Abstract. ZrO2 waveguides are prepared by the sol-gel process from a solution containing zirconium n-propoxide and acetylacetone in propanol-2. Structural characterizations are investigated for different annealing temperatures using suitable techniques including Waveguide Raman Spectroscopy, Electron Microscopy and Atomic Force Microscopy. Films are amorphous at 300~ and the pure ZrO2 tetragonal crystalline phase appears beyond 400~ Crystallized films present a dense, uniform and polycrystalline structure made up by randomly oriented nanocrystallites, the diameter of which increases from 38/~ at 400~ to 53/~ at 600~ Waveguides are at least monomode TE0 at 632.8 nm. At this wavelength, optical losses are about 0.8 4-0.2 dB/cm for amorphous layers and increase up to 2.5 4-0.4 dB/cm for 600~ heat-treated waveguides.

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