Real time in situ diagnostics of PVD growth using synchrotron radiation

For specific applications of hard coatings, the microstructure (or nanostructure) has to be tailored for optimum performance. This requires information about the mechanisms of growth and the connection between the microstructure and the deposition parameters. In order to obtain this knowledge, in situ real time growth studies of magnetron-sputtered thin films were carried out. A growth chamber, equipped with two magnetrons and Kapton windows for X-ray diffraction and reflectivity, was mounted on a six-circle goniometer at a synchrotron beam line at ESRF in Grenoble. As an example, X-ray diffraction measurements were carried out in situ during growth of TiN to follow the development of the microstructure. Recrystallization was identified as the mechanism which controlled the development of texture. The driving force for these texture changes arose from minimalization of the sum of the surface energy and the strain energy of the individual grains. As another example, the heteroepitaxial growth of TiN on MgO(001) was studied. Bragg-Brentano as well as grazing-incidence in-plane wide angle scattering was used to establish the pseudomorphic growth of TiN to the underlying MgO(001). Using real-time specular X-ray reflectivity, layer-by-layer growth was observed, with the surface roughening decreasing with an increase in the deposition temperature. The growth of nanocrystalline Au was also investigated. Among the results we found that changes in the (111) fiber texture arose from grain rotations.