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A new method is suggested for simultaneous determination of small misorientations of the surface from the chosen crystallographic plane and the thickness of the surface amorphous layer. The method is based on X-ray diffraction experiments under specular reflection conditions. The determination of misorientation consists of the comparison of diffraction curve intensities for hkl and {\bar h}{\bar k} {\bar l} reflections obtained from the plane normal to the crystallographic plane along which the crystal surface is cut. The accuracy of the determination exceeds the accuracy known for other methods. The amorphous layer is considered to be either an oxide film or any other disordered layer having no crystal structure. The layer thickness is determined from the consideration of the diffraction curve shapes using comparison with theoretical calculations. The method provides detection of layers ~5 Å in thickness, which seems to be unique for X-ray diffraction methods. The method may find wide application in the surface analysis of perfect crystalline specimens, in particular, of materials used in semiconductor microelectronics.

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