An in-depth characterization of nanoparticle-doped optical fibers is crucial to understand the potential new functionalities of the engineered glass and thus their applicability fields. The high temperatures of the manufacturing process strongly affect the nanoparticle features, and therefore, their analysis is necessary after fiber drawing. However, the difficulties associated with the use of atomic resolution microscopies to analyze the nanoparticle features in the fiber core, mainly related to sample preparation and expensive costs, usually prevent their study. In this work, we overcome some of those limitations and demonstrate, for the first time, the suitability of structurally and microstructurally studying in detail nanocrystals contained in a fiber core of ∼10 μm by combining confocal Raman microscopy, Rayleigh light-scattering microscopy, and scanning electron microscopy (SEM). A thorough study of cubic-shaped and rod-shaped YPO4 nanocrystals contained in optical fibers reveals their crystallization in tetragonal (t) and monoclinic (m) structures, respectively. The symmetric (ν1) and asymmetric stretching (ν3) Raman modes display a different and remarkable red shift as particle size decreases in both types of nanocrystals, which in the case of the cubic-shaped nanocrystals is fitted to an exponential function along with a Raman peak broadening. Moreover, their Raman dependence vs temperature is evaluated up to 600 °C, observing a phonon softening that follows a linear behavior, which is discussed in detail. These findings add new insights to pure m-YPO4, which was unknown to date, and the REPO4 family and open up new avenues that can be extrapolated to other nanostructures incorporated into optical fiber cores, which will advance progress in the field of nanoparticle-doped optical fibers.
Keywords: REPO4 nanocrystal; Rayleigh light-scattering microscopy; YPO4 nanocrystal-doped optical fiber; confocal Raman microscopy; monoclinic YPO4; tetragonal YPO4.