Nanoscale local atomic and structure determines most of unique properties of novel materials without long range order. To study its fine details one has to use both computer nanodesign and advanced experimental methods for nanodiagnostics. The status of modern theoretical analysis of the experimental x-ray absorption spectra to extract structural parameters is presented. Novel in- situ technique for nanodiagnostics - extracting of 3D structure parameters on the basis of advanced quantitative analysis of X-ray absorption near edge structure (XANES) - has been developed. The possibility to extract information on bond angles and bond-lengths (with accuracy up to 1 picometer) is demonstrated and it opens new perspectives of quantitative XANES analysis as a 3D local structure probe for any type of materials without long range order in atoms positions (all nanostructured materials and free clusters belong to this class of materials). Even more possibilities are opening by using simultaneously several experimental synchrotron based techniques: XANES, XES (X-ray Emission Spectroscopy) and RIXS (Resonant Inelastic X-ray Scattering), opening a possibilities to study the oxidation state of the ions inside the materials and the distribution of electron Density of States (DOS) in both valence and conduction bands of the nanostructured materials under the study.
The review of results obtained by this method for a wide class of nanostructured objects is presented: dilute magnetic semiconductors in the form of arrays of ZnO nanoneedles, thin films (ZnO: Mn, Co), ZnO: Mn nanowires, core-shell nanowires ZnO / ZnO : Mn, free copper nanoclusters, free titanium and the titanium oxide nanoclusters, Au complexes perspective as novel anticancer drugs . Another important application of this method is the possibility to analyze the time-dependent processes, in particular, to study the dynamics of nanoscale atomic and electronic structure of materials with high temporal resolution (up to 100 picoseconds). Some of the methods mentioned above could be realized only at large scale synchrotron radiation facilities, but another ones, for example XANES technique, could be performed using laboratory-scale devices (see http://nano.sfedu.ru/Rigaku.html).