The structure of nanomaterials can be evaluated using diffraction techniques such as Xray diffraction (XRD), and electron diffraction (ED, selected area electron diffraction (SAED). XRD is used for crystalline materials with sharp diffraction peaks at specific Bragg angles. The structure of poor crystalline materials can be solved via the pair distribution function (PDF) using the XRD pattern. XRD requires a big crystal to perform single-crystal XRD (SXRD). Small crystals can be characterized using powder XRD (PXRD). The structure solution of small crystals such as nanoparticles using PXRD is a big challenge due to several reasons such as peaks overlap, and preferred orientation. Thus, techniques such as SAED are used to calculate the unit cell parameters that can be then used to refine the PXRD data for structure solution. XRD offers the structure for the crystal's average. In some cases, the changes in the material take place in the point or plane of the crystal. Thus, it is hard to use XRD for the material characterization. This challenge can be solved using local structure techniques such as Mössbauer spectroscopy, X-ray absorption spectroscopy (XAS, e.g., extended XAS fine structure (EXAFS), electron energy loss spectroscopy (EELS), and X-ray absorption near edge structure (XANES)), and XPS. The connectivity can be also evaluated using techniques such as Fourier transform infrared (FT-IR), and nuclear magnetic resonance (NMR). The inner electronic structure (e.g. oxidation state and the ratio of multi-valence element) of specific atoms in a material can be characterized using techniques such as X-ray fluorescence (XRF), particle-induced X-ray emission, XPS, and Auger electron spectroscopy.