The investigation of nanosize thin film multilayer structures is needed in knowledge of the element concentration, the crystal structure and the thickness for every layer of the structures. Moreover, it is very important to have the information about properties of interlayer spaces. Again, the knowledge is usually obtained in result of intercomplamentary investigations. Because of this, the control methods must be characterized by the nondestructive influence on the structures. The complex of specific X-ray and ion beam testing methods can be effectively used for this problem solution.
The Rutherford backscattering of He⁺ and H⁺ ion fluxes by a multilayer target is the perfect method which allows to determinate the depth multielement concentration profile for it with thickness resolution near 10-20 nm. In case of the insufficient sensitivity of RBS method the measurements can be completed by the nuclear reaction spectrometry, the recoil nuclears method and the registration of X-ray fluorescence yield. The sensitivity maximum of X-ray fluorescence spectrometry can be achieved in condition of X-ray exciting beam total reflection on the surface target studied (in the framework of TXRF method). The using of planar X-ray waveguide-resonator (PXWR) for the exciting beam formation allows to improve TXRF method characteristics additionally. The method diagnoses the target element composition for very thin surface layer with thickness near 5 nm. The depth element diagnostics is possible in condition of the angular variation for X-ray exciting beam.
The crystal structure for every layer of the multilayer target can be studied by the initial X-ray beam grazing diffraction. The grazing diffraction efficiency can be enhanced by PXWR application. The complex method investigation is suitable for any structure state of layer, but it’s efficiency maximum will achieve at the epitaxial structure study.All possibilities of the complex method are illustrated experimentally.

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