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Grazing incidence small-angle X-ray scattering was used to study monocrystalline silicon samples implanted with deuterium ions at an energy of 24 keV and to the dose of 2 × 1016 ions/cm2. Samples were annealed isochronally at different temperatures in the range from 393 to 973 K. Due to the relaxation of the defects structures, i.e. redistribution of vacancies and deuterium, strong particle like contribution is observed in addition to the rough surface scattering, already at 393 K annealing. During the annealing, this particles (agglomerations of vacancies) are gradually dissolved till 623 K annealing temperature. Another agglomeration mechanism takes over at about 773 K when a different type of particle growth is observed, and these are dissolved again at about 973 K. The sizes of detected particles are in 2-3 nm range. Also, the interference type of scattering from a film of about 30 nm thickness (the top layer, mostly unaffected by implantation) is observed. This film is gradually getting thinner with the increasing annealing temperature, due to the redistribution of the defects and the structure relaxation.

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