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Fiber Bragg gratings are key components for optical fiber sensing applications in harsh environments. This paper investigates the structural and chemical characteristics of femtosecond laser photo-inscribed microvoids. These voids are at the base of type III fs-gratings consisting of a periodic array of microvoids inscribed at the core of an optical fiber. Using high-resolution techniques such as quantitative phase microscopy, electron transmission microscopy, and scattering-type scanning near-field IR optical microscopy, we examined the structure of the microvoids and the densified shells around them. We also investigated the high-temperature behavior of the voids, revealing their evolution in size and shape under step isochronal annealing conditions up to 1250 °C.