Pellegrino Anna Lucia, Milan Emil, Speghini Adolfo, Malandrino Graziella
Dipartimento di Scienze Chimiche, Università di Catania and INSTM UdR Catania, Viale A. Doria 6, I-95125 Catania, Italy.
Nanomaterials Research Group, Dipartimento di Biotecnologie, Università di Verona and INSTM UdR Verona, Strada le Grazie 15, I-37134 Verona, Italy.
Materials (Basel). 2023 Oct 27;16(21):6889. doi: 10.3390/ma16216889.
In the present work, an in-depth study on the sol-gel process for the fabrication of Eu-doped CaF materials in the form of thin films has been addressed for the production of down-shifting layers. Fine-tuning of the operative parameters, such as the annealing temperature, substrate nature and doping ion percentage, has been finalized in order to obtain Eu(III)-doped CaF thin films via a reproducible and selective solution process for down-shifting applications. An accurate balance of such parameters allows for obtaining films with high uniformity in terms of both their structural and compositional features. The starting point of the synthesis is the use of a mixture of Ca(hfa)•diglyme•HO and Eu(hfa)•diglyme adducts, with a suited ratio to produce 5%, 10% and 15% Eu-doped CaF films, in a water/ethanol solution. A full investigation of the structural, morphological and compositional features of the films, inspected using X-ray diffraction analysis (XRD), field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray analysis (EDX), respectively, has stated a correlation between the annealing temperature and the structural characteristics and morphology of the CaF thin films. Interestingly, crystalline CaF films are obtained at quite low temperatures of 350-400 °C. The down-shifting properties, validated by taking luminescence measurements under UV excitation, have allowed us to correlate the local environment in terms of the degree of symmetry around the europium ions with the relative doping ion percentages.
在本工作中,针对制备下转换层,对以薄膜形式制备铕掺杂CaF材料的溶胶 - 凝胶工艺进行了深入研究。为了通过可重复且选择性的溶液工艺获得用于下转换应用的铕(III)掺杂CaF薄膜,已完成对诸如退火温度、衬底性质和掺杂离子百分比等操作参数的微调。这些参数的精确平衡使得能够获得在结构和组成特征方面具有高均匀性的薄膜。合成的起始点是在水/乙醇溶液中使用Ca(hfa)•二甘醇二甲醚•H₂O和Eu(hfa)•二甘醇二甲醚加合物的混合物,以合适的比例制备5%、10%和15%铕掺杂的CaF薄膜。分别使用X射线衍射分析(XRD)、场发射扫描电子显微镜(FE - SEM)和能量色散X射线分析(EDX)对薄膜的结构、形态和组成特征进行了全面研究,结果表明退火温度与CaF薄膜的结构特征和形态之间存在相关性。有趣的是,在相当低的350 - 400°C温度下可获得结晶CaF薄膜。通过在紫外激发下进行发光测量验证的下转换特性,使我们能够将铕离子周围对称程度方面的局部环境与相对掺杂离子百分比相关联。