| 题名 | 掺镱氟磷酸锶(Yb3+5(PO4)3F)粉体的制备及机理研究 |
| 作者 | 柴宝燕 |
| 学位类别 | 硕士 |
| 答辩日期 | 2016 |
| 授予单位 | 中国科学院上海光学精密机械研究所 |
| 导师 | 张龙 |
| 关键词 | Yb3+5(PO4)3F 共沉淀法 固相法 发射光谱 固态核磁共振 |
| 其他题名 | Preparation and mechanism research of Yb3+ doped strontium fluoroapatite (Yb3+5(PO4)3F) particles |
| 中文摘要 | 掺镱氟磷酸锶(Yb3+:Sr5(PO4)3F，Yb:S-FAP)晶体具有卓越的光谱性能和激光性能，是未来重频高效强激光系统的最佳增益介质之一。然而，生长大口径Yb:S-FAP 晶体迄今仍然是激光材料领域一大技术挑战。相对于单晶而言，透明激光陶瓷因为制备周期短、生产成本低，容易实现大尺寸、高掺杂浓度、高光学均匀性样品的制备，是近年来材料领域的一个研究热点。 基于此，本论文开展有序多晶各向异性Yb:S-FAP透明陶瓷的相关研究工作，研究了共沉淀法和固相法制备Yb3+:Sr5(PO4)3F陶瓷粉体的各种影响因素，以及Yb3+掺杂对粉体微观形貌、光谱性能的影响。 本论文系统地研究了Yb3+:Sr5(PO4)3F陶瓷粉体的制备以及光谱性能，取得了一些创新性成果，主要包括以下几个方面的内容： 1、共沉淀法法制备Yb3+:Sr5(PO4)3F陶瓷粉体的研究 采用共沉淀法制备了纯相Sr5(PO4)3F粉体以及不同掺杂浓度的Yb3+:Sr5(PO4)3F粉体，系统研究了粉体制备过程中的各种主要影响因素。包括沉淀温度和阴离子溶液的pH值等。针对不同条件下合成的粉体物相以及形貌，结合经典成核理论和第一性原理计算结果，解释Sr5(PO4)3F粉体各种形貌的产生机理。最终获得形貌、尺寸可控的Sr5(PO4)3F粉体。结合不同煅烧温度、煅烧时间以及NMR测试分析研究液相法制备Sr5(PO4)3F粉体中Yb3+掺杂浓度极限和Yb3+离子在Sr5(PO4)3F晶格中占据的格位问题。结合光谱性能研究Yb3+掺杂量的变化对Yb3+:Sr5(PO4)3F光谱性能的影响。 2、固相法制备Yb3+:Sr5(PO4)3F陶瓷粉体的研究 采用固相法制备了纯相Sr5(PO4)3F粉体以及不同掺杂浓度的Yb3+:Sr5(PO4)3F粉体，系统研究了粉体制备过程中各种主要影响因素。包括原料配比、煅烧时间。结合XRD测试结果和NMR测试结果研究固相法制备Sr5(PO4)3F粉体中Yb3+掺杂浓度极限。结合光谱性能研究Yb3+掺杂量的变化对Yb3+:Sr5(PO4)3F光谱性能的影响。 3、液相法、固相法合成Yb3+:Sr5(PO4)3F粉体性能对比研究 采用光谱性能和NMR等测试对比分析，研究不同制备方法对Yb3+:Sr5(PO4)3F粉体的发光性能以及Yb3+离子在Sr5(PO4)3F中占据的格位问题。 |
| 英文摘要 | Yb3+ doped strontium fluoroapatite (Yb3+:Sr5(PO4)3F，Yb:S-FAP) crystal has excellent spectroscopic properties and laser performance, becoming one of the best performance gain medium for high power laser systems with practical repetition rate. However, it is still a technical challenge for growing high quality Yb3+:S-FAP crystals with diameter up to 7 cm because of its anisotropic thermo-mechanical properties. Compared to single crystal, transparent laser ceramic has a short production cycle and low production cost, and it is easy to get ceramic with large size, high doping concentration and good optical homogeneity, making it to be a research hotspot in the field of laser ceramic. Based on the background, we carried out a series of work for the preparation of oriented polycrystalline Yb:S-FAP laser ceramic. The keystone of our research is about the preparation of Yb3+:Sr5(PO4)3F powders using precipitation method and solid state reaction method, and the influence of Yb3+ doping concentration to the micro morphology and spectral property. In this paper, preparation and spectral properties of Yb3+:Sr5(PO4)3F powders are studied systematically, making some innovative achievements. Results obtained are described as follows: Part one: Co-precipitation of Yb3+:Sr5(PO4)3F powders We took co-precipitation method to prepare pure-phase Sr5(PO4)3F powders and Yb3+:Sr5(PO4)3F powders with different dopant concentration Yb3+. The main factors in the preparation process, including precipitation temperature and anionic solution pH value, were studied systematic. According to the phenomenon that powders synthesized under different conditions has various phase and morphology, combined with classical nucleation theory and first principles calculations, made a reasonable explanation for the various morphology of Sr5(PO4)3F powders. Ultimately, we got the conditions to fabricate Sr5(PO4)3F powders with controllable morphology and size. By combining different calcining temperature, calcining time and NMR results we gave research on the limit of Yb3+ doping concentration in Sr5(PO4)3F powders. The influence of the amout of Yb3+ doping concentration on the spectral performance were also studied. Part two: Solid-state reaction of Yb3+:Sr5(PO4)3F powders We took solid-state reaction method to prepare pure-phase Sr5(PO4)3F powders and Yb3+:Sr5(PO4)3F powders with different Yb3+ doping concentration. The main factors in the preparation process, including the ratio of raw material and calcination time were studied. Research on the limit of Yb3+ doping concentration in Sr5(PO4)3F powders were taken based on the XRD and NMR results. The influence of Yb3+ doping concentration on the spectral performance were also studied. Part three: Contrast research on the Yb3+:Sr5(PO4)3F powders synthesized by co-precipitation and solid-state reaction By the comparative study on the spectral performance and NMR results of Yb3+:Sr5(PO4)3F powders systhesized using different method, analysis the influence of preparation methods on the luminescent properties and the problem about site occupied of Yb3+ in Sr5(PO4)3F lattice. |
| 语种 | 中文 |
| 内容类型 | 学位论文 |
| 源URL | [http://ir.siom.ac.cn/handle/181231/17006]  |
| 专题 | 上海光学精密机械研究所_学位论文 |
| 推荐引用方式 GB/T 7714 | 柴宝燕. 掺镱氟磷酸锶(Yb3+5(PO4)3F)粉体的制备及机理研究[D]. 中国科学院上海光学精密机械研究所. 2016. |
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