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This paper describes the first synthesis of YbPO 4 nano-cylinders and nanoparticles within optical fiber preforms. To obtain YbPO 4 -doped silica monoliths, phosphosilicate powders, previously prepared by a sol–gel method, were impregnated with a solution containing an ytterbium salt. Then, they were compressed into cylinders and sintered at high temperature. These doped monoliths were densified under controlled atmosphere and then drawn at high temperature into 1.6 mm diameter-rods. The composition, structural and optical properties of these monoliths and rods were investigated using Electron Probe Micro-Analysis, Transmission Electron Microscopy (TEM), Raman spectroscopy and IR absorption measurements. The size of the YbPO 4 nanoparticles within the monoliths were found to be in the range of 8–15 nm and 13–25 nm, depending on the Yb-doping amount. Upon drawing the most concentrated Yb-doped monoliths into rods, the nanoparticles evolve to form nano-cylinders with a mean diameter around 40 nm and a length of about 400 nm. Similar behavior was observed for the less concentrated Yb-doped monoliths, once drawn into rods but a lower number of nano-cylinders were found in this case. Structural analysis, based on Raman spectroscopy and TEM experiments, shows that all these nano-objects have a tetragonal xenotime structure (I4 1 /amd ). Moreover, it was found that the nano-cylinders were all aligned parallel to the drawing direction. These SiO 2 -P 2 O 5 :YbPO 4 glass ceramics exhibit a structured absorption spectra around 980 nm, which corroborates the Yb 3+ crystalline environment.

International audience; Bismuth-doped glasses are attractive materials for the development of new optical amplifiers and tunable laser sources. In this paper, Bi-dopedphosphosilicate glasses are prepared using the sol-doping technique in combination with shaping using cold isostatic pressing. After a first drawingat high temperature (2000 C), the obtained glass cane presents a wide near infrared (NIR) photoluminescence band under visible excitation. The authors show that this NIR optical activity, connected to phosphorus center, is preserved after a second drawing into a conventional optical fiber. These results confirm the potentialities of this synthesis approach for the fabrication of Bi-activated optical fibers.