钙钛矿型复合氧化物的制备及其发光性能研究
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摘要
稀土离子因其具有稳定的物理化学性质、丰富的能级结构和较长的能级寿命，可作为发光中心掺杂到适当基质材料中，在近紫外或蓝光激发下，得到丰富的光致发光性质。稀土发光材料是一类重要的稀土功能材料，其中稀土掺杂氧化物发光材料已广泛应用于照明和显示技术等领域。随着稀土发光基础研究的不断深入和科学技术的发展，人们对发光材料的性能提出越来越高的要求。由于稀土离子具有独特的4f电子组态、4f5d电子组态及电荷迁移带结构，使其发光特性与基质材料的组成、结构等性质有很强的依赖关系，因此，寻找新型、有利于稀土离子掺杂的基质材料成为提高荧光性能的一个重要研究方向。
钙钛矿型复合氧化物的结构稳定且性能优异，其电学、磁学和催化等性质备受关注。近年来，人们开始对稀土掺杂钙钛矿型复合氧化物的光学性质产生越来越浓厚的兴趣。另外，钙钛矿结构氧化物所包含的晶体种类十分丰富，并且允许大量离子替换，因此稀土掺杂钙钛矿型氧化物的光学性质极具研究价值和应用前景。
本论文研究了一系列稀土掺杂钙钛矿型复合氧化物发光材料的制备方法及其发光性能。通过溶胶-凝胶法和高温固相法制备了一系列稀土离子掺杂钙钛矿型复合氧化物，并研究了掺杂离子（以Eu~(3+)为主）在不同钙钛矿基质中的发光性质。通过室温荧光激发和发射光谱、荧光衰减特性分析及高分辨格位选择性激光光谱等测试手段，对合成的样品进行表征分析并总结实验数据，结合部分理论计算，研究了稀土离子发光性能与基质组成和结构的关系。论文的具体研究内容如下：
第一部分：Eu~(3+)离子掺杂LnAlO_3(Ln=Gd, La)荧光粉的制备及光谱分析。
LnAlO_3(Ln=La, Gd)是典型的A~(3+)B~(3+)O_3钙钛矿型复合氧化物，我们采用溶胶-凝胶法合成Eu~(3+)离子掺杂LnAlO_3(Ln=La, Gd)荧光粉，通过综合热分析（TG-DSC）和X射线衍射（XRD）来表征其结晶化过程，并且对二者的发光性质进行了较细致地研究。通过较系统地研究掺杂浓度和退火温度对两种材料发光强度的影响，得到最优掺杂浓度及最佳煅烧温度。研究发现，在适当紫外光激发下，GdAlO_3:Eu~(3+)具有较好的红橙光发光亮度，有潜力成为理想的光学显示用红橙色荧光粉。LnAlO_3:Eu~(3+)(Ln=Gd, La)的室温荧光激发谱表明基质结构对Eu~(3+)―O2–电荷迁移能有一定的影响，因此我们根据复杂晶体化学键的介电理论进行理论计算，结合实验数据，研究Eu~(3+)―O~(2–)电荷迁移能与基质化学键的键长、键性的关系。另外，通过进一步测量LnAlO_3:Eu~(3+)(Ln=Gd, La)的室温高分辨格位选择性激光光谱及5D0能级寿命，研究两种基质中Eu~(3+)周围晶场环境和格位分布情况，结果显示Eu~(3+)在LaAlO_3:Eu~(3+)中存在三种不同格位，而在GdAlO_3:Eu~(3+)中仅占据一种格位。
第二部分：CaRlO_3:Ln (R=Zr, Ti; Ln=Pr~(3+), Eu~(3+), Tb~(3+), Tm~(3+), Dy~(3+), Sm~(3+))荧光粉的制备及光谱调控。
CaZrO_3和CaTiO_3都是典型的A2+B4+O_3钙钛矿型复合氧化物，我们采用高温固相法合成CaRlO_3:Ln (R=Zr, Ti; Ln=Pr~(3+), Eu~(3+), Tb~(3+), Tm~(3+), Dy~(3+), Sm~(3+))荧光粉，并对其发光性质进行研究。通过测量室温荧光光谱，对Pr3+/Eu~(3+)在CaZrO_3和CaTiO_3中不同的发光行为进行定性研究；另外，我们进一步研究了改变掺杂稀土离子对CaZrO_3的光谱调控作用，发现CaZrO_3是一种良好的可供稀土离子掺杂的基质材料，在近紫外光或蓝光激发下，通过改变掺杂离子可实现发光颜色调控，有潜力成为新型光学显示用荧光粉基质材料。
第三部分：Eu~(3+)掺杂立方复杂钙钛矿氧化物Ba_3Y_2WO_9的制备及发光性质研究。
前两部分所研究的基质材料属于简单钙钛矿结构氧化物，接下来将对复杂钙钛矿结构A(B′_(2/3)B″_(1/3))O_3型复合氧化物的发光性质进行研究，因为目前对此类型氧化物光学性质的研究是十分有限的。我们采用溶胶-凝胶法合成Eu~(3+)掺杂立方结构的复杂钙钛矿复合氧化物Ba_3Y_2WO_9（Ba(Y_(2/3)W_(1/3))O_3），通过XRD和场发射扫描电镜（FE-SEM）对合成样品的物相及微观形貌进行表征。通过测量Ba_3Y_2WO_9:Eu~(3+)的室温荧光光谱、高分辨格位选择性激光光谱及~5D0能级寿命，研究了Eu~(3+)在该基质中的发光性能和格位分布情况。研究表明Ba_3Y_2WO_9:Eu~(3+)是一种良好的可允许大量稀土离子掺杂（约为30mol%）的红橙色发光材料；Eu~(3+)取代Bs~(2+)和Y~(3+)格位，且其取代Bs~(2+)格位的同时形成电荷补偿缺陷，这种缺陷结构使Eu~(3+)周围晶格环境产生剧烈扰动。
本论文的研究，有助于更好地理解稀土离子的发光行为，丰富对稀土掺杂钙钛矿结构氧化物发光性能的认识，对进一步研究稀土掺杂钙钛矿结构氧化物的光学性质及其实际应用具有一定的科学参考价值。
Rare earth ions have stable physical and chemical properties, abundant levelstructure and longer lifetime.Under proper near UV or blue light excitation, rare earthions can be doped into appropriate host as the activator, to get excellent luminescenceproperties. Rare earth doped phosphors is an important class of function materials,and the rare eath doped oxides phosphors could be widely used in the field ofillumination and displays. With the advance of science and technology, and the basictheoretical study goes deeper and wider, people make higher demand on theluminescence properties of optical materials. The optical properities of rare earth ionsshow strong dependce on the compositon and structure of matrix materials, because oftheir unique4f intraconfiguration,4f5d configuration and the charge transfer bandstructure. Therefore, in the exploration of new phosphors, a selection of new hostmaterials to enhance the optical properties is a major concern.
Perovskite oxides are one of the most studied groups of materials, owing to theirwidely technological applications. In recent years, the optical properties of rareearth-doped perovskie oxides have attracted more and more interest of scientist.Furthermore, an incredibly high versatility of structures and phases with totallydifferent functions can be obtained depending upon the combination of chemicalelements into the formula ABO_3. So the optical properties of rare earth-dopedperovskite composite oxides show well research value and potential applications.
In this thesis, we systematically investigated on the synthesis and opticalproperties of rare earth-doped perovskite composite oxides. We synthesized a serielsof rare-earth-doped-perovskite composite oxides through sol-gel method and high temperature solid state reaction method, study on the optical properties of the rareearth ions (mainly Eu~(3+)) doped in different host materials. The main experimentalresearch includes photoluminescence excitation and emission spectra, concentrationquenching, lifetime and high resolution laser spectra. The experimental data weresummarized, analyzed and followed by partial theoretical calculation and analysis, toinvestigate the relation between composition, structure and luminescent properties.The thesis mainly consists of three parts, as follows:
Firstly, the preparation and analysis of Eu~(3+)-doped LnAlO_3(Ln=Gd, La).
LnAlO_3(Ln=Gd, La) are typical A~(3+)B~(3+)O_3perovskites. In this part, Eu~(3+)-dopedLaAlO_3and GdAlO_3phosphors were synthesized with sol-gel method. Thecrystallization processes of the phosphors were characterized by X-ray diffraction(XRD) and thermogravimetry-differential scanning calorimetry (TG-DSC), and theoptical properties were investigated in details. The influences of doping concentrationand annealing temperature on the luminescent intensity were investigated, and finallywe got the optimal doping concentration and calcining temperature for the twophosphors. Under appropriate UV-radiation, the reddish orange light emitted fromGdAlO_3:Eu~(3+)was brighter than that from LaAlO_3:Eu~(3+). Such a brightly luminescentphosphor could be considered as an ideal optical material for the development of newoptical display systems. As can be seen from the PLE spectra of Eu~(3+)-doped LaAlO_3and GdAlO_3, the CT band energy of Eu~(3+)―O2-was strongly influenced by the hostmaterials. Correspondingly, we calculated the bond lengths and bond covalency ofLa-O and Gd-O based on the chemical bond theory to investigate relations betweenthe CT band energy and bond convalency. Furthermore, the site-selective laserspectroscopy and luminescence decay of Eu~(3+)-doped GdAlO_3and LaAlO_3preparedby sol-gel method have been investigated at room temperature. As can be seen fromthe site-selective excitation spectra in the7F0→5D0region, there were threecrystallographic sites for Eu~(3+)in LaAlO_3:Eu~(3+), and one crystallographic site for Eu~(3+)in GdAlO_3:Eu~(3+).
Secondly, preparation and tunable spectra of CaRlO_3:Ln (R=Zr, Ti; Ln=Pr~(3+), Eu~(3+)),Tb~(3+), Tm~(3+), Dy~(3+), Sm~(3+)).
CaZrO_3and CaTiO_3are typical A2+B4+O_3perovskites. In this part, CaRlO_3:Ln(R=Zr, Ti; Ln=Pr~(3+), Eu~(3+), Tb~(3+), Tm~(3+), Dy~(3+), Sm~(3+)) phosphors were prepared byconventional solid state reaction. We investigated luminescent properties thePr3+/Eu~(3+)-doped CaRlO_3:Ln (R=Zr, Ti) through photoluminescence spectrameasurement, although CaZrO_3and CaTiO_3both possess orthorhombic structure,their luminescent properties were different. Furthermore, the tunable spectra ofCaZrO_3were investigated by changing the doped rare earth ions. As a result, CaZrO_3is a kind of well host materials, under appropriate UV or blue light excitation, CaZrO_3could get tunable color light emission, can be exploited as potential host materials foroptical display systems to get better color light output.
Thirdly, synthesis and investigation of luminescence properties of Eu~(3+)-dopedcubic perovskite Ba_3Y_2WO_9.
In the above two sections, we investigated the optical properties of rare earthdoped simple perovskite oxides. In this part, we focused on the luminescenceproperties of A(B′_(2/3)B″_(1/3))O_3type complex provskiteoxides, and the study on theoptical properties of this kind of provskite oxides is limited at present. Eu~(3+)-dopedcubic Ba_3Y_2WO_9phosphors were synthesized by sol-gel method. The preparedsamples were characterized by XRD and field emission-scanning electron microscopy(FE-SEM). The luminescence excitation emission spectra in the UV region, thesite-selective laser spectra along with luminescence decay were measured in the5D0-7F0region were used to characterize the luminescence properties and the sitedistributions of Eu~(3+)in Ba_3Y_2WO_9. As the result, the Ba_3Y_2WO_9:Eu~(3+)phosphorsexhibit strong orange-red luminescence, and the optimal concentration of Eu~(3+)in thehost of cubic Ba_3Y_2WO_9is30mol%; Eu~(3+)ions replace both theY~(3+)and Bs~(2+)ions,and the Eu~(3+)in Bs~(2+)sites accompanied by a charge-compensating defect leading tothe disordered surrounding.
钙钛矿型复合氧化物的结构稳定且性能优异，其电学、磁学和催化等性质备受关注。近年来，人们开始对稀土掺杂钙钛矿型复合氧化物的光学性质产生越来越浓厚的兴趣。另外，钙钛矿结构氧化物所包含的晶体种类十分丰富，并且允许大量离子替换，因此稀土掺杂钙钛矿型氧化物的光学性质极具研究价值和应用前景。
本论文研究了一系列稀土掺杂钙钛矿型复合氧化物发光材料的制备方法及其发光性能。通过溶胶-凝胶法和高温固相法制备了一系列稀土离子掺杂钙钛矿型复合氧化物，并研究了掺杂离子（以Eu~(3+)为主）在不同钙钛矿基质中的发光性质。通过室温荧光激发和发射光谱、荧光衰减特性分析及高分辨格位选择性激光光谱等测试手段，对合成的样品进行表征分析并总结实验数据，结合部分理论计算，研究了稀土离子发光性能与基质组成和结构的关系。论文的具体研究内容如下：
第一部分：Eu~(3+)离子掺杂LnAlO_3(Ln=Gd, La)荧光粉的制备及光谱分析。
LnAlO_3(Ln=La, Gd)是典型的A~(3+)B~(3+)O_3钙钛矿型复合氧化物，我们采用溶胶-凝胶法合成Eu~(3+)离子掺杂LnAlO_3(Ln=La, Gd)荧光粉，通过综合热分析（TG-DSC）和X射线衍射（XRD）来表征其结晶化过程，并且对二者的发光性质进行了较细致地研究。通过较系统地研究掺杂浓度和退火温度对两种材料发光强度的影响，得到最优掺杂浓度及最佳煅烧温度。研究发现，在适当紫外光激发下，GdAlO_3:Eu~(3+)具有较好的红橙光发光亮度，有潜力成为理想的光学显示用红橙色荧光粉。LnAlO_3:Eu~(3+)(Ln=Gd, La)的室温荧光激发谱表明基质结构对Eu~(3+)―O2–电荷迁移能有一定的影响，因此我们根据复杂晶体化学键的介电理论进行理论计算，结合实验数据，研究Eu~(3+)―O~(2–)电荷迁移能与基质化学键的键长、键性的关系。另外，通过进一步测量LnAlO_3:Eu~(3+)(Ln=Gd, La)的室温高分辨格位选择性激光光谱及5D0能级寿命，研究两种基质中Eu~(3+)周围晶场环境和格位分布情况，结果显示Eu~(3+)在LaAlO_3:Eu~(3+)中存在三种不同格位，而在GdAlO_3:Eu~(3+)中仅占据一种格位。
第二部分：CaRlO_3:Ln (R=Zr, Ti; Ln=Pr~(3+), Eu~(3+), Tb~(3+), Tm~(3+), Dy~(3+), Sm~(3+))荧光粉的制备及光谱调控。
CaZrO_3和CaTiO_3都是典型的A2+B4+O_3钙钛矿型复合氧化物，我们采用高温固相法合成CaRlO_3:Ln (R=Zr, Ti; Ln=Pr~(3+), Eu~(3+), Tb~(3+), Tm~(3+), Dy~(3+), Sm~(3+))荧光粉，并对其发光性质进行研究。通过测量室温荧光光谱，对Pr3+/Eu~(3+)在CaZrO_3和CaTiO_3中不同的发光行为进行定性研究；另外，我们进一步研究了改变掺杂稀土离子对CaZrO_3的光谱调控作用，发现CaZrO_3是一种良好的可供稀土离子掺杂的基质材料，在近紫外光或蓝光激发下，通过改变掺杂离子可实现发光颜色调控，有潜力成为新型光学显示用荧光粉基质材料。
第三部分：Eu~(3+)掺杂立方复杂钙钛矿氧化物Ba_3Y_2WO_9的制备及发光性质研究。
前两部分所研究的基质材料属于简单钙钛矿结构氧化物，接下来将对复杂钙钛矿结构A(B′_(2/3)B″_(1/3))O_3型复合氧化物的发光性质进行研究，因为目前对此类型氧化物光学性质的研究是十分有限的。我们采用溶胶-凝胶法合成Eu~(3+)掺杂立方结构的复杂钙钛矿复合氧化物Ba_3Y_2WO_9（Ba(Y_(2/3)W_(1/3))O_3），通过XRD和场发射扫描电镜（FE-SEM）对合成样品的物相及微观形貌进行表征。通过测量Ba_3Y_2WO_9:Eu~(3+)的室温荧光光谱、高分辨格位选择性激光光谱及~5D0能级寿命，研究了Eu~(3+)在该基质中的发光性能和格位分布情况。研究表明Ba_3Y_2WO_9:Eu~(3+)是一种良好的可允许大量稀土离子掺杂（约为30mol%）的红橙色发光材料；Eu~(3+)取代Bs~(2+)和Y~(3+)格位，且其取代Bs~(2+)格位的同时形成电荷补偿缺陷，这种缺陷结构使Eu~(3+)周围晶格环境产生剧烈扰动。
本论文的研究，有助于更好地理解稀土离子的发光行为，丰富对稀土掺杂钙钛矿结构氧化物发光性能的认识，对进一步研究稀土掺杂钙钛矿结构氧化物的光学性质及其实际应用具有一定的科学参考价值。
Rare earth ions have stable physical and chemical properties, abundant levelstructure and longer lifetime.Under proper near UV or blue light excitation, rare earthions can be doped into appropriate host as the activator, to get excellent luminescenceproperties. Rare earth doped phosphors is an important class of function materials,and the rare eath doped oxides phosphors could be widely used in the field ofillumination and displays. With the advance of science and technology, and the basictheoretical study goes deeper and wider, people make higher demand on theluminescence properties of optical materials. The optical properities of rare earth ionsshow strong dependce on the compositon and structure of matrix materials, because oftheir unique4f intraconfiguration,4f5d configuration and the charge transfer bandstructure. Therefore, in the exploration of new phosphors, a selection of new hostmaterials to enhance the optical properties is a major concern.
Perovskite oxides are one of the most studied groups of materials, owing to theirwidely technological applications. In recent years, the optical properties of rareearth-doped perovskie oxides have attracted more and more interest of scientist.Furthermore, an incredibly high versatility of structures and phases with totallydifferent functions can be obtained depending upon the combination of chemicalelements into the formula ABO_3. So the optical properties of rare earth-dopedperovskite composite oxides show well research value and potential applications.
In this thesis, we systematically investigated on the synthesis and opticalproperties of rare earth-doped perovskite composite oxides. We synthesized a serielsof rare-earth-doped-perovskite composite oxides through sol-gel method and high temperature solid state reaction method, study on the optical properties of the rareearth ions (mainly Eu~(3+)) doped in different host materials. The main experimentalresearch includes photoluminescence excitation and emission spectra, concentrationquenching, lifetime and high resolution laser spectra. The experimental data weresummarized, analyzed and followed by partial theoretical calculation and analysis, toinvestigate the relation between composition, structure and luminescent properties.The thesis mainly consists of three parts, as follows:
Firstly, the preparation and analysis of Eu~(3+)-doped LnAlO_3(Ln=Gd, La).
LnAlO_3(Ln=Gd, La) are typical A~(3+)B~(3+)O_3perovskites. In this part, Eu~(3+)-dopedLaAlO_3and GdAlO_3phosphors were synthesized with sol-gel method. Thecrystallization processes of the phosphors were characterized by X-ray diffraction(XRD) and thermogravimetry-differential scanning calorimetry (TG-DSC), and theoptical properties were investigated in details. The influences of doping concentrationand annealing temperature on the luminescent intensity were investigated, and finallywe got the optimal doping concentration and calcining temperature for the twophosphors. Under appropriate UV-radiation, the reddish orange light emitted fromGdAlO_3:Eu~(3+)was brighter than that from LaAlO_3:Eu~(3+). Such a brightly luminescentphosphor could be considered as an ideal optical material for the development of newoptical display systems. As can be seen from the PLE spectra of Eu~(3+)-doped LaAlO_3and GdAlO_3, the CT band energy of Eu~(3+)―O2-was strongly influenced by the hostmaterials. Correspondingly, we calculated the bond lengths and bond covalency ofLa-O and Gd-O based on the chemical bond theory to investigate relations betweenthe CT band energy and bond convalency. Furthermore, the site-selective laserspectroscopy and luminescence decay of Eu~(3+)-doped GdAlO_3and LaAlO_3preparedby sol-gel method have been investigated at room temperature. As can be seen fromthe site-selective excitation spectra in the7F0→5D0region, there were threecrystallographic sites for Eu~(3+)in LaAlO_3:Eu~(3+), and one crystallographic site for Eu~(3+)in GdAlO_3:Eu~(3+).
Secondly, preparation and tunable spectra of CaRlO_3:Ln (R=Zr, Ti; Ln=Pr~(3+), Eu~(3+)),Tb~(3+), Tm~(3+), Dy~(3+), Sm~(3+)).
CaZrO_3and CaTiO_3are typical A2+B4+O_3perovskites. In this part, CaRlO_3:Ln(R=Zr, Ti; Ln=Pr~(3+), Eu~(3+), Tb~(3+), Tm~(3+), Dy~(3+), Sm~(3+)) phosphors were prepared byconventional solid state reaction. We investigated luminescent properties thePr3+/Eu~(3+)-doped CaRlO_3:Ln (R=Zr, Ti) through photoluminescence spectrameasurement, although CaZrO_3and CaTiO_3both possess orthorhombic structure,their luminescent properties were different. Furthermore, the tunable spectra ofCaZrO_3were investigated by changing the doped rare earth ions. As a result, CaZrO_3is a kind of well host materials, under appropriate UV or blue light excitation, CaZrO_3could get tunable color light emission, can be exploited as potential host materials foroptical display systems to get better color light output.
Thirdly, synthesis and investigation of luminescence properties of Eu~(3+)-dopedcubic perovskite Ba_3Y_2WO_9.
In the above two sections, we investigated the optical properties of rare earthdoped simple perovskite oxides. In this part, we focused on the luminescenceproperties of A(B′_(2/3)B″_(1/3))O_3type complex provskiteoxides, and the study on theoptical properties of this kind of provskite oxides is limited at present. Eu~(3+)-dopedcubic Ba_3Y_2WO_9phosphors were synthesized by sol-gel method. The preparedsamples were characterized by XRD and field emission-scanning electron microscopy(FE-SEM). The luminescence excitation emission spectra in the UV region, thesite-selective laser spectra along with luminescence decay were measured in the5D0-7F0region were used to characterize the luminescence properties and the sitedistributions of Eu~(3+)in Ba_3Y_2WO_9. As the result, the Ba_3Y_2WO_9:Eu~(3+)phosphorsexhibit strong orange-red luminescence, and the optimal concentration of Eu~(3+)in thehost of cubic Ba_3Y_2WO_9is30mol%; Eu~(3+)ions replace both theY~(3+)and Bs~(2+)ions,and the Eu~(3+)in Bs~(2+)sites accompanied by a charge-compensating defect leading tothe disordered surrounding.
引文
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