Al_2O_3-B_2O_3-SiO_2系统光功能玻璃制备、结构及性能研究
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摘要
Al_2O_3-B_2O_3-SiO_2系统玻璃是一种重要的无机材料,其具有良好的理化性能,且原料简单易得,因而在日用化工、信息显示、核废料处理等方面有着广泛的用途。本文工作以Al_2O_3-B_2O_3-SiO_2系统玻璃为基质,一方面旨在研究解决在防火、信息显示、光伏等节能方面有重要用途的微型浮法低铝高硼硅平板玻璃若干技术难点,另一方面旨在开发出一种具有优良热稳定性、可在紫外光激发下发射出白光的在白光LED领域有潜在用途的稀土离子掺杂发光玻璃。
本文首先全面回顾了Al_2O_3-B_2O_3-SiO_2系统玻璃结构研究、微型浮法技术制备低铝高硼硅平板玻璃现状及白光发光玻璃的研究进展。在此基础上,用高温熔融-退火、淬火及热处理方法制备了低铝高硼硅玻璃、稀土离子掺杂发光玻璃和稀土离子掺杂氟氧微晶发光玻璃。并用X射线衍射、透射电子显微镜、固体核磁共振、红外光谱、X光电子能谱、差热分析及荧光光谱等手段分析了其微观结构、光学及热学等性能。具体研究内容和主要结果如下:
(1)研究了温度制度对高温熔融-退火制备低铝高硼硅玻璃的影响,获得了熔化质量好、热膨胀系数低、可见光透过率极高的轻质低铝高硼硅玻璃。研究在低铝高硼硅玻璃中引入混合碱土金属氧化物对其析晶性能的影响,结果表明引入混合碱土金属氧化物能在一定程度上降低析晶倾向。利用静态浮法模拟装置对微型浮法制备低铝高硼硅玻璃表面渗锡状态进行了研究,结果表明浮法热处理温度高于850℃时,SEM照片中可观察到一典型渗锡层,渗锡的深度随着浮法热处理温度从850℃上升到950℃而增大,但当进一步升高浮法热处理温度从950℃到1050℃,渗锡深度反而下降。
(2)利用高温熔融-退火方法,选择合适的温度制度,在铝硼硅酸盐玻璃中共掺Eu-Dy及Tm-Dy离子,实现了这两个系列样品在紫外光激发下的白光发射。同时,研究了稀土离子掺杂浓度比、稀土离子共掺浓度及激发光波长对白光发光色度和强度的影响。之后,进一步研究了玻璃基体组分对Tm-Dy共掺铝硼硅酸盐玻璃白光发光性能的影响,结果表明,改变玻璃基体组分对玻璃白光发光色度影响较小,其白光发射色度基本稳定。研究了Tm-Dy共掺玻璃受激时各激发能级间跃迁机制,结果表明Tm-Dy之间可能存在一个Tm~(3+)→Dy~(3+)的能量传递过程,该能量传递几率受Tm-Dy离子在玻璃基质中分散程度影响。另一方面,在530℃经过2～32 h热处理后的Tm-Dy共掺玻璃仍保持了稳定的白光发光色度,同时其发光强度并没有出现明显降低,说明其具有一定热稳定性。
(3)在空气气氛下通过高温熔融-退火方法制备Eu_2O_3掺杂铝硼硅酸盐玻璃,实现了在非还原气氛下Eu~(3+)→Eu~(2+)的还原。由于Eu~(3+)离子和Eu~(2+)离子分别为可合成白光的三原色光——红光和蓝光的重要发光离子,因此,本工作中还系统研究了该氧化还原反应的影响因素,如玻璃网络修饰体阳离子、网络中间体阳离子、网络形成体阳离子、热处理制度等对其的影响。结果表明,玻璃基质光碱度和玻璃三维网络结构在此扮演主要角色。随着玻璃光碱度的降低及三维网络结构完整度提高,Eu还原程度增强。同时,在引入的一价网络修饰阳离子与二价网络修饰阳离子的对应氧化物光碱度一致时,二价阳离子的存在更有利于Eu还原反应的进行。
(4)进一步研究了网络阴离子对铝硼硅酸盐玻璃基质中Eu在空气中还原反应的影响。利用高温熔融-淬火方法在空气气氛中制备了Eu_2O_3掺杂氟氧铝硼硅酸盐玻璃,发现在玻璃内部发生了Eu~(3+)→Eu~(2+)的还原反应。该还原反应随着玻璃内F~-/O~(2-)离子含量比例的增大而增强,其原因与不同网络阴离子的电负性不同带来的玻璃基质“电子施主能力”的改变有关,引入玻璃基质的网络阴离子电负性增强,玻璃基质的“电子施主能力”降低,从而有助于Eu还原反应。
(5)研究了稀土离子掺杂氟氧铝硼硅酸盐玻璃及微晶玻璃的制备、结构及性能。在空气气氛下通过高温熔融-淬火/热处理方法制备Eu_2O_3掺杂氟氧铝硼硅酸盐玻璃及微晶玻璃。研究了热处理温度和时间对Eu_2O_3掺杂氟氧铝硼硅酸盐玻璃析晶行为和光学性能的影响。选择合适的热处理温度和时间得到了Ba_2LaF_7微晶相析出的透明氟氧化物微晶玻璃。该微晶化行为对Eu_2O_3掺杂玻璃的发光性能产生一定影响,改变了Eu~(2+)和Eu~(3+)发射峰强度比例。另一方面,研究了Eu_2O_3掺杂浓度对氟氧铝硼硅酸盐微晶玻璃结构及光学性能的影响。随着Eu_2O_3含量增加,La_2O_3含量降低,Ba_2LaF_7析晶倾向减弱,淬火样和热处理样的Eu~(2+)和Eu~(3+)发射峰强度比例变化程度减弱。同时Eu_2O_3掺杂较低时,热处理后的玻璃可观察到Eu~(3+)离子的~5D_1→~7F_2跃迁发射,但在高浓度Eu_2O_3掺杂时,~5D_1→~7F_2跃迁发射消失。
(6)研究了微晶化行为对稀土离子掺杂氟氧铝硼硅酸盐白光发光玻璃的影响。通过高温熔融-淬火/热处理方法在空气气氛中制备了Tm_2O_3和Dy_2O_3共掺氟氧铝硼硅酸盐玻璃及透明微晶玻璃。热处理过程会影响玻璃的发光强度,但不影响白光发射的色度。同时增大Tm-Dy共掺浓度时,Ba_2LaF_7析晶倾向降低。此外,Tm_2O_3和Dy_2O_3共掺浓度淬灭点可由原淬火样的1 mol.%提高到热处理样的2 mol.%,白光发光色度保持不变。
Al_2O_3-B_2O_3-SiO_2 glass was one of important inorganic materials.It possessed good physical and chemical properties,and the raw materlas are cheap.Therefore,it had wide application in chemical engineering,information display,and nuclear waste treatment and so on.This work introduced Al_2O_3-B_2O_3-SiO_2 glass system as the matrix,and focused on two research points.One point was to solve some technical problems of flat alumino-borosilicate glass prepared by micro-float process,which had important energy saving application in fire-resistance,information display and photovoltaics.The other point was to develop a kind of rare earth ions doped luminescence glasses which possessed good thermal stability,could emit white ligh under UV-light excitation and had potaintial application in White-LED area.
First,this thesis reviewd the studies of three aspects as following:(ⅰ) the structure investigations of Al_2O_3-B_2O_3-SiO_2 glasses,(ⅱ) the investigations of flat alumino-borosilicate glasses prepared by micro-float method,and(ⅲ) the investigation progress of white ligh emission glasses.Second,the alumino-borosilcate glasses,rare earth ions doped luminescence aluminoborosilicate glasses and rare earth ions doped luminescence oxyfluoride aluminoborosilicate glass ceramics were prepared by melting-annealing/quenching/thermal treatment method.The micro-structure,optical and thermal properties were mearsured by XRD,TEM,NMR,IR,XPS,DTA,PL and so on.The details were listed as following:
(1) The effects of temperature system on preparation of alumino-borosilcate glasses by melting and annealing method were investigated.The alumino-boroslicate glasses with good melting quality,low coefficient of thermal expansion,high transmission of visible ligh,and low density were prepared.The effects of mixed alkaline earth oxides on crystallization property of alumino-borosilicate glasses were also investigated.The results indicated that the crystallization degree was reduced by introducing mixed alkaline earth oxides to alumino-borosilicate glasses.The tin penetration at bottom surface of float alumino-borosilicate glasses was studied by a lab-scale float apparatus.SEM image showed that a typical tin penetration layer could be detected above 850℃.The tin penetration depth increased with increasing reaction temperature from 850 to 950℃,while it decreased with further increasing reaction temperature from 950℃to 1050℃.
(2) Two serieses samples of Eu-Dy and Tm-Dy ions co-doped aluminoborosilicate glasses were prepared by melting-annealing method with appropriate temperature system.The two serieses samples emited white light under UV light excitation.Meanwhile,the effects of concentration ratio among different rare earth ions,total concentration of rare earth ions and excitation wavelength on chrominance of white ligh emission were investigated in this work. The effects of glass matrix composition on white light huninescence properties of Tm-Dy ions co-doped aluminoborosilicate glasses were studied in the thesis.The results showed that the chroinance of white light emission was not affected by changing glasses matrix composition and the chroinance of white light emission is stable.The transition mechanism between different excitation energy levels in Tm-Dy ions co-doped aluminoborosilicate glasses was also studied.It indicated that an energy transfer progress of Tm~(3+)→Dy~(3+) may exsit between Tm-Dy ions.The probability of the energy transfer progress could be affected by the separation degree of Tm-Dy ions in glass matrix.On the other hand,the chrominance of white ligh emission is stable even though the Tm-Dy co-doped aluminoborosilicate glass had been thermally treated on 530℃for 2～32 h,and the luminescence intensity of the samples did not decrease after thermal treatment.It indicated that the glass possessed good thermal stability.
(3) Eu_2O_3 doped aluminoborosilicate glasses were prepared by melting-annealing method in air.The reduction of Eu~(3+)→Eu~(2+) was observed the samples prepared in air atmosphere. Since Eu~(3+) and Eu~(2+) ions were important actors of red and blue light emission which could synthesize white light,the effects of network modifier cations,network former cantions and thermal treatment on the reduction reaction were systematically investigated in the work. The results showed that the optical basicity of glass matrix and three dimension network structure of glass played important roles in the reduction reaction.The reduction degree was enhanced by the decrease of glass optical basicity and the stabilization of glass three dimension network structures.Meanwhile,when the optical basicity of introduced univalent network modifier cations was equal to that of bivalent network modifier cations,the existence of bivalent network modifier cations was more benefit for the Eu reduction in air.
(4) Futhermore,the effects of network anions on the Eu reduction in aluminoborosilicate glasses prepared in air were investigated in this thesis.Eu_2O_3 doped oxyfluoride aluminoborosilicate glasses were prepared by melting-quenching method in air.The reduction of Eu~(3+)→Eu~(2+) was observed in the samples prepared in air atmosphere.The Eu reduction reaction was enhanced by the increase of concentration ratio between F~-/O~(2-) ions. The effects were related with the changing of "electron donor powers" of glass matrix with different network anions.The "electron donor powers" of glass matrix would decrease with increasing of the electronegetivity of network anions,which resulted in preferable of Eu reduction.
(5) The preparation,structures and properties of rare earth ions doped oxyfluoride aluminoborosilicate glasses and glass ceramics were investigated in this thesis.The Eu_2O_3 doped oxyfluoride aluminoborosilicate glasses and glass ceramics were prepared by melting-quenching and melting-thermal treatment method in air.The effects of thermal treatment temperature and time on the crystallization behavior and optical properties of Eu_2O_3 doped oxyfluoride aluminoborosilicate glasses were investigated.Transparent oxyfluoride aluminoborosilicate glass ceramics with Ba_2LaF_7 micro-crystalline were obtained by thermal treatment under appropriate temperature and time.The crystallization behavior affected the optical properties of Eu_2O_3 doped glasses to some extent.The emission intensity ratio between Eu~(2+) and Eu~(3+) ions was changed with crystallization behavior.Moreover,the effects of Eu_2O_3 concentration on the crystallization behavior and optical properties of oxyfluoride aluminoborosilicate glasses were studied.The Ba_2LaF_7 crystallization degree decreased with the increase of Eu_2O_3 concentration and decrease of La_2O_3 concentration.Meanwhile,the degree of variation of emission intensity ratio between Eu~(2+) and Eu~(3+) ions decreased.The ~5D_1→~7F_2 transition emission was observed in the samples been thermally treated with low Eu_2O_3 concentration,while it could not be observed in the samples with high Eu_2O_3 concentration.
(6) The effects of crystallization behavior on the rare earth ions doped oxyfluoride aluminoborosilicate white light emission glasses were investigated.The Tm_2O_3 and Dy_2O_3 co-doped oxyfluoride aluminoborosilicate glasses and glass ceramics were prepared by melting-quenching and melting-thermal treatment method in air.The thermal treatment process affected the luminescence intensity,but it would not affect the chroinance of white light emission.The Ba_2LaF_7 crystallization degree decreased with the increase of Tm_2O_3 and Dy_2O_3 co-doping concentration and decrease of La_2O_3 concentration.Moreover,the Tm_2O_3 and Dy_2O_3 co-doping concemtration quenching point of quenched samples was about 1 mol.%, and that of thermal treated samles was 2 mol.%.Meanwhile,the chroinance of white light cmission was stable with different Tm_2O_3 and Dy_2O_3 co-doping concentration.
本文首先全面回顾了Al_2O_3-B_2O_3-SiO_2系统玻璃结构研究、微型浮法技术制备低铝高硼硅平板玻璃现状及白光发光玻璃的研究进展。在此基础上,用高温熔融-退火、淬火及热处理方法制备了低铝高硼硅玻璃、稀土离子掺杂发光玻璃和稀土离子掺杂氟氧微晶发光玻璃。并用X射线衍射、透射电子显微镜、固体核磁共振、红外光谱、X光电子能谱、差热分析及荧光光谱等手段分析了其微观结构、光学及热学等性能。具体研究内容和主要结果如下:
(1)研究了温度制度对高温熔融-退火制备低铝高硼硅玻璃的影响,获得了熔化质量好、热膨胀系数低、可见光透过率极高的轻质低铝高硼硅玻璃。研究在低铝高硼硅玻璃中引入混合碱土金属氧化物对其析晶性能的影响,结果表明引入混合碱土金属氧化物能在一定程度上降低析晶倾向。利用静态浮法模拟装置对微型浮法制备低铝高硼硅玻璃表面渗锡状态进行了研究,结果表明浮法热处理温度高于850℃时,SEM照片中可观察到一典型渗锡层,渗锡的深度随着浮法热处理温度从850℃上升到950℃而增大,但当进一步升高浮法热处理温度从950℃到1050℃,渗锡深度反而下降。
(2)利用高温熔融-退火方法,选择合适的温度制度,在铝硼硅酸盐玻璃中共掺Eu-Dy及Tm-Dy离子,实现了这两个系列样品在紫外光激发下的白光发射。同时,研究了稀土离子掺杂浓度比、稀土离子共掺浓度及激发光波长对白光发光色度和强度的影响。之后,进一步研究了玻璃基体组分对Tm-Dy共掺铝硼硅酸盐玻璃白光发光性能的影响,结果表明,改变玻璃基体组分对玻璃白光发光色度影响较小,其白光发射色度基本稳定。研究了Tm-Dy共掺玻璃受激时各激发能级间跃迁机制,结果表明Tm-Dy之间可能存在一个Tm~(3+)→Dy~(3+)的能量传递过程,该能量传递几率受Tm-Dy离子在玻璃基质中分散程度影响。另一方面,在530℃经过2～32 h热处理后的Tm-Dy共掺玻璃仍保持了稳定的白光发光色度,同时其发光强度并没有出现明显降低,说明其具有一定热稳定性。
(3)在空气气氛下通过高温熔融-退火方法制备Eu_2O_3掺杂铝硼硅酸盐玻璃,实现了在非还原气氛下Eu~(3+)→Eu~(2+)的还原。由于Eu~(3+)离子和Eu~(2+)离子分别为可合成白光的三原色光——红光和蓝光的重要发光离子,因此,本工作中还系统研究了该氧化还原反应的影响因素,如玻璃网络修饰体阳离子、网络中间体阳离子、网络形成体阳离子、热处理制度等对其的影响。结果表明,玻璃基质光碱度和玻璃三维网络结构在此扮演主要角色。随着玻璃光碱度的降低及三维网络结构完整度提高,Eu还原程度增强。同时,在引入的一价网络修饰阳离子与二价网络修饰阳离子的对应氧化物光碱度一致时,二价阳离子的存在更有利于Eu还原反应的进行。
(4)进一步研究了网络阴离子对铝硼硅酸盐玻璃基质中Eu在空气中还原反应的影响。利用高温熔融-淬火方法在空气气氛中制备了Eu_2O_3掺杂氟氧铝硼硅酸盐玻璃,发现在玻璃内部发生了Eu~(3+)→Eu~(2+)的还原反应。该还原反应随着玻璃内F~-/O~(2-)离子含量比例的增大而增强,其原因与不同网络阴离子的电负性不同带来的玻璃基质“电子施主能力”的改变有关,引入玻璃基质的网络阴离子电负性增强,玻璃基质的“电子施主能力”降低,从而有助于Eu还原反应。
(5)研究了稀土离子掺杂氟氧铝硼硅酸盐玻璃及微晶玻璃的制备、结构及性能。在空气气氛下通过高温熔融-淬火/热处理方法制备Eu_2O_3掺杂氟氧铝硼硅酸盐玻璃及微晶玻璃。研究了热处理温度和时间对Eu_2O_3掺杂氟氧铝硼硅酸盐玻璃析晶行为和光学性能的影响。选择合适的热处理温度和时间得到了Ba_2LaF_7微晶相析出的透明氟氧化物微晶玻璃。该微晶化行为对Eu_2O_3掺杂玻璃的发光性能产生一定影响,改变了Eu~(2+)和Eu~(3+)发射峰强度比例。另一方面,研究了Eu_2O_3掺杂浓度对氟氧铝硼硅酸盐微晶玻璃结构及光学性能的影响。随着Eu_2O_3含量增加,La_2O_3含量降低,Ba_2LaF_7析晶倾向减弱,淬火样和热处理样的Eu~(2+)和Eu~(3+)发射峰强度比例变化程度减弱。同时Eu_2O_3掺杂较低时,热处理后的玻璃可观察到Eu~(3+)离子的~5D_1→~7F_2跃迁发射,但在高浓度Eu_2O_3掺杂时,~5D_1→~7F_2跃迁发射消失。
(6)研究了微晶化行为对稀土离子掺杂氟氧铝硼硅酸盐白光发光玻璃的影响。通过高温熔融-淬火/热处理方法在空气气氛中制备了Tm_2O_3和Dy_2O_3共掺氟氧铝硼硅酸盐玻璃及透明微晶玻璃。热处理过程会影响玻璃的发光强度,但不影响白光发射的色度。同时增大Tm-Dy共掺浓度时,Ba_2LaF_7析晶倾向降低。此外,Tm_2O_3和Dy_2O_3共掺浓度淬灭点可由原淬火样的1 mol.%提高到热处理样的2 mol.%,白光发光色度保持不变。
Al_2O_3-B_2O_3-SiO_2 glass was one of important inorganic materials.It possessed good physical and chemical properties,and the raw materlas are cheap.Therefore,it had wide application in chemical engineering,information display,and nuclear waste treatment and so on.This work introduced Al_2O_3-B_2O_3-SiO_2 glass system as the matrix,and focused on two research points.One point was to solve some technical problems of flat alumino-borosilicate glass prepared by micro-float process,which had important energy saving application in fire-resistance,information display and photovoltaics.The other point was to develop a kind of rare earth ions doped luminescence glasses which possessed good thermal stability,could emit white ligh under UV-light excitation and had potaintial application in White-LED area.
First,this thesis reviewd the studies of three aspects as following:(ⅰ) the structure investigations of Al_2O_3-B_2O_3-SiO_2 glasses,(ⅱ) the investigations of flat alumino-borosilicate glasses prepared by micro-float method,and(ⅲ) the investigation progress of white ligh emission glasses.Second,the alumino-borosilcate glasses,rare earth ions doped luminescence aluminoborosilicate glasses and rare earth ions doped luminescence oxyfluoride aluminoborosilicate glass ceramics were prepared by melting-annealing/quenching/thermal treatment method.The micro-structure,optical and thermal properties were mearsured by XRD,TEM,NMR,IR,XPS,DTA,PL and so on.The details were listed as following:
(1) The effects of temperature system on preparation of alumino-borosilcate glasses by melting and annealing method were investigated.The alumino-boroslicate glasses with good melting quality,low coefficient of thermal expansion,high transmission of visible ligh,and low density were prepared.The effects of mixed alkaline earth oxides on crystallization property of alumino-borosilicate glasses were also investigated.The results indicated that the crystallization degree was reduced by introducing mixed alkaline earth oxides to alumino-borosilicate glasses.The tin penetration at bottom surface of float alumino-borosilicate glasses was studied by a lab-scale float apparatus.SEM image showed that a typical tin penetration layer could be detected above 850℃.The tin penetration depth increased with increasing reaction temperature from 850 to 950℃,while it decreased with further increasing reaction temperature from 950℃to 1050℃.
(2) Two serieses samples of Eu-Dy and Tm-Dy ions co-doped aluminoborosilicate glasses were prepared by melting-annealing method with appropriate temperature system.The two serieses samples emited white light under UV light excitation.Meanwhile,the effects of concentration ratio among different rare earth ions,total concentration of rare earth ions and excitation wavelength on chrominance of white ligh emission were investigated in this work. The effects of glass matrix composition on white light huninescence properties of Tm-Dy ions co-doped aluminoborosilicate glasses were studied in the thesis.The results showed that the chroinance of white light emission was not affected by changing glasses matrix composition and the chroinance of white light emission is stable.The transition mechanism between different excitation energy levels in Tm-Dy ions co-doped aluminoborosilicate glasses was also studied.It indicated that an energy transfer progress of Tm~(3+)→Dy~(3+) may exsit between Tm-Dy ions.The probability of the energy transfer progress could be affected by the separation degree of Tm-Dy ions in glass matrix.On the other hand,the chrominance of white ligh emission is stable even though the Tm-Dy co-doped aluminoborosilicate glass had been thermally treated on 530℃for 2～32 h,and the luminescence intensity of the samples did not decrease after thermal treatment.It indicated that the glass possessed good thermal stability.
(3) Eu_2O_3 doped aluminoborosilicate glasses were prepared by melting-annealing method in air.The reduction of Eu~(3+)→Eu~(2+) was observed the samples prepared in air atmosphere. Since Eu~(3+) and Eu~(2+) ions were important actors of red and blue light emission which could synthesize white light,the effects of network modifier cations,network former cantions and thermal treatment on the reduction reaction were systematically investigated in the work. The results showed that the optical basicity of glass matrix and three dimension network structure of glass played important roles in the reduction reaction.The reduction degree was enhanced by the decrease of glass optical basicity and the stabilization of glass three dimension network structures.Meanwhile,when the optical basicity of introduced univalent network modifier cations was equal to that of bivalent network modifier cations,the existence of bivalent network modifier cations was more benefit for the Eu reduction in air.
(4) Futhermore,the effects of network anions on the Eu reduction in aluminoborosilicate glasses prepared in air were investigated in this thesis.Eu_2O_3 doped oxyfluoride aluminoborosilicate glasses were prepared by melting-quenching method in air.The reduction of Eu~(3+)→Eu~(2+) was observed in the samples prepared in air atmosphere.The Eu reduction reaction was enhanced by the increase of concentration ratio between F~-/O~(2-) ions. The effects were related with the changing of "electron donor powers" of glass matrix with different network anions.The "electron donor powers" of glass matrix would decrease with increasing of the electronegetivity of network anions,which resulted in preferable of Eu reduction.
(5) The preparation,structures and properties of rare earth ions doped oxyfluoride aluminoborosilicate glasses and glass ceramics were investigated in this thesis.The Eu_2O_3 doped oxyfluoride aluminoborosilicate glasses and glass ceramics were prepared by melting-quenching and melting-thermal treatment method in air.The effects of thermal treatment temperature and time on the crystallization behavior and optical properties of Eu_2O_3 doped oxyfluoride aluminoborosilicate glasses were investigated.Transparent oxyfluoride aluminoborosilicate glass ceramics with Ba_2LaF_7 micro-crystalline were obtained by thermal treatment under appropriate temperature and time.The crystallization behavior affected the optical properties of Eu_2O_3 doped glasses to some extent.The emission intensity ratio between Eu~(2+) and Eu~(3+) ions was changed with crystallization behavior.Moreover,the effects of Eu_2O_3 concentration on the crystallization behavior and optical properties of oxyfluoride aluminoborosilicate glasses were studied.The Ba_2LaF_7 crystallization degree decreased with the increase of Eu_2O_3 concentration and decrease of La_2O_3 concentration.Meanwhile,the degree of variation of emission intensity ratio between Eu~(2+) and Eu~(3+) ions decreased.The ~5D_1→~7F_2 transition emission was observed in the samples been thermally treated with low Eu_2O_3 concentration,while it could not be observed in the samples with high Eu_2O_3 concentration.
(6) The effects of crystallization behavior on the rare earth ions doped oxyfluoride aluminoborosilicate white light emission glasses were investigated.The Tm_2O_3 and Dy_2O_3 co-doped oxyfluoride aluminoborosilicate glasses and glass ceramics were prepared by melting-quenching and melting-thermal treatment method in air.The thermal treatment process affected the luminescence intensity,but it would not affect the chroinance of white light emission.The Ba_2LaF_7 crystallization degree decreased with the increase of Tm_2O_3 and Dy_2O_3 co-doping concentration and decrease of La_2O_3 concentration.Moreover,the Tm_2O_3 and Dy_2O_3 co-doping concemtration quenching point of quenched samples was about 1 mol.%, and that of thermal treated samles was 2 mol.%.Meanwhile,the chroinance of white light cmission was stable with different Tm_2O_3 and Dy_2O_3 co-doping concentration.
引文
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