The effects of heat treatments in a vacuum chamber for a (001) single
crystal of LiNbO3 have been examined with XPS, TPD and CAICISS. The si
ngle crystal of an as-received LiNbO3 lost lithium from its surface, a
nd the lower valence niobium ion (Nb4+) was observed in the XPS spectr
um for the Nb 3d level. The atomic ratios of Li/Nb and Nb4+/Nb changed
very little, even after annealing at 600 degrees C for 1 h in a vacuu
m chamber from those for an as-received sample, but a TPD spectrum sho
wed the desorption of Li2O from the surface in the region of over 400
degrees C. The loss of Li and O, induced by annealing, was compensated
to a certain extent by the out-diffusion of these elements from the b
ulk. The crystal structure of the topmost layer of an as-received LiNb
O3 and its annealed one was detected as LiNbO3 from its threefold symm
etry on the azimuthal angle dependence of Nb signal intensities by CAI
CISS even after 600 degrees C annealing for 1 h. (C) 1998 Elsevier Sci
ence B.V. All rights reserved.