The mechanisms of optical losses in bismuth-doped silica glass (Bi:SiO(2)) and fibers were studied. It was found that in the fibers of this composition the up-conversion processes occur even at bismuth concentrations lower than 0.02 at.%. Bi:SiO(2) core holey fiber drawn under oxidizing conditions was investigated. The absorption spectrum of this fiber has no bands of the bismuth infrared active center. Annealing of this fiber under reducing conditions leads to the formation of the IR absorption bands of the bismuth active center (BAC) and to the simultaneous growth of background losses. Under the realized annealing conditions (argon atmosphere, T(max) = 1100°C, duration 30 min) the BAC concentration reaches its maximum and begins to decrease in the process of excessive Bi reduction, while the background losses only increase. It was shown that the cause of these background losses is the absorption of light by nanoparticles of metallic bismuth formed in bismuth-doped glasses as a result of reduction of a part of the bismuth ions to Bi(0) and their following aggregation. The growth of background losses occurs owing to the increase of the concentration and the size of the metallic bismuth nanoparticles.

A spectroscopic protocol is proposed to implement confocal microfluorescence imaging to the analysis of microinhomogeneity in the nanocrystallization of the core of fibers belonging to a new kind of broadband fiber amplifier based on glass with embedded nanocrystals. Nanocrystallization, crucial for achieving an adequate light emission efficiency of transition metal ions in these materials, has to be as homogeneous as possible in the fiber to assure optical amplification. This requirement calls for a sensitive method for monitoring nanostructuring in oxide glasses. Here we show that mapping microfluorescence excited at 633 nm by a He-Ne laser may give a useful tool in this regard, thanks to quasi-resonant excitation of coordination defects typical of germanosilicate materials, such as nonbridging oxygens and charged Ge-O-Ge sites, whose fluorescence are shown to undergo spectral modifications when nanocrystals form into the glass. The method has been positively checked on prototypes of optical fibers-preventively characterized by means of scanning electron microscopy and energy dispersive spectroscopy-fabricated from preforms of Ni-doped Li 2 O-Na 2 OSb 2 O 3 -Ga 2 O 3 -GeO 2 -SiO 2 glass in silica cladding and subjected to heat treatment to activate gallium oxide nanocrystal growth. The method indeed enables not only the mapping of the crystallization degree but also the identification of drawing-induced defects in the fiber cladding.

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