稀土掺杂硼酸盐系透明玻璃陶瓷的制备与表征
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摘要
本文阐述了玻璃陶瓷的透光原理及透明玻璃陶瓷的形成条件,从组成、结构和工艺和性能四个方面进行了分析和讨论,综述了玻璃陶瓷的产生与发展过程、合成方法及应用,并对透明玻璃陶瓷的发展前景进行了展望。
采用熔融和晶化技术合成出B2O3-Al2O3-SiO2(BAS)系透明玻璃陶瓷。根据差热分析结果制定玻璃的晶化热处理制度,基于X-ray衍射(XRD)分析结果确定了晶相组成和结构。析晶性能良好的BAS系玻璃在540～71℃C核化,650～810℃晶化,可获得主晶相为2Al2O3·B2O3,次晶相为p-石英固溶体、红柱石和9Al2O3·2SiO2的硼铝硅透明玻璃陶瓷。采用分光光度计测定了BAS系玻璃陶瓷的光透过率,讨论了晶化热处理制度对光透过率的影响。采用扫描电子显微镜(SEM)分析了样品的显微结构,探究了显微结构与光学性能的关系。
采用熔融和晶化技术合成出ZnO-B2O3-Al2O3-SiO2(ZBAS)系透明玻璃陶瓷。根据差热分析结果制定玻璃的晶化热处理制度,基于XRD分析结果确定了晶相组成和结构,讨论了热处理制度对晶相结构的影响,可获得主晶相为立方锌尖晶石ZnAl2O4的锌硼铝硅系透明玻璃陶瓷。采用分光光度计测定ZBAS系玻璃陶瓷的光透过率,讨论了晶化热处理制度对光透过率的影响。采用SEM分析了样品的显微结构,探究了显微结构与光学性能的关系。针对稀土铕,钐,铒的掺杂对其荧光性能进行了测试和分析。
采用熔融和晶化技术合成出Nd3+离子掺杂BaO-B2O3-Al2O3-SiO2(BBAS)系透明玻璃陶瓷。根据差热分析结果制定玻璃的晶化热处理制度,基于XRD分析结果确定了晶相组成和结构,讨论了热处理制度对晶相结构的影响,可分别获得主晶相组成为六方钡长石,次晶相为单斜钡长石的透明玻璃陶瓷。测量了基质玻璃和不同热处理制度下样品的荧光光谱,探讨了晶相组成、结构对钕离子发光性能的影响。钕离子发光光谱与晶相组成和晶粒大小密切相关。中心波长位于890nm.1065nm和1330nm处的三个发光谱带分别对应于钕离子的F3/2→4I9/2、4F3/2→4I11/2和4F3/2→4I13/2跃迁。
对所制备玻璃陶瓷的晶化行为进行了动力学分析,分别确定了BAS,ZBAS,BBAS三种体系的晶化动力学参数。根据玻璃陶瓷的分形特征,利用分形原理进行建立了生长模型,分析了晶化过程中的控制方式,确定了其动力学参数,用分形理论对其扩散控制的晶相生长动力学过程进行了分析。
This text expatiates the optical transparency principles and the forming conditions of glass-ceramics. The factors affected the optical transmittances of glass-ceramics were discussed in the terms of compositions, structure, performance and processes. The origin and development, synthetic methods and applications of glass-ceramics were outlined, and the developing trend was forecasted as well.
B2O3-Al2O3-SiO2(BAS) system transparent glass-ceramics were synthesized by the melting method and crystallization technique. The crystallization heat-treated schedules were based on DSCA results. The compositions and structure of crystal phases were determined on the base of XRD results. The transparent BAS glass s-ceramics with main crystal phase-2Al2O3·B2O3and minor crystal phase-(3-SiO2solid solutions, Al2O3·B2O3and9Al2O3·2SiO2were obtained, It was shown that the little change to the compositions influenced the crystal phases unmarkedly. The short-range structure of the transparent glass-ceramics was researched by XPS. The optical transmittances of the BAS glass-ceramics were measured by spectrophotometer. The influences of crystallization heat-treated schedules to the optical transmittance were discussed. The microstructure of the transparent BAS glass-ceramics was characterized by SEM, and the microstructure parameters were obtained by means of automatic image analysis technique.
The microstructure was studied by stereology principles and method, and the relationship between the microstructure and the optical properties was explored. Transparent ZnO-B2O3-Al2O3-SiO2(ZBAS) system glass-ceramics were synthesized by the melting method and annealing technique. The crystallization heat-treated schedules were based on DSC results. The compositions and structure of crystal phases were determined on the base of XRD results. The transparent ZBAS glass-ceramics with main crystal phase-cubic gahnite ZnAl2O4at the same time, gahnite became to the minor crystal phase. The influences of crystallization heat-treated schedules to the optical transmittance were discussed. The microstructure of the transparent ZBAS system glass-ceramics was characterized by SEM, and the microstructure parameters were obtained by means of automatic image analysis technique. The microstructure was studied by stereology principles and method, and the relationship between the microstructure and the optical properties was explored. The optical transmittance decreased with the increasing of the three dimensional sphere diameters and the mean specific area of grains per volume. The optical transmittance increased with the enhancing of the mean three-dimensional free distance of grain boundaries and the mean specific area of single grain.
BaO-B2O3-O2-Al2O3-SiO2system transparent glass-ceramics were synthesized by the melting method and annealing technique. The crystallization heat-treated schedules were based on DSC results. The compositions and structure of crystal phases were determined on the base of XRD results. The transparent glass-ceramics doped Nd3+with main crystal phase.Three main fluorescence bands centering at about890nm,1065nm and1330nm were observed, which were correspondent to the transitions of4F3/2→4I9/2,4F3/2→4I11/2and4F3/2→4I13/2, respectively. The fluorescent intensity increased markedly.which grain size was approaching to the wavelength of the visual light. Quenching disappeared after the precipitation of the B-spodumene.
The precipitation of crystal phases from glass phase includes the nucleus forming and crystal growing dynamic processes. The mechanism of the crystal phase precipitation and growth in transparent glass-ceramics system was studied, and it was submitted to the function. The kinetics of crystal phase growth controlled by the diffusion in fractal structure was analyzed by fractal spectrum dimension. It was presented that the difference between the fractal kinetics and traditional kinetics, and the relationship between the reaction kinetics and fractal structure as well. The fractal spectrum dimension ds is1.2688calculated by fitting curve of experimental data.
采用熔融和晶化技术合成出B2O3-Al2O3-SiO2(BAS)系透明玻璃陶瓷。根据差热分析结果制定玻璃的晶化热处理制度,基于X-ray衍射(XRD)分析结果确定了晶相组成和结构。析晶性能良好的BAS系玻璃在540～71℃C核化,650～810℃晶化,可获得主晶相为2Al2O3·B2O3,次晶相为p-石英固溶体、红柱石和9Al2O3·2SiO2的硼铝硅透明玻璃陶瓷。采用分光光度计测定了BAS系玻璃陶瓷的光透过率,讨论了晶化热处理制度对光透过率的影响。采用扫描电子显微镜(SEM)分析了样品的显微结构,探究了显微结构与光学性能的关系。
采用熔融和晶化技术合成出ZnO-B2O3-Al2O3-SiO2(ZBAS)系透明玻璃陶瓷。根据差热分析结果制定玻璃的晶化热处理制度,基于XRD分析结果确定了晶相组成和结构,讨论了热处理制度对晶相结构的影响,可获得主晶相为立方锌尖晶石ZnAl2O4的锌硼铝硅系透明玻璃陶瓷。采用分光光度计测定ZBAS系玻璃陶瓷的光透过率,讨论了晶化热处理制度对光透过率的影响。采用SEM分析了样品的显微结构,探究了显微结构与光学性能的关系。针对稀土铕,钐,铒的掺杂对其荧光性能进行了测试和分析。
采用熔融和晶化技术合成出Nd3+离子掺杂BaO-B2O3-Al2O3-SiO2(BBAS)系透明玻璃陶瓷。根据差热分析结果制定玻璃的晶化热处理制度,基于XRD分析结果确定了晶相组成和结构,讨论了热处理制度对晶相结构的影响,可分别获得主晶相组成为六方钡长石,次晶相为单斜钡长石的透明玻璃陶瓷。测量了基质玻璃和不同热处理制度下样品的荧光光谱,探讨了晶相组成、结构对钕离子发光性能的影响。钕离子发光光谱与晶相组成和晶粒大小密切相关。中心波长位于890nm.1065nm和1330nm处的三个发光谱带分别对应于钕离子的F3/2→4I9/2、4F3/2→4I11/2和4F3/2→4I13/2跃迁。
对所制备玻璃陶瓷的晶化行为进行了动力学分析,分别确定了BAS,ZBAS,BBAS三种体系的晶化动力学参数。根据玻璃陶瓷的分形特征,利用分形原理进行建立了生长模型,分析了晶化过程中的控制方式,确定了其动力学参数,用分形理论对其扩散控制的晶相生长动力学过程进行了分析。
This text expatiates the optical transparency principles and the forming conditions of glass-ceramics. The factors affected the optical transmittances of glass-ceramics were discussed in the terms of compositions, structure, performance and processes. The origin and development, synthetic methods and applications of glass-ceramics were outlined, and the developing trend was forecasted as well.
B2O3-Al2O3-SiO2(BAS) system transparent glass-ceramics were synthesized by the melting method and crystallization technique. The crystallization heat-treated schedules were based on DSCA results. The compositions and structure of crystal phases were determined on the base of XRD results. The transparent BAS glass s-ceramics with main crystal phase-2Al2O3·B2O3and minor crystal phase-(3-SiO2solid solutions, Al2O3·B2O3and9Al2O3·2SiO2were obtained, It was shown that the little change to the compositions influenced the crystal phases unmarkedly. The short-range structure of the transparent glass-ceramics was researched by XPS. The optical transmittances of the BAS glass-ceramics were measured by spectrophotometer. The influences of crystallization heat-treated schedules to the optical transmittance were discussed. The microstructure of the transparent BAS glass-ceramics was characterized by SEM, and the microstructure parameters were obtained by means of automatic image analysis technique.
The microstructure was studied by stereology principles and method, and the relationship between the microstructure and the optical properties was explored. Transparent ZnO-B2O3-Al2O3-SiO2(ZBAS) system glass-ceramics were synthesized by the melting method and annealing technique. The crystallization heat-treated schedules were based on DSC results. The compositions and structure of crystal phases were determined on the base of XRD results. The transparent ZBAS glass-ceramics with main crystal phase-cubic gahnite ZnAl2O4at the same time, gahnite became to the minor crystal phase. The influences of crystallization heat-treated schedules to the optical transmittance were discussed. The microstructure of the transparent ZBAS system glass-ceramics was characterized by SEM, and the microstructure parameters were obtained by means of automatic image analysis technique. The microstructure was studied by stereology principles and method, and the relationship between the microstructure and the optical properties was explored. The optical transmittance decreased with the increasing of the three dimensional sphere diameters and the mean specific area of grains per volume. The optical transmittance increased with the enhancing of the mean three-dimensional free distance of grain boundaries and the mean specific area of single grain.
BaO-B2O3-O2-Al2O3-SiO2system transparent glass-ceramics were synthesized by the melting method and annealing technique. The crystallization heat-treated schedules were based on DSC results. The compositions and structure of crystal phases were determined on the base of XRD results. The transparent glass-ceramics doped Nd3+with main crystal phase.Three main fluorescence bands centering at about890nm,1065nm and1330nm were observed, which were correspondent to the transitions of4F3/2→4I9/2,4F3/2→4I11/2and4F3/2→4I13/2, respectively. The fluorescent intensity increased markedly.which grain size was approaching to the wavelength of the visual light. Quenching disappeared after the precipitation of the B-spodumene.
The precipitation of crystal phases from glass phase includes the nucleus forming and crystal growing dynamic processes. The mechanism of the crystal phase precipitation and growth in transparent glass-ceramics system was studied, and it was submitted to the function. The kinetics of crystal phase growth controlled by the diffusion in fractal structure was analyzed by fractal spectrum dimension. It was presented that the difference between the fractal kinetics and traditional kinetics, and the relationship between the reaction kinetics and fractal structure as well. The fractal spectrum dimension ds is1.2688calculated by fitting curve of experimental data.
引文
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