On the basis of glancing-incidence X-ray diffraction (GIXRD) spectra collected at different incidence angles, it is possible to obtain structural information at different depths. In the case of an ideal crystalline material, the integrated intensity of each crystalline-phase reflection is correlated to the irradiated volume of the phase. In this work, it is shown that quantitative information on the thickness of thin polycrystalline layers can be obtained by means of GIXRD. Experiments have been performed on thin films of gold with different thicknesses, sputtered on glass slides. The film thickness has been carefully evaluated by X-ray reflectivity (XRR) experiments. XRR and GIXRD data are compared, and the consistency of the thickness values of the crystalline gold layer is shown.

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The development of new devices has created needs of precision, conformal at the atomic level deposition of high quality thin film materials. In the last years, Atomic Layer Deposition (ALD) has received much interest as a potential deposition method for advanced thin film structures. ALD presents several advantages: the film is excellently conformal and reproducible; the film thickness depends only on the number of reaction cycles, which makes the thickness control accurate and simple; the film can be deposited onto all kind of substrates. Because of the process slowness, layer thickness is generally less than 100 nm. This makes more difficult to study all characteristics of the coating. Thin layers deposited onto bulk substrates are generally in tensile or compressive stress state, which may significantly affect physical properties and possibly compromise their lifetime. To determine the residual stress it is mandatory to know the elastic constants that may also depend on the microstructure of the layers and thus the deposition process.In this work, 2D X-ray diffraction (XRD 2 ) in combination with in situ tensile testing has been applied for the first time to measure elastic properties of TiO 2 anatase films obtained by ALD. Experimental conditions, the tensile stage being installed in a laboratory micro-diffractometer equipped with a 2D imageplate detector, and the information that can be extracted from 2D diffraction patterns will be discussed. Based on these preliminary results, synchrotron radiation beam time has been allocated to study elastic properties of these thin films. The advantages and disadvantages of the proposed laboratory equipment, with respect to the synchrotron beam lines, are discussed.

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One of the main problems in electrochemical Pd deposition of coatings is the hydrogen desorption that causes microcracking phenomena. With the aim of understanding the structural changes due to the hydrogen desorption, the kinetics of the phase transformation from hydride to metallic structure has been followed by in situ X-ray diffraction (XRD) experiments. The structural evolution of samples obtained by two different electrochemical baths has been compared. It was found that the solubility and the desorption kinetics of hydrogen are significantly influenced by the presence of structural defects. Residual stresses have been evaluated for both samples by means of 2D X-ray diffraction (XRD 2 ). The presence of amine complexes in the bath seems to contribute to reducing the crystalline dimension of the Pd-phase, and the differences between the specific volumes of a and b phases is reduced for nanostructured coatings.