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In this work, a method that takes advantage of the three-dimensional nature of the X-ray multiple-diffraction (MD) phenomenon for evaluating the crystalline perfection of semiconductors is proposed. The energy-transfer process among the MD beams can occur in a kinematical (secondary extinction) or a dynamical (primary extinction) regime. The effects that each regime can have on MD Bragg condition are theoretically investigated. The method provides information on size and misorientation of perfect-crystal regions as well as on the probability of interaction between them. The perfection of GaAs and Ge (001) surfaces after mechanical and/or chemical polishing has been investigated with this method and, as an extension of its applicability, porous silicon and GaAs (001) with Se ions implanted were also investigated.

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