Li_2O-SrO-B_2O_3玻璃中Sm~（3+）、Eu~（3+）的还原、发光和微结构研究
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摘要
Sm~(2+)离子可以实现永久光谱烧孔,对高密度光存储具有潜在的的应用前景。Eu~(2+)离子可以根据基质的不同发出深红至紫外的各种光,使之在照明和显示领域得到广泛应用。常规得到Sm~(2+)、Eu~(2+)离子的主要方法是在还原气氛中进行高温还原,要求试验条件苛刻,所以空气气氛下的反常还原和高能射线辐照还原成为广受关注的新型方法。
本论文选择了硼酸盐玻璃作为基质材料,目标是研究Eu~(3+)、Sm~(3+)在Li_2O-SrO-B_2O_3玻璃和玻璃陶瓷中的还原、X射线辐照还原效应、Sm~(2+)和Eu~(2+)离子的发光性能、Sm~(2+)离子的室温光谱烧孔:运用发光表征阐述还原机理、对光谱烧孔、光稳定性、玻璃微结构等进行探讨。
第三章论述了Li_2O-SrO-B_2O_3玻璃陶瓷中Eu~(3+)反常还原(空气气氛),以及F离子对还原的影响。制备了Eu~(3+)掺杂的Li_2O-SrO-B_2O_3玻璃,通过空气气氛下退火再结晶制得相应的玻璃陶瓷,并实现了Eu~(2+)离子的反常还原。Eu~(3+)不等价取代Sr~(2+)后产生了带负电的Sr空穴,负电荷转移至Eu~(3+)处后使其还原为Eu~(2+)。BO_4基团形成刚性的网络结构,使Eu~(2+)离子不被氧化。F~-离子可以增加Li_2O-SrO-B_2O_3原生玻璃中带负电荷的V_(Sr)”缺陷,有利于提高还原效率。
第四章实现了Sm~(2+)离子的室温光谱烧孔并探讨烧孔机理。得到的光谱孔宽度为2.5 cm~(-1),深度为40%(与总发光强度比)。其机理为光致电离的电子在Sm~(3+)离子外的其他缺陷位置被俘获,从而导致光谱中特定位置的变化。Sm~(2+)的发光寿命随温度增加而降低。
第五章研究了Sm~(2+)的X射线辐照还原和玻璃的微观结构。Sm~(2+)的还原程度与X射线辐照时间线性相关。光稳定性测试表明,光发射强度的减少是因为光学缺陷中心造成的。Sm~(2+)离子相关的缺陷呈现两种不同类型的陷阱特性,即玻璃中有至少两种与Sm~(2+)离子相关的缺陷。X射线辐照形成的缺陷中心被认为是非桥氧空穴心和硼氧空穴心。非桥氧空穴心主要受玻璃组成和辐照强度的影响。Sm离子被硼氧基的桥氧和非桥氧包围。负电荷分布于BO_4四面体上,而Li~+离子则在临近区域实现电荷补偿。
为了进一步了解Eu~(3+)离子在红光发光材料方面的应用,第六章中对Eu~(3+)掺杂的Ca_3Zn_3(TeO_6)_2合成和发光性能进行了初步研究。其可被395 nm或465 nm蓝光激发。这与紫外或蓝光LED输出波长相匹配,且在611 nm处有源于~5Do→~7F_2跃迁的强烈红光发射,说明其具有成为新型红色荧光粉的良好潜质。
本论文创新点是在Li_2O-SrO-B_2O_3玻璃陶瓷中成功实现了Eu~(2+)和Sm~(2+)在氧化气氛下的还原,并首次报道了X射线辐照剂量关系、玻璃微结构、室温永久光谱烧孔,有较高的创新价值。这些对于Li_2O-SrO-B_2O_3玻璃和玻璃陶瓷的进一步应用、稀土离子的还原方法发展、Sm~(2+)和Eu~(2+)离子的应用等方面都具有参考借鉴和实际应用价值。
Sm~(2+) ion has potential application in high-density optical storage because of its property of persistent spectral hole burning (PSHB). The luminescence of Eu~(2+) strongly depends on the host, which may lie anywhere from the UV to the deep-red region of the electromagnetic spectrum. Eu~(2+) has been widely used in the field of luminescence and display. The most widely used reduction method for these two ions is to heat the samples under a highly reduced atmosphere. It needs more strict operation conditions while the request of reduction in air and reduction by X-ray radiation are easier.
The main topic in this work is to realize reduction of Eu~(2+), Sm~(2+) in Li_2O-SrO-B_2O_3as-made glass and glass-ceramics by heat-treatment in air and by X-ray radiation. The luminescence spectra, delay curves were measured for the reduced Eu~(2+) and Sm~(2+) ions. The optical stability of Sm~(2+) ions was evaluated by photo-bleaching method. The PSHB at room-temperature was onserved in Sm~(2+)-doped glass-ceramics. The microstructure of Li_2O-SrO-B_2O_3 as-made glass are studied.
In the chapter three, Eu-doped Li_2O-SrO-B_2O_3 as-made glasses were prepared by high-temperature melting quenching; the glass-ceramics were obtained by heating the as-made glasses in air. The abnormal reduction of Eu~(2+) doped in Li_2O-SrO-B_2O_3 glass-ceramics crystallizied in air was studied. Moreover, F~- ions had a positive influence on the reduction of Eu~(3+) to Eu~(2+) ions. Reduction of the Eu~(3+) to Eu~(2+) could occur in the process of crystallization of the glass-ceramics in air. When trivalent Eu~(3+) occupied the lattice site of divalent Sr~(2+),vacancy defects of Sr were created. The negative charges could transfer to Eu~(3+) site in resulting the reduction of Eu~(2+).The rigid three-dimensional networks of BO_4 tetrahedral act as a shield partially isolate the Eu~(2+) ions from each other and resist the attack of oxygen. There were two luminescence centers of Eu~(2+) ions.
In the chapter four, PSHB of Sm~(2+) ions at room temperature was realized and the burning mechanism was studied. The width and depth of the obtained spectral hole were 2.5 cm~(-1) and 40 % of the total intensity, respectively. This result was better than the reported PSHB results in the reference for borates. The burning mechanism was the photoionization of electron trapped at a site other than the Sm~(3+) ions. The lifetime of Eu~(2+) ions emission decreased with increasing of temperature.
In the chapter five, the photo-reduction of Sm~(3+) to Sm~(2+) ions by X-ray irradiation was observed. The microstructure of the as-made borate-glass was studied. The dependence of Sm~(2+) reducing efficiency on the X-ray irradiation time showed a linear relationship. The related defects of Sm~(2+) ions showed two different types of trap characteristics. The reducing mechanism by X-ray irradiation was explained by the trapping of the free electrons created by X-ray irradiation by the metal cations or structural defects due to Sm~(3+) ions. The radiation induced defect centers were porposed to be boron electron centers, (NBOHC), and boron oxygen hole centers (BOHC). The NBOHCs are mainly dependent on the components of the glass and the irradiation intensity. The existence of Li atoms in the glass provide non-bridging oxygen in borate groups which leads to a higher optical basicity (electron donor power). It can be suggested that the samarium ions are mainly surrounded by non-bridging oxygen and bridging oxygen of the borate groups. The negative charge is distributed on BO_4 tetrahedral and the Li~+ ions can act as charge compensation in the near location.
In the chapter five, a novel red-emitting phosphor Eu~(3+)-doped Ca_3Zn_3(TeO_6)_2,a Garnet type calcium-tellurium-zinc oxide was synthesized by the general high temperature solid-state reaction in air atmosphere. Ca_3Zn_3(TeO_6)_2:Eu~+ can be effectively excited by UV-visible light 395, 465 and 537 nm.This phosphor exhibits an intense red emission at 611 nm. The wavelengths at 395 and 465 nm can match with the widely applied output wavelengths of ultraviolet or blue LED chips. The long-wavelength excitation properties of this material have benefit as a red phosphor for application of white light-emitting diodes.
The novelties of this desertation are the following: the abnormal reduction Eu~(3+), Sm~(3+) to their bivalent states were realized by crystallization of this as-made glasses in air atmosphere. The microstructure of the borate glass, photoreduction by X-ray irradiation, PSHB of Sm~(2+) ions at room-temperature in this borate glasses were first reported. These results are helpful in further research of Li_2O-SrO-B_2O_3 glasses and glass-ceramics. And this also are good references for the reduction of rare-earth ions and applications of Sm~(2+),Eu~(2+) ions.
本论文选择了硼酸盐玻璃作为基质材料,目标是研究Eu~(3+)、Sm~(3+)在Li_2O-SrO-B_2O_3玻璃和玻璃陶瓷中的还原、X射线辐照还原效应、Sm~(2+)和Eu~(2+)离子的发光性能、Sm~(2+)离子的室温光谱烧孔:运用发光表征阐述还原机理、对光谱烧孔、光稳定性、玻璃微结构等进行探讨。
第三章论述了Li_2O-SrO-B_2O_3玻璃陶瓷中Eu~(3+)反常还原(空气气氛),以及F离子对还原的影响。制备了Eu~(3+)掺杂的Li_2O-SrO-B_2O_3玻璃,通过空气气氛下退火再结晶制得相应的玻璃陶瓷,并实现了Eu~(2+)离子的反常还原。Eu~(3+)不等价取代Sr~(2+)后产生了带负电的Sr空穴,负电荷转移至Eu~(3+)处后使其还原为Eu~(2+)。BO_4基团形成刚性的网络结构,使Eu~(2+)离子不被氧化。F~-离子可以增加Li_2O-SrO-B_2O_3原生玻璃中带负电荷的V_(Sr)”缺陷,有利于提高还原效率。
第四章实现了Sm~(2+)离子的室温光谱烧孔并探讨烧孔机理。得到的光谱孔宽度为2.5 cm~(-1),深度为40%(与总发光强度比)。其机理为光致电离的电子在Sm~(3+)离子外的其他缺陷位置被俘获,从而导致光谱中特定位置的变化。Sm~(2+)的发光寿命随温度增加而降低。
第五章研究了Sm~(2+)的X射线辐照还原和玻璃的微观结构。Sm~(2+)的还原程度与X射线辐照时间线性相关。光稳定性测试表明,光发射强度的减少是因为光学缺陷中心造成的。Sm~(2+)离子相关的缺陷呈现两种不同类型的陷阱特性,即玻璃中有至少两种与Sm~(2+)离子相关的缺陷。X射线辐照形成的缺陷中心被认为是非桥氧空穴心和硼氧空穴心。非桥氧空穴心主要受玻璃组成和辐照强度的影响。Sm离子被硼氧基的桥氧和非桥氧包围。负电荷分布于BO_4四面体上,而Li~+离子则在临近区域实现电荷补偿。
为了进一步了解Eu~(3+)离子在红光发光材料方面的应用,第六章中对Eu~(3+)掺杂的Ca_3Zn_3(TeO_6)_2合成和发光性能进行了初步研究。其可被395 nm或465 nm蓝光激发。这与紫外或蓝光LED输出波长相匹配,且在611 nm处有源于~5Do→~7F_2跃迁的强烈红光发射,说明其具有成为新型红色荧光粉的良好潜质。
本论文创新点是在Li_2O-SrO-B_2O_3玻璃陶瓷中成功实现了Eu~(2+)和Sm~(2+)在氧化气氛下的还原,并首次报道了X射线辐照剂量关系、玻璃微结构、室温永久光谱烧孔,有较高的创新价值。这些对于Li_2O-SrO-B_2O_3玻璃和玻璃陶瓷的进一步应用、稀土离子的还原方法发展、Sm~(2+)和Eu~(2+)离子的应用等方面都具有参考借鉴和实际应用价值。
Sm~(2+) ion has potential application in high-density optical storage because of its property of persistent spectral hole burning (PSHB). The luminescence of Eu~(2+) strongly depends on the host, which may lie anywhere from the UV to the deep-red region of the electromagnetic spectrum. Eu~(2+) has been widely used in the field of luminescence and display. The most widely used reduction method for these two ions is to heat the samples under a highly reduced atmosphere. It needs more strict operation conditions while the request of reduction in air and reduction by X-ray radiation are easier.
The main topic in this work is to realize reduction of Eu~(2+), Sm~(2+) in Li_2O-SrO-B_2O_3as-made glass and glass-ceramics by heat-treatment in air and by X-ray radiation. The luminescence spectra, delay curves were measured for the reduced Eu~(2+) and Sm~(2+) ions. The optical stability of Sm~(2+) ions was evaluated by photo-bleaching method. The PSHB at room-temperature was onserved in Sm~(2+)-doped glass-ceramics. The microstructure of Li_2O-SrO-B_2O_3 as-made glass are studied.
In the chapter three, Eu-doped Li_2O-SrO-B_2O_3 as-made glasses were prepared by high-temperature melting quenching; the glass-ceramics were obtained by heating the as-made glasses in air. The abnormal reduction of Eu~(2+) doped in Li_2O-SrO-B_2O_3 glass-ceramics crystallizied in air was studied. Moreover, F~- ions had a positive influence on the reduction of Eu~(3+) to Eu~(2+) ions. Reduction of the Eu~(3+) to Eu~(2+) could occur in the process of crystallization of the glass-ceramics in air. When trivalent Eu~(3+) occupied the lattice site of divalent Sr~(2+),vacancy defects of Sr were created. The negative charges could transfer to Eu~(3+) site in resulting the reduction of Eu~(2+).The rigid three-dimensional networks of BO_4 tetrahedral act as a shield partially isolate the Eu~(2+) ions from each other and resist the attack of oxygen. There were two luminescence centers of Eu~(2+) ions.
In the chapter four, PSHB of Sm~(2+) ions at room temperature was realized and the burning mechanism was studied. The width and depth of the obtained spectral hole were 2.5 cm~(-1) and 40 % of the total intensity, respectively. This result was better than the reported PSHB results in the reference for borates. The burning mechanism was the photoionization of electron trapped at a site other than the Sm~(3+) ions. The lifetime of Eu~(2+) ions emission decreased with increasing of temperature.
In the chapter five, the photo-reduction of Sm~(3+) to Sm~(2+) ions by X-ray irradiation was observed. The microstructure of the as-made borate-glass was studied. The dependence of Sm~(2+) reducing efficiency on the X-ray irradiation time showed a linear relationship. The related defects of Sm~(2+) ions showed two different types of trap characteristics. The reducing mechanism by X-ray irradiation was explained by the trapping of the free electrons created by X-ray irradiation by the metal cations or structural defects due to Sm~(3+) ions. The radiation induced defect centers were porposed to be boron electron centers, (NBOHC), and boron oxygen hole centers (BOHC). The NBOHCs are mainly dependent on the components of the glass and the irradiation intensity. The existence of Li atoms in the glass provide non-bridging oxygen in borate groups which leads to a higher optical basicity (electron donor power). It can be suggested that the samarium ions are mainly surrounded by non-bridging oxygen and bridging oxygen of the borate groups. The negative charge is distributed on BO_4 tetrahedral and the Li~+ ions can act as charge compensation in the near location.
In the chapter five, a novel red-emitting phosphor Eu~(3+)-doped Ca_3Zn_3(TeO_6)_2,a Garnet type calcium-tellurium-zinc oxide was synthesized by the general high temperature solid-state reaction in air atmosphere. Ca_3Zn_3(TeO_6)_2:Eu~+ can be effectively excited by UV-visible light 395, 465 and 537 nm.This phosphor exhibits an intense red emission at 611 nm. The wavelengths at 395 and 465 nm can match with the widely applied output wavelengths of ultraviolet or blue LED chips. The long-wavelength excitation properties of this material have benefit as a red phosphor for application of white light-emitting diodes.
The novelties of this desertation are the following: the abnormal reduction Eu~(3+), Sm~(3+) to their bivalent states were realized by crystallization of this as-made glasses in air atmosphere. The microstructure of the borate glass, photoreduction by X-ray irradiation, PSHB of Sm~(2+) ions at room-temperature in this borate glasses were first reported. These results are helpful in further research of Li_2O-SrO-B_2O_3 glasses and glass-ceramics. And this also are good references for the reduction of rare-earth ions and applications of Sm~(2+),Eu~(2+) ions.
引文
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