Novel special optical fibers nowadays can take advantage of several new preform production techniques. During the last years we have devoted our attention to the granulated silica method. It is one of the variants of the powder-in-tube technique and potentially offers a high degree of freedom regarding the usable dopants, the maximum possible dopant concentration, the homogeneity of the dopants, the geometry and minimal refractive index contrast. We developed and refined an approach for the production of doped granulated silica material based on the sol-gel process. Here, we present material analysis results of an ytterbium (Yb) doped, aluminum (Al) and phosphorous (P) co-doped glass on the basis of our sol-gel glass based granulated silica method as well as first measurements of two LMA fibers obtained from this material. For the material analysis we used advanced analysis techniques, such as HAADF-STEM and STEM-EDX spectroscopy to determine the composition of the material and the distribution of the dopants and the codopants. The chemical mapping of the STEM-EDX shows an extremely homogeneous distribution of the dopants and co-dopants in nano-scale. Based on self-made LMA fibers, we measured the refractive index contrast of the sol-gelbased granulated silica derived core compared to the pure silica cladding. In addition we quantified optical characteristics such as the emission and absorption spectrum. The measured upper state lifetime of the optical active dopant ytterbium was 0.99ms, which in turn confirms the homogeneous distribution of the Yb atoms. The propagation losses were determined to be 0.2dB/m at 633nm and 0.02414dB/m at1550nm.
Fabrication of Ytterbium-doped active fibers with different designs, compositions and high Yb concentration has attracted an intense interest. For making highly Yb-doped fibers, co-dopants like phosphorous (P) and aluminum (Al) are also employed in order to modify refractive index and increase Yb solubility, avoiding clusters and phase segregations. Indeed, Yb-clustering results in quenching effects and increased propagation losses due to energy transfer between clustered ions. Therefore, the chemical composition and phase homogeneity of the fiber core have key influences on the performance of an active fiber. However, conventional fabrication techniques such as MCVD (modified chemical vapor deposition) and OVD (outside vapor deposition) are approaching the limit. In this contribution, we have developed an approach for fabrication of such active fibres based on granulated silica derived from the sol-gel process. The advantage of this method is the fabrication of active fibers with high dopant contents and homogeneity. Here, using high angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) in atomic scale, we report the direct, nano-scale and atomic-resolution observation of individual Yb dopant and co-dopant (i.e. Al, P) atoms for different fabricated fibers. The chemical mapping from STEM-EDX shows an extremely homogeneous distribution of the dopants and co-dopants in nano-scale for our fabrication protocol. However in atomic resolution, we also identified the possible Yb clusters in the range of 10 atoms within the core structure. The size, structure, and distribution of these clusters are determined with an Yb-atom detection efficiency of almost 100% by STEM.
The production of special fibers relies on new methods and materials to incorporate new functionalities into optical fibers by virtues of dopants and structure. In particular, the granulated silica method allows to rapidly produce active fibers with high dopant content and with virtually any microstructure. The implementation of this production method requires a multitude of process steps at various temperatures and temperature gradients that can significantly influence the optical properties of the produced preforms and fibers. To better understand and optimize the processes of active material production and fiber drawing parameters we have done a thorough analysis of microstructure, phase development, crystallinity and chemical mapping of active fiber cores produced by a combination of sol-gel process and granulated silica method with and without employment of a CO2 laser treatment. The microstructure of fibers have been analyzed with a diverse suite of techniques in Transmission Electron Microscopy (TEM), revealing formation of various silica polymorphs and distribution of active elements (i.e. Yb and P) into the core structure. Our results show the presence of another polymorph of silica with low crystallinity dispersed in the main amorphous polymorph (i.e. quartz). We conclude that in spite of importance of homogeneous distribution of Yb and P into the core, the formation of various silica polymorphs resulting from materials processing has to be considered.