用于白光LED的CaO-SiO_2体系混晶荧光体的光谱调控研究
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摘要
本学位论文针对现有InGaN基光转换白光二极管（pc-wLED）的白光配色技术中存在的荧光体混粉、色品等问题，以CaO-SiO2体系的混晶直接白光荧光体为研究目标，分别研究了铕（Eu）激活的Ca_2SiO_4绿色荧光体和Ca_3Si_2O_7红色荧光体，对荧光体的粉体和玻璃两种材料形态的结构和光致发光性质的关系进行了研究，获得了如下研究结果：
1.采用第一原理计算方法，研究了Ca_3Si_2O_7和Ca_2SiO_4两个荧光体基质的电子结构和光学性质，通过计算得出Ca_3Si_2O_7和Ca_2SiO_4为直接带隙，带隙宽度前者小于后者。
2.研究了绿色荧光粉Ca_2SiO_4:Eu~(2+)和橙红色荧光粉Ca_3Si_2O_7:Eu~(2+)的结构和特征发射位置的关系。结合Ca_2SiO_4和Ca_3Si_2O_7的理论带隙宽度数据和实测的X射线衍射数据和光致光谱数据，通过Van Uitert经验公式及Pauling键价理论和化学键共价性理论关联结构和光谱性质，认为Eu~(2+)在Ca_2SiO_4和Ca_3Si_2O_7基质中分别取代8配位和7配位的Ca~(2+)位置，分别发射峰值在505nm的宽带绿光和600nm的宽带橙红光。
3.研究了宽带橙红光发射的Ca_3Si_2O_7:Eu~(2+)粉及其荧光增强机理。发现添加3wt.%NH4Cl，1300℃可以获得纯相，共掺Ce3+具有基于共振能量传递机理的敏化增强效应。得出优化的Eu~(2+)的掺杂浓度为2.5%，荧光光谱显示该荧光粉的使用可以降低InGaN基白光LED色温。
4.提出了用助溶剂调控同时发射绿光Ca_2SiO_4:Eu~(2+)和橙红光的Ca_3Si_2O_7:Eu~(2+)混相荧光体的基质相成分的新方案。在400nm的蓝紫光泵浦下可以有效激发混相荧光粉，同时发射出峰值在505nm的绿光和峰值在600nm的橙红光。
5.探索了获得同时发射绿光和橙红光的混相混晶荧光体的玻璃陶瓷体的方案。发现按照(Ca_(0.99)Eu_(0.01))3Si_2O_7计量比，在固液两相区熔融淬冷可以直接得到Ca_2SiO_4:Eu~(2+)体混晶玻璃陶瓷发光体，在两相区保温时间不同，可以控制其中的β-Ca_2SiO_4球形颗粒的大小和发光性质。对基于散射理论的分析表明，荧光晶体相的折射率、大小和形貌对玻璃陶瓷发光体的光学性质密切相关。
上述荧光体的结构-发光性质关系研究结果，对于发展高显色白光LED具有重要意义；基于混晶可免除现有微米级多组分混粉的配色方案，对发展新型白光LED具有重要的应用价值。
To approach the solutions associated with the problems in phosphor blending andwhite-light quality in the present color-mix combination of blue InGaNchip/phosphor-converted white light-emitting-diodes (pc-wLED), a variety ofphase-mixed phosphors in both powder and glassceramics forms involved inCaO-SiO2system were investigated. A green-emitting phosphor Ca_2SiO_4and ared-emitting phosphor Ca_3Si_2O_7activated by europium were examined in detail,respectively. The relations of structure, photoluminescence and color-mix involvedwere investigated experimentally. The main achievements made in this work include:
1. The electronic structure and optical properties of Ca_3Si_2O_7and Ca_2SiO_4werecalculated in terms of the First Principle Calculation method. The calculatedresults showed both of host compounds exhibit in direct band gap while theformer is smaller than the later.
2. A relationship between atomic structure of host and characteristicphotoluminescence properties of green-emitting phosphor Ca_2SiO_4: Eu~(2+)and thatof the orange-red-emitting phosphor Ca_3Si_2O_7: Eu~(2+)were investigated.Integrating the information of calculated results of band gaps, XRD andphotoluminescence spectra, the calculated lower energy edge position from VanUitert formula, Pauling bond valence and covalent bonding theory as well, wedraw the conclusion that Eu~(2+)substitutes for Ca~(2+)at the sites in8-coordination inCa_2SiO_4lattice to emit a505nm-peaked broad band green light, while that in7-coordination to give out600nm-peaked reddish orange band emission.
3. The orange-red-emitting Ca_3Si_2O_7: Eu~(2+)in pure phase was particularlyinvestigated by the addition of flux NH4Cl in an amount of3wt. percent at1300°C. It was found that the co-doping of Ce3+ions has an enhancement effecton the luminescent intensity of Eu~(2+)in a resonance energy transfer. A suitabledoping concentration of Eu~(2+)was optimized to be around2.5wt. percent. Thefeatured photoluminescence spectral properties indicate that this phosphor ispotential to be used to lower the color temperature of white-light as combinedwith blue InGaN chips.
4. A strategy was proposed further for Ca_3Si_2O_7-Ca_2SiO_4phopshor system that a color-mix combination of simultaneously green-emitting from Ca_2SiO_4:Eu~(2+)andorange-red-emitting from Ca_3Si_2O_7:Eu~(2+)can be achieved through adjusting thephase-mixed composition by changing the flux amount of NH4Cl. The phosphorceramics can be pumped effectively by400nm blue and violet light to emit thedual light simultaneously.
5. A new variety of glass ceramics phosphor that contains crystallite-mixed phaseswith both green and the orange-red emissions was explored primarily. It wasfound that in the designed heating process, starting with raw material in thenominal composition of (Ca_(0.99)Eu_(0.01))3Si_2O_7, a direct glass ceramics with Ca_2SiO_4:Eu~(2+)crystal was obtained through melt-quenching method in terms of asolid-liquid (SL) two-phase region of CaO-SiO2binary phase diagram. The meansize of spherical β-Ca_2SiO_4crystal in microsize and different luminescenceproperties were found to be varied with the holding time in SL two-phase region.Based on scattering theory, a trade-off of the luminescence and optical propertiesare discussed by closely associating with refractive index, size and morphology ofluminous crystal phase in glass.
The results of structure-property relation we obtained above could be ofscientifical significance in developing some new phosphors for pc-wLED withhigher color rendering index, while those phase-mixed phosphors in both powderand glass ceramics forms are of potential in the application of WLED packagingprocess with blending–free color-mix operation as compared to the present powdermix with multicomponent phosphors in microsize.
1.采用第一原理计算方法，研究了Ca_3Si_2O_7和Ca_2SiO_4两个荧光体基质的电子结构和光学性质，通过计算得出Ca_3Si_2O_7和Ca_2SiO_4为直接带隙，带隙宽度前者小于后者。
2.研究了绿色荧光粉Ca_2SiO_4:Eu~(2+)和橙红色荧光粉Ca_3Si_2O_7:Eu~(2+)的结构和特征发射位置的关系。结合Ca_2SiO_4和Ca_3Si_2O_7的理论带隙宽度数据和实测的X射线衍射数据和光致光谱数据，通过Van Uitert经验公式及Pauling键价理论和化学键共价性理论关联结构和光谱性质，认为Eu~(2+)在Ca_2SiO_4和Ca_3Si_2O_7基质中分别取代8配位和7配位的Ca~(2+)位置，分别发射峰值在505nm的宽带绿光和600nm的宽带橙红光。
3.研究了宽带橙红光发射的Ca_3Si_2O_7:Eu~(2+)粉及其荧光增强机理。发现添加3wt.%NH4Cl，1300℃可以获得纯相，共掺Ce3+具有基于共振能量传递机理的敏化增强效应。得出优化的Eu~(2+)的掺杂浓度为2.5%，荧光光谱显示该荧光粉的使用可以降低InGaN基白光LED色温。
4.提出了用助溶剂调控同时发射绿光Ca_2SiO_4:Eu~(2+)和橙红光的Ca_3Si_2O_7:Eu~(2+)混相荧光体的基质相成分的新方案。在400nm的蓝紫光泵浦下可以有效激发混相荧光粉，同时发射出峰值在505nm的绿光和峰值在600nm的橙红光。
5.探索了获得同时发射绿光和橙红光的混相混晶荧光体的玻璃陶瓷体的方案。发现按照(Ca_(0.99)Eu_(0.01))3Si_2O_7计量比，在固液两相区熔融淬冷可以直接得到Ca_2SiO_4:Eu~(2+)体混晶玻璃陶瓷发光体，在两相区保温时间不同，可以控制其中的β-Ca_2SiO_4球形颗粒的大小和发光性质。对基于散射理论的分析表明，荧光晶体相的折射率、大小和形貌对玻璃陶瓷发光体的光学性质密切相关。
上述荧光体的结构-发光性质关系研究结果，对于发展高显色白光LED具有重要意义；基于混晶可免除现有微米级多组分混粉的配色方案，对发展新型白光LED具有重要的应用价值。
To approach the solutions associated with the problems in phosphor blending andwhite-light quality in the present color-mix combination of blue InGaNchip/phosphor-converted white light-emitting-diodes (pc-wLED), a variety ofphase-mixed phosphors in both powder and glassceramics forms involved inCaO-SiO2system were investigated. A green-emitting phosphor Ca_2SiO_4and ared-emitting phosphor Ca_3Si_2O_7activated by europium were examined in detail,respectively. The relations of structure, photoluminescence and color-mix involvedwere investigated experimentally. The main achievements made in this work include:
1. The electronic structure and optical properties of Ca_3Si_2O_7and Ca_2SiO_4werecalculated in terms of the First Principle Calculation method. The calculatedresults showed both of host compounds exhibit in direct band gap while theformer is smaller than the later.
2. A relationship between atomic structure of host and characteristicphotoluminescence properties of green-emitting phosphor Ca_2SiO_4: Eu~(2+)and thatof the orange-red-emitting phosphor Ca_3Si_2O_7: Eu~(2+)were investigated.Integrating the information of calculated results of band gaps, XRD andphotoluminescence spectra, the calculated lower energy edge position from VanUitert formula, Pauling bond valence and covalent bonding theory as well, wedraw the conclusion that Eu~(2+)substitutes for Ca~(2+)at the sites in8-coordination inCa_2SiO_4lattice to emit a505nm-peaked broad band green light, while that in7-coordination to give out600nm-peaked reddish orange band emission.
3. The orange-red-emitting Ca_3Si_2O_7: Eu~(2+)in pure phase was particularlyinvestigated by the addition of flux NH4Cl in an amount of3wt. percent at1300°C. It was found that the co-doping of Ce3+ions has an enhancement effecton the luminescent intensity of Eu~(2+)in a resonance energy transfer. A suitabledoping concentration of Eu~(2+)was optimized to be around2.5wt. percent. Thefeatured photoluminescence spectral properties indicate that this phosphor ispotential to be used to lower the color temperature of white-light as combinedwith blue InGaN chips.
4. A strategy was proposed further for Ca_3Si_2O_7-Ca_2SiO_4phopshor system that a color-mix combination of simultaneously green-emitting from Ca_2SiO_4:Eu~(2+)andorange-red-emitting from Ca_3Si_2O_7:Eu~(2+)can be achieved through adjusting thephase-mixed composition by changing the flux amount of NH4Cl. The phosphorceramics can be pumped effectively by400nm blue and violet light to emit thedual light simultaneously.
5. A new variety of glass ceramics phosphor that contains crystallite-mixed phaseswith both green and the orange-red emissions was explored primarily. It wasfound that in the designed heating process, starting with raw material in thenominal composition of (Ca_(0.99)Eu_(0.01))3Si_2O_7, a direct glass ceramics with Ca_2SiO_4:Eu~(2+)crystal was obtained through melt-quenching method in terms of asolid-liquid (SL) two-phase region of CaO-SiO2binary phase diagram. The meansize of spherical β-Ca_2SiO_4crystal in microsize and different luminescenceproperties were found to be varied with the holding time in SL two-phase region.Based on scattering theory, a trade-off of the luminescence and optical propertiesare discussed by closely associating with refractive index, size and morphology ofluminous crystal phase in glass.
The results of structure-property relation we obtained above could be ofscientifical significance in developing some new phosphors for pc-wLED withhigher color rendering index, while those phase-mixed phosphors in both powderand glass ceramics forms are of potential in the application of WLED packagingprocess with blending–free color-mix operation as compared to the present powdermix with multicomponent phosphors in microsize.
引文
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