Eu~(2+,3+)掺杂ABPO_4（A=Li，Na，K，B=Mg，Ca，Sr，Ba）的发光性能及结构研究
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摘要
稀土掺杂的荧光粉在显示器、荧光灯等领域得到了广泛的应用。磷酸盐由于具有良好的物理、化学稳定性和热稳定性，可以用作发光材料的基质，在PDP、FED、LED等领域显示出极好的应用价值。Eu~(2+)是研究最为集中的稀土离子之一，其吸收与发射光谱通常是比较宽的带状谱，主要来自于基态与电子组态4f65d1的最低激发态之间的跃迁。激发与发射波长主要依赖于基质晶体，因此，基质的选取对稀土离子的发光有重要的影响。Eu~(3+)不但是最主要的红发光激活离子，而且还是重要的结构探针离子，微小的晶体学结构变化在其选择激发和发射光谱上会得到不同的~5D_0→~7F_0跃迁，对应不同的发光光谱和衰减变化。利用这一特点，可以研究稀土离子所处的晶体学环境，提供基质中不同发光中心的格位对称性，进一步分析微观结构与发光性质的关系。
本论文选择了正磷酸盐ABPO_4(A=Li, Na, K, B=Mg, Ca, Sr, Ba）系列为基质材料，该体系具有丰富的结构类型，且结构中含有PO_4四面刚性网络结构，易实现稀土离子的还原和在刚性网络结构中的稳定。稀土离子选择了Eu~(2+)、Eu~(3+)，采用高温固相法制备了Eu~(2+,3+)掺杂ABPO_4(A=Li, Na, K, B=Mg, Ca, Sr, Ba）系列的荧光粉，详细研究了其结构组成、发光性能、热稳定性、微观晶体学结构，讨论了该系列荧光粉作为新型发光材料在显示照明等领域的应用前景，特别是在UV、近UV白发光LEDs方面的潜在应用。
第二章，利用XRD对LiMgPO_4: Eu~(2+)的物相结构进行了表征，分析结果表明该样品具有纯相的橄榄石结构，空间群是Pnma。利用荧光光谱仪测试了Eu~(2+)掺杂LiMgPO_4的发射光谱及衰减曲线，低温下观察到了360nm处的发射峰，来自4f7(6P7/2)→4f~7(~8S_(7/2))辐射跃迁与零声子谱线的重叠。研究了温度对发光强度及衰减时间的影响。利用脉冲染料激光器测试了Eu~(3+)离子在LiMgPO_4中的位置选择激发与发射光谱，位置选择激发光谱由579.0nm (M)处的主峰与579.9nm (M')处的弱峰组成，表明Eu~(3+)离子占据一个固有的晶体学位置Eu~(3+)(M)与一个无序的位置Eu~(3+)(M')；讨论了稀土离子掺杂LiMgPO_4的电荷补偿机制，本研究工作对于稀土离子掺杂这种磷酸盐基质的发光研究具有重要的意义。
第三章，采用传统的高温固态反应合成了荧光粉KMgPO_4:Eu~(2+)，利用荧光光谱仪测试了样品的光致激发与发射光谱，激发光谱是从230-400nm的宽带谱，近紫外光激发下，发射光谱为主发射峰在470nm的光谱带，该光谱来自于室温下Eu~(2+)离子4f~65d~1→4f7的辐射跃迁。研究了温度对发光与衰减时间的影响，发现基质晶格中有两个不同的Eu~(2+)位置，它们呈现了不同的发光与衰减。根据其发光性质与晶体结构讨论了Eu~(2+)离子在晶格中占据两个不同的K+位置。报道了从10K到室温发光衰减反常增大的现象。
第四章，深入研究了荧光粉NaMgPO_4:Eu~(2+)的发光性能，激发光谱是从220到430nm的宽带谱，来自于4f~65d~1→4f~7(~8S_(7/2))的辐射跃迁。低温下观察到了4f7(6P7/2)→4f~7(~8S_(7/2))跃迁的发射谱线，峰值为360nm。报道了Eu~(2+)离子掺杂NaMgPO_4的发光量子效率、结晶学位置及微观结构，讨论了Eu~(2+)在NaMgPO_4晶格中的多位置结构，结果表明Eu~(2+)处于无序的结构环境。测试了发光与温度之间的依赖关系曲线（18-300K），计算了发光猝灭温度与热激活能。讨论了该荧光粉的发光热稳定性与晶体结构的关系。
第五章，采用高温固态反应合成了绿色荧光粉LiBaPO_4:Eu~(2+)，测试了激发与发射光谱、发光强度与温度的关系及发光衰减曲线(12-450K)，计算了热猝灭温度与激活能。结果表明随着温度的升高发射光有反常的蓝移现象，热猝灭温度较低。观察到该荧光粉有余晖现象。
通过Eu~(3+)结构探针离子的位置选择激发和发射光谱，研究了Eu掺杂LiBaPO_4的微观结构与晶体学环境，表明晶格中Eu有三种发光位置即Eu(2)(578.0nm)，Eu(1)(578.7nm)和Eu(3)(580.3nm)。讨论了荧光粉的发光机制，测试了发光量子效率并与文献报道的结果进行了比较，表明LiBaPO_4:Eu~(2+)不适合应用于W-LEDs。
第六章，利用XRD测试了NaBaPO_4:Eu~(2+)荧光粉的物相结构，分析结果表明所制得的样品为纯相NaBaPO_4晶体，与钾芒硝同构，空间群为P3|-m1。测试了NaBaPO_4:Eu~(2+)的激发光谱与发射光谱。研究了温度依赖发光强度和衰减时间，计算了斯托克斯位移、发光量子效率(QE)、热猝灭激活能(ΔE)，结果表明T0.5为550K，热稳定性较好，而QE较低只有38.5%，并且发现随着温度的升高发射带出现了反常的蓝移现象。
测试了Eu~(3+)结构探针离子的位置选择激发和发射光谱，与7F0→~5D_0跃迁对应的激发光谱由峰值为579.6nm Eu(I)和578.9nm Eu(II)的谱线组成，表明Eu~(3+)在基质晶格中占据两种不同的晶体学位置。测试了两种Eu~(3+)位置的衰减时间，研究了发光特征与晶体结构位置的关系。最后讨论了Eu~(3+)掺杂NaBaPO_4的电荷补偿机制，对于稀土离子掺杂这类磷酸盐的发光研究具有重要的借鉴意义。
第七章，研究了Eu~(2+)掺杂具有β-K2SO_4结构的正磷酸盐NaSrPO_4和KBaPO_4的发光性质及热稳定性，结果表明，KBaPO_4:Eu~(2+)的发射光谱只有一个发射峰，中心波长为420nm；而NaSrPO_4:Eu~(2+)的发射光谱是非对称光谱。测试了其物相结构、衰减曲线、发光量子效率(QE)。根据发光强度与温度的关系及衰减曲线(10-435K)，计算了NaSrPO_4:Eu~(2+)和KBaPO_4:Eu~(2+)热猝灭的激活能，分别为0.053eV与0.121eV。为了确定稀土掺杂KBaPO_4和NaSrPO_4的结构分布，研究了Eu~(3+)离子的位置选择激发与发射光谱，表明稀土掺杂KBaPO_4中只有一个高度有序的结构位置，而NaSrPO_4中，稀土离子处于高度无序的结构环境，这种不同的结构环境决定了它们不同的发光性质。
第八章，详细研究了LiCaPO_4:Eu~(2+)荧光粉的激发光谱、掺杂浓度与发光强度的关系、温度与发光衰减的关系，结果表明，该荧光粉能够被280-420nm的紫外光有效地激发，与近UV LEDs芯片相匹配，在365nm紫外光激发下，发射出中心波长为470nm的蓝色光谱。研究了温度与浓度分别对发光强度的影响。计算了不同温度下的发光衰减时间与色度坐标，发现该荧光粉具有极好的热稳定性与色稳定性，表明LiCaPO_4:Eu~(2+)在W-LEDs应用中是一种潜在的蓝色荧光粉。
第九章，通过传统的高温固相法合成了绿色荧光粉KCaPO_4:Eu~(2+)，利用X RD测试了荧光粉的物相结构。测试了光致激发与发射光谱，分析了发光强度对温度的依赖关系，随着温度的升高，发射光谱显示了反常的蓝移现象。计算和讨论了色度坐标、发光猝灭温度和热激活能，利用Eu~(3+)结构探针离子的位置选择激发和发射光谱研究了KCaPO_4基质中阳离子Ca2+的微观结构特征，讨论了Eu~(2+)在KCaPO_4中的多位置结构，这有助于进一步研究稀土离子掺磷酸盐系列的发光性质。
本论文创新点是：系统研究了Eu~(2+,3+)掺杂正磷酸盐ABPO_4(A=Li, Na, K, B=Mg,Ca, Sr, Ba）的物相结构、发光性能及其发光衰减特征；首次利用Eu~(3+)离子的激光位置选择激发和发射光谱技术分别研究了体系的微观结构特点，以及稀土离子在基质中的占位问题；研究了不同格位的发光性能及衰减时间，从更高理论深度探讨了稀土离子（尤其是多格位掺杂）的微观晶体学结构与其发光性能的关系，揭示了结构特征对其发光性能有重要的影响。对于稀土掺杂磷酸盐的进一步开发应用具有重要的参考和借鉴价值。
Rare-earth (RE) doped materials have been widely applied in display, fluorescentlamp, WLED and many other fields. The phosphates with ABPO_4formula (A and B aremono-and divalent cations, respectively) are a large family of mono-phosphates withthe different structure types. These compounds have been considered to be efficientluminescent hosts due to its excellent physical, chemical and thermal stability and haverepresented excellent application value in PDP, FED and LED areas.
The absorption and emission spectra of Eu~(2+)usually comprise broad bands due totransitions between the4f7ground state and the crystal field components of the4f~65d~1excited state configuration. The wavelengths of excitation and emission bands stronglydepend on the host crystal. So the choice of the hosts greatly affects the opticalproperties of Eu~(2+)ions.
As one of the most important activator ions, Eu~(3+)is widely applied in redluminescent materials. The luminescence of Eu~(3+)being the well-known probe ion ishighly affected by the surrounding environments in a lattice. The luminescence from~5D_0→~7F_0transitions of Eu~(3+)ions can present different emission spectra and decayprofiles when their crystallographic surroundings have even small changes. Thesurrounding environment of Eu~(3+)ions doped in a host can be elucidated by applying thesite-selective excitation and emission spectra technique. And this also can provide thesymmetry of different luminescence centers in the matrix and then give relation betweenthe microscopic structure and luminescence properties.
In this work, the phosphates with ABPO_4(A=Li, Na, K, B=Mg, Ca, Sr, Ba) with various structure types were selected to be the host material and can promote rare earthions reduction and stability in host lattice due to their PO_4tetrahedra rigid networkstructure. Eu~(2+),3+-doped ABPO_4(A=Li, Na, K, B=Mg, Ca, Sr, Ba) were prepared byhigh temperature solid-state reaction. Their crystal structures, luminescence properties,thermal stability and microscopic crystal structure were investigated. Their potentialapplications as a new phosphor were discussed in display, fluorescent lamp, in particular,in WLED field.
In the chapter two, the formation of LiMgPO_4: Eu~(2+)was confirmed by X-raypowder diffraction measurement to be single LiMgPO_4phase. It belongs to the orderedolivine-type structure with the space group Pnma. The photoluminescence excitationand emission spectra and decay curves were measured. At low temperature it is foundthat the emission line of the4f7(6P7/2)→4f~7(~8S_(7/2)) transition is overlapped with thezero-phonon line at nearly the same position of360nm. The influences of temperatureon the luminescence spectra and decay times were investigated. The site-selectiveexcitation and emission spectra have been investigated in the~5D_0→~7F_0region by using apulsed, tunable and narrowband dye laser. The excitation spectra consist of the strongestline at579.0nm (M) and a weak broad peak at579.9nm (M'. The results clearlyindicate that the Eu~(3+)ions occupy one intrinsic crystallographic site Eu~(3+)(M) and otherdisturbed sites Eu~(3+)(M') in LiMgPO_4. The charge compensation mechanisms of Eu~(3+)doping in LiMgPO_4were discussed. This is helpful for the luminescence investigationof RE ions doped in this kind of phosphate host.
In the chapter three, Eu~(2+)-doped KMgPO_4was prepared by high-temperaturesolid-state reaction. Photoluminescence excitation spectrum measurements show thatthe phosphor can be efficiently excited by near UV light from230to400nm andpresents a dominant luminescence band centered at470nm due to the4f~65d~1→4f7transition of Eu~(2+)ions at room temperature. The influence of temperature on theluminescence and decay times were investigated. There are two distinct Eu~(2+)sites inKMgPO_4lattices, which present different luminescence and lifetimes. The assignmentsof the Eu~(2+)sites were discussed on the base of the luminescence properties and the structure of KMgPO_4crystal. The unusual increase of the decay time of the4f65demission in KMgPO_4from10K to room temperature was reported.
In the chapter four, the luminescence of NaMgPO_4:Eu~(2+)was given an insightinvestigation. The phosphor can be excited by UV-visible light from220to430nm torealize emission from4f~65d~1→4f~7(~8S_(7/2)) transition in the blue range. The4f7(6P7/2)→4f~7(~8S_(7/2)) transition in the4f7electronic configuration of Eu~(2+)at360nm was observedat low temperature. The luminescence absolute quantum efficiency, the crystallographicsites and the microstructure of Eu~(2+)ions doped in NaMgPO_4lattices were reported. Themultiple sites structure of Eu~(2+)ions in NaMgPO_4lattices was discussed. Theluminescence quenching temperatures and the thermal activation energy forNaMgPO_4:Eu~(2+)were obtained from the temperature dependent (18–300K)luminescence decay curves. Eu~(2+)ions have the “disordered environment” in NaMgPO_4lattices. The relation between the luminescence thermal stabilities and the crystalstructures were discussed.
In the chapter five, Eu~(2+)-activated LiBaPO_4phosphor was synthesized byconventional solid-state reaction. The photoluminescence excitation and emissionspectra, the temperature dependent luminescence intensities (12-450K) and decaycurves of the phosphor were investigated. With the increasing of temperatures, theemission bands of LiBaPO_4:Eu~(2+)show the abnormal blue-shift and the decreasing ofemission intensity. The natures of the Eu~(2+)emission in LiBaPO_4, e.g., the luminescencequenching temperature, and the activation energy for thermal quenching (ΔE), werereported. The afterglow fluorescence was detected in LiBaPO_4:Eu~(2+)phosphor. Thesite-selective excitation in the~5D_0→~7F_0region for Eu~(3+)ions, emission spectra and decaycurves have been investigated using a pulsed, tunable and narrowband dye laser todetect the micro-structure and crystallographic surrounding of Eu~(3+),2+at Ba2+sites inLiBaPO_4. The multiple sites structure of Eu~(2+)and Eu~(3+)ions in LiBaPO_4lattices wassuggested. The lower quenching temperature, afterglow and luminescence mechanismwere discussed. The Photoluminescence quantum efficiencies of LiBaPO_4:Eu~(2+)weremeasured and compared with the reported phosphors. Different from the published data on LiBaPO_4:Eu~(2+), this investigation indicate that LiBaPO_4:Eu~(2+)is not a good phosphorcandidate applied in white light emitting diode.
In the chapter six, the phase formation of NaBaPO_4:Eu~(2+)was confirmed by X-raypowder diffraction measurements. No impurity lines were observed and the structurewith the space group P3m1is isotypic with that of glaserite. The photoluminescenceexcitation and emission spectra, and the luminescence quantum efficiency of Eu~(2+)ionswere investigated. The dependence of luminescence intensities on temperatures, and thetemperature-dependent decay times of Eu~(2+)doped NaBaPO_4were measured anddiscussed. The natures of the Eu~(2+)emission in NaBaPO_4, e.g., the Stokes shifts, theluminescence quenching temperature (T0.5), the activation energy for thermal quenching(ΔE) were reported. The phosphor shows an excellent thermal stability on temperaturequenching effects. With the increasing of temperature, the emission bands show theabnormal blue-shift.
The laser site-selective excitation and emission spectra have been investigated inthe~5D_0→~7F_0region by using a pulsed, tunable and narrowband dye laser. The excitationspectra corresponding to the~7F_0→~5D_0transition consist of two transitions at579.6nmEu(I) and578.9nm Eu(II), indicating the Eu~(3+)ions occupy two crystallographic sites ofBa2+ions. The decay lifetimes of the two Eu~(3+)sites were measured. Twocrystallographic sites for Eu~(3+)ions doped in NaBaPO_4lattice were assigned from theluminescence characteristic and structure features. Meanwhile, the charge compensationmechanism of Eu~(3+)doping in NaBaPO_4was discussed
In the chapter seven, two Eu~(2+,3+)-doped mono-phosphate hosts NaSrPO_4andKBaPO_4with β-K2SO_4structure have been selected to investigate the luminescenceproperties and thermal stabilities. KBaPO_4:Eu~(2+)shows one emission band peaking at420nm, however, the emission spectra of NaSrPO_4:Eu~(2+)have an asymmetric spectrum.The phase formation, the decay curves and the luminescence absolute quantumefficiencies were measured. The luminescence quenching temperatures and the thermalactivation energy for NaSrPO_4:Eu~(2+)and KBaPO_4:Eu~(2+)were obtained from thetemperature dependent (10-435K) luminescence intensities and decay curves. KBaPO_4:Eu~(2+)presents only one emission center, however, Eu~(2+)ions have the“disordered environment” in NaSrPO_4lattices. This was analogically analyzed by thesite-selective emission spectra and the excitation spectra of the~7F_0→~5D_0transitions ofEu~(3+)ions in the hosts using a pulsed, tunable and narrowband dye laser. In KBaPO_4, theEu~(3+)ions could be distributed in the host with a high “ordered state” in only one site inthe lattices. However, the multiple sites structure of Eu~(3+)ions with highly disordereddistributions in NaSrPO_4lattices was suggested. The relation between the luminescencethermal stabilities and the crystal structures were discussed.
In the chapter eight, the photoluminescence excitation and emission spectra wereinvestigated. The results showed that LiCaPO_4:Eu~(2+)can be efficiently excited by theincident lights of280-420nm, which well match with the emissions of near-UV LEDs.The phosphor showed bright blue luminescence. The temperature and concentrationdependence of luminescence intensities were investigated. The phosphor has anexcellent thermal stability on temperature quenching effects. The luminescence decayand the color coordinates were discussed in order to further investigate its potentialapplications for white light-emitting diode phosphors pumped by near-UV chip.
In the chapter nine, a green-emitting phosphor, Eu~(2+)-activated KCaPO_4, wassynthesized by conventional solid-state reaction. The phase formation was confirmed byX-ray powder diffraction measurements. The photoluminescence excitation andemission spectra, the temperature dependent luminescence intensities (293-438K) anddecay curves of the phosphor were measured. With the increasing of temperature, theemission bands show the abnormal blue-shift with broadening bandwidth. The naturesof the Eu~(2+)emission in KCaPO_4, e.g., the chromaticity coordinates, the luminescencequenching temperature, activation energy for thermal quenching (ΔE), were reported.The excitation spectra have been investigated in the~5D_0→~7F_0region for Eu~(3+)ions inKCaPO_4by using a pulsed, tunable and narrowband dye laser to detect the cation site ofCa2+in KCaPO_4. The multiple sites structure of Eu~(2+)ions in KMgPO_4lattices weresuggested and discussed.
The novelties of this dissertation are as follows: the structure characteristics, photoluminescence properties and decay curves of Eu~(2+,3+)-doped ABPO_4(A=Li, Na, K,B=Mg, Ca, Sr, Ba) were systematically studied. The features about microstructure ofABPO_4and crystallographic site-occupations of Eu ions were firstly investigated by thesite-selective excitation and emission spectra. The luminescence performances ofdifferent crystallographic sites have been investigated. The relation between themicroscopic structure and luminescence properties of Eu ions was insight discussed intheory to obtain the influence of the structure characteristic on luminescence features. Ina word, this provided a helpful reference for further development and application of rareearth doped ABPO_4phosphor.
本论文选择了正磷酸盐ABPO_4(A=Li, Na, K, B=Mg, Ca, Sr, Ba）系列为基质材料，该体系具有丰富的结构类型，且结构中含有PO_4四面刚性网络结构，易实现稀土离子的还原和在刚性网络结构中的稳定。稀土离子选择了Eu~(2+)、Eu~(3+)，采用高温固相法制备了Eu~(2+,3+)掺杂ABPO_4(A=Li, Na, K, B=Mg, Ca, Sr, Ba）系列的荧光粉，详细研究了其结构组成、发光性能、热稳定性、微观晶体学结构，讨论了该系列荧光粉作为新型发光材料在显示照明等领域的应用前景，特别是在UV、近UV白发光LEDs方面的潜在应用。
第二章，利用XRD对LiMgPO_4: Eu~(2+)的物相结构进行了表征，分析结果表明该样品具有纯相的橄榄石结构，空间群是Pnma。利用荧光光谱仪测试了Eu~(2+)掺杂LiMgPO_4的发射光谱及衰减曲线，低温下观察到了360nm处的发射峰，来自4f7(6P7/2)→4f~7(~8S_(7/2))辐射跃迁与零声子谱线的重叠。研究了温度对发光强度及衰减时间的影响。利用脉冲染料激光器测试了Eu~(3+)离子在LiMgPO_4中的位置选择激发与发射光谱，位置选择激发光谱由579.0nm (M)处的主峰与579.9nm (M')处的弱峰组成，表明Eu~(3+)离子占据一个固有的晶体学位置Eu~(3+)(M)与一个无序的位置Eu~(3+)(M')；讨论了稀土离子掺杂LiMgPO_4的电荷补偿机制，本研究工作对于稀土离子掺杂这种磷酸盐基质的发光研究具有重要的意义。
第三章，采用传统的高温固态反应合成了荧光粉KMgPO_4:Eu~(2+)，利用荧光光谱仪测试了样品的光致激发与发射光谱，激发光谱是从230-400nm的宽带谱，近紫外光激发下，发射光谱为主发射峰在470nm的光谱带，该光谱来自于室温下Eu~(2+)离子4f~65d~1→4f7的辐射跃迁。研究了温度对发光与衰减时间的影响，发现基质晶格中有两个不同的Eu~(2+)位置，它们呈现了不同的发光与衰减。根据其发光性质与晶体结构讨论了Eu~(2+)离子在晶格中占据两个不同的K+位置。报道了从10K到室温发光衰减反常增大的现象。
第四章，深入研究了荧光粉NaMgPO_4:Eu~(2+)的发光性能，激发光谱是从220到430nm的宽带谱，来自于4f~65d~1→4f~7(~8S_(7/2))的辐射跃迁。低温下观察到了4f7(6P7/2)→4f~7(~8S_(7/2))跃迁的发射谱线，峰值为360nm。报道了Eu~(2+)离子掺杂NaMgPO_4的发光量子效率、结晶学位置及微观结构，讨论了Eu~(2+)在NaMgPO_4晶格中的多位置结构，结果表明Eu~(2+)处于无序的结构环境。测试了发光与温度之间的依赖关系曲线（18-300K），计算了发光猝灭温度与热激活能。讨论了该荧光粉的发光热稳定性与晶体结构的关系。
第五章，采用高温固态反应合成了绿色荧光粉LiBaPO_4:Eu~(2+)，测试了激发与发射光谱、发光强度与温度的关系及发光衰减曲线(12-450K)，计算了热猝灭温度与激活能。结果表明随着温度的升高发射光有反常的蓝移现象，热猝灭温度较低。观察到该荧光粉有余晖现象。
通过Eu~(3+)结构探针离子的位置选择激发和发射光谱，研究了Eu掺杂LiBaPO_4的微观结构与晶体学环境，表明晶格中Eu有三种发光位置即Eu(2)(578.0nm)，Eu(1)(578.7nm)和Eu(3)(580.3nm)。讨论了荧光粉的发光机制，测试了发光量子效率并与文献报道的结果进行了比较，表明LiBaPO_4:Eu~(2+)不适合应用于W-LEDs。
第六章，利用XRD测试了NaBaPO_4:Eu~(2+)荧光粉的物相结构，分析结果表明所制得的样品为纯相NaBaPO_4晶体，与钾芒硝同构，空间群为P3|-m1。测试了NaBaPO_4:Eu~(2+)的激发光谱与发射光谱。研究了温度依赖发光强度和衰减时间，计算了斯托克斯位移、发光量子效率(QE)、热猝灭激活能(ΔE)，结果表明T0.5为550K，热稳定性较好，而QE较低只有38.5%，并且发现随着温度的升高发射带出现了反常的蓝移现象。
测试了Eu~(3+)结构探针离子的位置选择激发和发射光谱，与7F0→~5D_0跃迁对应的激发光谱由峰值为579.6nm Eu(I)和578.9nm Eu(II)的谱线组成，表明Eu~(3+)在基质晶格中占据两种不同的晶体学位置。测试了两种Eu~(3+)位置的衰减时间，研究了发光特征与晶体结构位置的关系。最后讨论了Eu~(3+)掺杂NaBaPO_4的电荷补偿机制，对于稀土离子掺杂这类磷酸盐的发光研究具有重要的借鉴意义。
第七章，研究了Eu~(2+)掺杂具有β-K2SO_4结构的正磷酸盐NaSrPO_4和KBaPO_4的发光性质及热稳定性，结果表明，KBaPO_4:Eu~(2+)的发射光谱只有一个发射峰，中心波长为420nm；而NaSrPO_4:Eu~(2+)的发射光谱是非对称光谱。测试了其物相结构、衰减曲线、发光量子效率(QE)。根据发光强度与温度的关系及衰减曲线(10-435K)，计算了NaSrPO_4:Eu~(2+)和KBaPO_4:Eu~(2+)热猝灭的激活能，分别为0.053eV与0.121eV。为了确定稀土掺杂KBaPO_4和NaSrPO_4的结构分布，研究了Eu~(3+)离子的位置选择激发与发射光谱，表明稀土掺杂KBaPO_4中只有一个高度有序的结构位置，而NaSrPO_4中，稀土离子处于高度无序的结构环境，这种不同的结构环境决定了它们不同的发光性质。
第八章，详细研究了LiCaPO_4:Eu~(2+)荧光粉的激发光谱、掺杂浓度与发光强度的关系、温度与发光衰减的关系，结果表明，该荧光粉能够被280-420nm的紫外光有效地激发，与近UV LEDs芯片相匹配，在365nm紫外光激发下，发射出中心波长为470nm的蓝色光谱。研究了温度与浓度分别对发光强度的影响。计算了不同温度下的发光衰减时间与色度坐标，发现该荧光粉具有极好的热稳定性与色稳定性，表明LiCaPO_4:Eu~(2+)在W-LEDs应用中是一种潜在的蓝色荧光粉。
第九章，通过传统的高温固相法合成了绿色荧光粉KCaPO_4:Eu~(2+)，利用X RD测试了荧光粉的物相结构。测试了光致激发与发射光谱，分析了发光强度对温度的依赖关系，随着温度的升高，发射光谱显示了反常的蓝移现象。计算和讨论了色度坐标、发光猝灭温度和热激活能，利用Eu~(3+)结构探针离子的位置选择激发和发射光谱研究了KCaPO_4基质中阳离子Ca2+的微观结构特征，讨论了Eu~(2+)在KCaPO_4中的多位置结构，这有助于进一步研究稀土离子掺磷酸盐系列的发光性质。
本论文创新点是：系统研究了Eu~(2+,3+)掺杂正磷酸盐ABPO_4(A=Li, Na, K, B=Mg,Ca, Sr, Ba）的物相结构、发光性能及其发光衰减特征；首次利用Eu~(3+)离子的激光位置选择激发和发射光谱技术分别研究了体系的微观结构特点，以及稀土离子在基质中的占位问题；研究了不同格位的发光性能及衰减时间，从更高理论深度探讨了稀土离子（尤其是多格位掺杂）的微观晶体学结构与其发光性能的关系，揭示了结构特征对其发光性能有重要的影响。对于稀土掺杂磷酸盐的进一步开发应用具有重要的参考和借鉴价值。
Rare-earth (RE) doped materials have been widely applied in display, fluorescentlamp, WLED and many other fields. The phosphates with ABPO_4formula (A and B aremono-and divalent cations, respectively) are a large family of mono-phosphates withthe different structure types. These compounds have been considered to be efficientluminescent hosts due to its excellent physical, chemical and thermal stability and haverepresented excellent application value in PDP, FED and LED areas.
The absorption and emission spectra of Eu~(2+)usually comprise broad bands due totransitions between the4f7ground state and the crystal field components of the4f~65d~1excited state configuration. The wavelengths of excitation and emission bands stronglydepend on the host crystal. So the choice of the hosts greatly affects the opticalproperties of Eu~(2+)ions.
As one of the most important activator ions, Eu~(3+)is widely applied in redluminescent materials. The luminescence of Eu~(3+)being the well-known probe ion ishighly affected by the surrounding environments in a lattice. The luminescence from~5D_0→~7F_0transitions of Eu~(3+)ions can present different emission spectra and decayprofiles when their crystallographic surroundings have even small changes. Thesurrounding environment of Eu~(3+)ions doped in a host can be elucidated by applying thesite-selective excitation and emission spectra technique. And this also can provide thesymmetry of different luminescence centers in the matrix and then give relation betweenthe microscopic structure and luminescence properties.
In this work, the phosphates with ABPO_4(A=Li, Na, K, B=Mg, Ca, Sr, Ba) with various structure types were selected to be the host material and can promote rare earthions reduction and stability in host lattice due to their PO_4tetrahedra rigid networkstructure. Eu~(2+),3+-doped ABPO_4(A=Li, Na, K, B=Mg, Ca, Sr, Ba) were prepared byhigh temperature solid-state reaction. Their crystal structures, luminescence properties,thermal stability and microscopic crystal structure were investigated. Their potentialapplications as a new phosphor were discussed in display, fluorescent lamp, in particular,in WLED field.
In the chapter two, the formation of LiMgPO_4: Eu~(2+)was confirmed by X-raypowder diffraction measurement to be single LiMgPO_4phase. It belongs to the orderedolivine-type structure with the space group Pnma. The photoluminescence excitationand emission spectra and decay curves were measured. At low temperature it is foundthat the emission line of the4f7(6P7/2)→4f~7(~8S_(7/2)) transition is overlapped with thezero-phonon line at nearly the same position of360nm. The influences of temperatureon the luminescence spectra and decay times were investigated. The site-selectiveexcitation and emission spectra have been investigated in the~5D_0→~7F_0region by using apulsed, tunable and narrowband dye laser. The excitation spectra consist of the strongestline at579.0nm (M) and a weak broad peak at579.9nm (M'. The results clearlyindicate that the Eu~(3+)ions occupy one intrinsic crystallographic site Eu~(3+)(M) and otherdisturbed sites Eu~(3+)(M') in LiMgPO_4. The charge compensation mechanisms of Eu~(3+)doping in LiMgPO_4were discussed. This is helpful for the luminescence investigationof RE ions doped in this kind of phosphate host.
In the chapter three, Eu~(2+)-doped KMgPO_4was prepared by high-temperaturesolid-state reaction. Photoluminescence excitation spectrum measurements show thatthe phosphor can be efficiently excited by near UV light from230to400nm andpresents a dominant luminescence band centered at470nm due to the4f~65d~1→4f7transition of Eu~(2+)ions at room temperature. The influence of temperature on theluminescence and decay times were investigated. There are two distinct Eu~(2+)sites inKMgPO_4lattices, which present different luminescence and lifetimes. The assignmentsof the Eu~(2+)sites were discussed on the base of the luminescence properties and the structure of KMgPO_4crystal. The unusual increase of the decay time of the4f65demission in KMgPO_4from10K to room temperature was reported.
In the chapter four, the luminescence of NaMgPO_4:Eu~(2+)was given an insightinvestigation. The phosphor can be excited by UV-visible light from220to430nm torealize emission from4f~65d~1→4f~7(~8S_(7/2)) transition in the blue range. The4f7(6P7/2)→4f~7(~8S_(7/2)) transition in the4f7electronic configuration of Eu~(2+)at360nm was observedat low temperature. The luminescence absolute quantum efficiency, the crystallographicsites and the microstructure of Eu~(2+)ions doped in NaMgPO_4lattices were reported. Themultiple sites structure of Eu~(2+)ions in NaMgPO_4lattices was discussed. Theluminescence quenching temperatures and the thermal activation energy forNaMgPO_4:Eu~(2+)were obtained from the temperature dependent (18–300K)luminescence decay curves. Eu~(2+)ions have the “disordered environment” in NaMgPO_4lattices. The relation between the luminescence thermal stabilities and the crystalstructures were discussed.
In the chapter five, Eu~(2+)-activated LiBaPO_4phosphor was synthesized byconventional solid-state reaction. The photoluminescence excitation and emissionspectra, the temperature dependent luminescence intensities (12-450K) and decaycurves of the phosphor were investigated. With the increasing of temperatures, theemission bands of LiBaPO_4:Eu~(2+)show the abnormal blue-shift and the decreasing ofemission intensity. The natures of the Eu~(2+)emission in LiBaPO_4, e.g., the luminescencequenching temperature, and the activation energy for thermal quenching (ΔE), werereported. The afterglow fluorescence was detected in LiBaPO_4:Eu~(2+)phosphor. Thesite-selective excitation in the~5D_0→~7F_0region for Eu~(3+)ions, emission spectra and decaycurves have been investigated using a pulsed, tunable and narrowband dye laser todetect the micro-structure and crystallographic surrounding of Eu~(3+),2+at Ba2+sites inLiBaPO_4. The multiple sites structure of Eu~(2+)and Eu~(3+)ions in LiBaPO_4lattices wassuggested. The lower quenching temperature, afterglow and luminescence mechanismwere discussed. The Photoluminescence quantum efficiencies of LiBaPO_4:Eu~(2+)weremeasured and compared with the reported phosphors. Different from the published data on LiBaPO_4:Eu~(2+), this investigation indicate that LiBaPO_4:Eu~(2+)is not a good phosphorcandidate applied in white light emitting diode.
In the chapter six, the phase formation of NaBaPO_4:Eu~(2+)was confirmed by X-raypowder diffraction measurements. No impurity lines were observed and the structurewith the space group P3m1is isotypic with that of glaserite. The photoluminescenceexcitation and emission spectra, and the luminescence quantum efficiency of Eu~(2+)ionswere investigated. The dependence of luminescence intensities on temperatures, and thetemperature-dependent decay times of Eu~(2+)doped NaBaPO_4were measured anddiscussed. The natures of the Eu~(2+)emission in NaBaPO_4, e.g., the Stokes shifts, theluminescence quenching temperature (T0.5), the activation energy for thermal quenching(ΔE) were reported. The phosphor shows an excellent thermal stability on temperaturequenching effects. With the increasing of temperature, the emission bands show theabnormal blue-shift.
The laser site-selective excitation and emission spectra have been investigated inthe~5D_0→~7F_0region by using a pulsed, tunable and narrowband dye laser. The excitationspectra corresponding to the~7F_0→~5D_0transition consist of two transitions at579.6nmEu(I) and578.9nm Eu(II), indicating the Eu~(3+)ions occupy two crystallographic sites ofBa2+ions. The decay lifetimes of the two Eu~(3+)sites were measured. Twocrystallographic sites for Eu~(3+)ions doped in NaBaPO_4lattice were assigned from theluminescence characteristic and structure features. Meanwhile, the charge compensationmechanism of Eu~(3+)doping in NaBaPO_4was discussed
In the chapter seven, two Eu~(2+,3+)-doped mono-phosphate hosts NaSrPO_4andKBaPO_4with β-K2SO_4structure have been selected to investigate the luminescenceproperties and thermal stabilities. KBaPO_4:Eu~(2+)shows one emission band peaking at420nm, however, the emission spectra of NaSrPO_4:Eu~(2+)have an asymmetric spectrum.The phase formation, the decay curves and the luminescence absolute quantumefficiencies were measured. The luminescence quenching temperatures and the thermalactivation energy for NaSrPO_4:Eu~(2+)and KBaPO_4:Eu~(2+)were obtained from thetemperature dependent (10-435K) luminescence intensities and decay curves. KBaPO_4:Eu~(2+)presents only one emission center, however, Eu~(2+)ions have the“disordered environment” in NaSrPO_4lattices. This was analogically analyzed by thesite-selective emission spectra and the excitation spectra of the~7F_0→~5D_0transitions ofEu~(3+)ions in the hosts using a pulsed, tunable and narrowband dye laser. In KBaPO_4, theEu~(3+)ions could be distributed in the host with a high “ordered state” in only one site inthe lattices. However, the multiple sites structure of Eu~(3+)ions with highly disordereddistributions in NaSrPO_4lattices was suggested. The relation between the luminescencethermal stabilities and the crystal structures were discussed.
In the chapter eight, the photoluminescence excitation and emission spectra wereinvestigated. The results showed that LiCaPO_4:Eu~(2+)can be efficiently excited by theincident lights of280-420nm, which well match with the emissions of near-UV LEDs.The phosphor showed bright blue luminescence. The temperature and concentrationdependence of luminescence intensities were investigated. The phosphor has anexcellent thermal stability on temperature quenching effects. The luminescence decayand the color coordinates were discussed in order to further investigate its potentialapplications for white light-emitting diode phosphors pumped by near-UV chip.
In the chapter nine, a green-emitting phosphor, Eu~(2+)-activated KCaPO_4, wassynthesized by conventional solid-state reaction. The phase formation was confirmed byX-ray powder diffraction measurements. The photoluminescence excitation andemission spectra, the temperature dependent luminescence intensities (293-438K) anddecay curves of the phosphor were measured. With the increasing of temperature, theemission bands show the abnormal blue-shift with broadening bandwidth. The naturesof the Eu~(2+)emission in KCaPO_4, e.g., the chromaticity coordinates, the luminescencequenching temperature, activation energy for thermal quenching (ΔE), were reported.The excitation spectra have been investigated in the~5D_0→~7F_0region for Eu~(3+)ions inKCaPO_4by using a pulsed, tunable and narrowband dye laser to detect the cation site ofCa2+in KCaPO_4. The multiple sites structure of Eu~(2+)ions in KMgPO_4lattices weresuggested and discussed.
The novelties of this dissertation are as follows: the structure characteristics, photoluminescence properties and decay curves of Eu~(2+,3+)-doped ABPO_4(A=Li, Na, K,B=Mg, Ca, Sr, Ba) were systematically studied. The features about microstructure ofABPO_4and crystallographic site-occupations of Eu ions were firstly investigated by thesite-selective excitation and emission spectra. The luminescence performances ofdifferent crystallographic sites have been investigated. The relation between themicroscopic structure and luminescence properties of Eu ions was insight discussed intheory to obtain the influence of the structure characteristic on luminescence features. Ina word, this provided a helpful reference for further development and application of rareearth doped ABPO_4phosphor.
引文
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