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Rare-earth (RE) doped transparent glass-ceramics are presented as very promising materials for optical applications. In this work, Transmission Electron Microscopy techniques have been used to structurally characterize a glass of composition 55SiO2-20Al2O3-15Na 2O-10LaF3 (mol%), doped with 1 mol% Tm2O 3, and the corresponding glass-ceramic. The proposed crystallization mechanism for this glass has been modified from the results obtained through advanced STEM/EDXS techniques. The parent glass contains phase separated regions mainly enriched in F and La and also in Al, Si and Tm. After annealing, 10-20 nm LaF3 nano-crystals are formed from these phase separated droplets. The partial incorporation of the doping Tm3+ ions into the LaF 3 nano-crystals has been verified and the interphase crystal/glassy matrix has been more precisely characterized through EDXS. An Al enriched layer is formed around the crystals followed by a Si enriched shell, which greatly increase the viscosity in the periphery of the crystals, inhibiting further crystal growth and thus, keeping the nano size of the crystals. © 2013 The Royal Society of Chemistry. ; The authors acknowledge the financial support of the project MAT2010-20459 of Spanish Government and the FhG Internal Programs under Grant No. Attract 692 280. ; Peer Reviewed

Trabajo presentado al SPIE Photonic West: Optical Components and Materials XV, celebrado en San Francisco, California (USA) del 29 al 31 de enero de 2018. ; Transparent oxyfluoride glass-ceramics obtained by the adequate heat treatment of Nd3+-doped glass with composition SiO2-Al2O3-Na2O-LaF3 are investigated. X-ray diffraction (XRD) and high resolution transmission electron microscopy (HR-TEM) show that the precipitated nanocrystals are LaF3 with a crystal size between 9-12 nm. Furthermore, energy dispersive X-ray (EDX) analysis shows the incorporation of Nd3+ ions into the LaF3 nanocrystals. Site-selective and time-resolved emission and excitation spectra of the 4F3/2 and 4F5/2 states, allows to unambiguously isolate the emission of Nd3+ ions in LaF3 nanocrystals which shows well defined spectra, similar to those obtained for pure LaF3 crystal. ; This work was supported by the Spanish Government MEC under Projects No. MAT2013-48246-C2-1-P, MAT2013-48246-C2-2-P, and MAT2017-87035-C2-2-P and the University of the Basque Country PPG17/07. ; Peer Reviewed

This article belongs to the Special Issue Preparation and Application of Nanostructured Glass–Ceramics and Nanocomposites. ; Transparent oxyfluoride glass–ceramics containing NaGdF4 nanocrystals were prepared by melt-quenching and doped with Er3+ (0.5 mol%) and different amounts of Yb3+ (0–2 mol%). The selected dopant concentration the crystallization thermal treatments were chosen to obtain the most efficient visible up-conversion emissions, together with near infrared emissions. The crystal size increased with dopant content and treatment time. NaGdF4 NCs with a size ranging 9–30 nm were obtained after heat treatments at Tg + 20–80 °C as confirmed by X-ray diffraction and high-resolution transmission electron microscopy. Energy dispersive X-ray analysis shows the incorporation of rare earth ions into the NaGdF4 nanocrystals. Near-infrared emission spectra, together with the up-conversion emissions were measured. The optical characterization of the glass–ceramics clearly shows that Er3+ and Yb3+ ions are incorporated in the crystalline phase. Moreover, visible up-conversion emissions could be tuned by controlling the nanocrystals size through appropriated heat treatment, making possible a correlation between structural and optical properties. ; This research was funded by Spanish National projects MAT2017-87035-C2-1-P/2-P (AEI/FEDER, UE), Basque Country University PPG17/07 and GIU17/014 and Basque Government PIBA2018-24. This study is part of the dissemination activities of project FunGlass. This project has received funding from the European Union's Horizon 2020 research and innovation program under grant agreement No 739566. This study was also created in the frame of the project Centre for Functional and Surface Functionalized Glass (CEGLASS), ITMS code is 313011R453, operational program Research and innovation, co-funded from European Regional Development Fund. ; Peer reviewed

Transparent NaLuF4 glass-ceramics (GCs) doped with Tm3+ and Tm3+/Yb3+ have been prepared by melting-quenching followed by thermal treatment at temperatures near the glass transition temperature. The crystallization process has been studied using X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). NaLuF4 nanocrystals (NCs) ranging 9–30 nm in size are the only crystalline phase, the crystal size increasing with the dopant concentration. Energy dispersive X-ray (EDX) measurements confirm the Tm3+ and Yb3+ incorporation in the NCs. Optical characterization included the analysis of up-conversion (UC) as well as the Near-infrared (NIR) luminescence. NIR emission spectra of Tm3+ and Yb3+ in co-doped samples confirmed an efficient energy transfer between both ions. No UC emissions are observed in Tm3+ single-doped glass and GCs. Yb3+ incorporation favors the Tm3+-Tm3+ UC processes resulting in Tm3+ blue, yellowish-red and NIR UC emissions after excitation at 975 nm. Blue UC emission is also observed in the codoped samples after Tm3+ excitation at 791 nm. These effects were more evident for the GCs compared to the base glasses, confirming the RE ions incorporation in the NCs. As a result, these GCs can be used to tune the UC emission from NIR to blue by selective excitation. ; This work was supported by MINECO under Projects MAT2017-87035-C2-1-P/-2-P (AEI/FEDER, UE), Basque Country Government PIBA2018-24 and Basque Country University GIU17/014. This article is part of the dissemination activities of project FunGlass. This project has received funding from the European Union´s Horizon 2020 research and innovation programme under grant agreement No 739566. This article was also created in the frame of the project Centre for Functional and Surface Functionalized Glass (CEGLASS), ITMS code is 313011R453, operational program Research and innovation, co-funded from European Regional Development Fund. This research work has been supported by the Research Agency of the Ministry of Education, Science, Research and Sport of the Slovak Republic, by the project: Advancement and support of R&D for "Centre for diagnostics and quality testing of materials" in the domains of the RIS3 SK specialization, Acronym: CEDITEK II., ITMS2014+ code 313011W442. ; Peer reviewed

[EN] Novel glass-ceramic optical fibers containing NaLuF nanocrystals doped with 0.5ErF and 2YbF (mol%) have been prepared by the rod-in-tube method and controlled crystallization. NaLuF nanocrystals with a size around 20 nm are obtained after heat treatment at 600 °C. Intense upconverted green and red emissions due to (H, S) → I and F → I transitions, respectively, together with a blue emission due to H → I transition have been observed under excitation at 980 nm. The intensity of the green and red upconversion bands shows a nearly linear dependence on the excitation power which can be explained by saturation effects in the intermediate energy states and proves that a sensitized energy transfer upconversion process is responsible for the population of the emitting levels of Er ions. The upconversion emission color changes from yellow to green by increasing the excitation power density which allows to manipulate the color output of the Er emission in the glass-ceramic fibers. The tunable emission color is easily detected with the naked eye. This interesting characteristic makes these glass-ceramic fibers promising materials for photonic applications. ; This work was supported by MINECO under the project MAT2017-87035-C2-1-P/-2-P (AEI/FEDER, UE) and Basque Country University PPG17/07 and GIU17/014, and Basque Government PIBA2018-24. Funding from MPNS Cost Action MP1401 is also acknowledged. This paper is a part of dissemination activities of project FunGlass. This project has received funding from the European Union's Horizon 2020 research and innovation programme under grant agreement no. 739566.