The method of using deuterium probes was proposed for studying the defect structure of oxide nanoparticles. It was based on the fact that in the course of annealing nanoparticles in deuterium, clusters consisting of point defects and deuterium atoms are formed. The content of the clusters depended on the type of defects. The concentration of deuterium and the content of the clusters were determined by the method of nuclear reactions. The technique was applied to study the defect structures of the nanoparticles of YSZ10, cubic zirconium dioxide doped with yttrium, and TiO _(2) . The nanopowders of YSZ10 and TiO _(2) were synthesized by means of the laser evaporation of the ceramic target; besides, TiO _(2) was obtained using the sol–gel method. It was shown that the method of the use of deuterium probes allowed one to reveal the presence of one or several types of point defects in nanoparticles and determine their concentration in the bulk and near the surface of nanoparticles with an accuracy of several percent and sensitivity of about 0.01 at%.
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