Transmission electron microscopy of proton‐exchanged LiNbO 3 waveguide channels reveals regions of diffuse intensity within the single‐crystal electron diffraction patterns of LiNbO 3 . The diffuse intensity was not observed from areas of LiNbO 3 which had been masked with Cr before exchange. Heating the waveguides in air at 550 °C for 2 h sharpened some of the diffuse intensity into diffraction spots, some of whose lattice spacings matched Nb 2 O 5 or LiNb 3 O 8 . Other reflections also appeared which matched these phases. Small (∼20 nm diam) cavities were also observed in the exchanged channels after heating and suggest the occurrence of a dehydration reaction.
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