With the development of material sciences, the characterization of nanomaterials has become a critical issue in managing their fascinating size-dependent physical and chemical properties. Controlling these properties from synthesis to the application phase, and consequently to their fate as a worldwide environmental is becoming more and more imperative. More specifically, semiconductor nanomaterials are promising for applications in many fields based on energy storage and conversion (e.g. solar cells, batteries, LED, waveguide, chemicals and biosensors, nanoscale devices for electronic, for lasers) that show some economic potential worldwide. We will show that microwave chemistry is an alternative technique to conventional chemistry methods (e.g. colloidal, sol-gel, hydrothermal), for elaboration of semiconducting nanostructures when synthesis parameters such as power and temperature range, are controlled [1]. Then we will go on to concepts on nanometrology in regards to specific nanoparticles (CdS, ZnS, ZnO, Sb2S3, Sb2Se3, and coated systems). Nanometrology is thus a logical step towards a complete monitoring of their properties throughout their life-cycle. We will focus on joint physical and chemical characterization (TEM, X-Ray Diffraction, Raman, Photoluminescence, Absorption Spectroscopy, XPS and Mass Spectrometry) to explore the size, geometry and activity of these small quantum dots [2]. In-situ high-temperature XRD characterization will be also described showing how to follow formation of crystallographic phases during an annealing process [3]. Finally we will evaluate the potential use of some of these nanosystems at an industrial scale. [1] M. Fregnaux, S.Dalmasso, P. Durand, Y. Zhang, J.J. Gaumet and J.P. Laurenti, Mater. Chem. Phys. 52-60 (2013): 142 (1). [2] J.J. Gaumet, G. Gaiffe, C. Dezanet, S. Dalmasso, P. Magri, L. Balan and R. Schneider: MRS Symp. Proc., 7-12, (2015): 1793. [3] W. Luo, F. Li, J.J. Gaumet, P. Magri, S. Diliberto, L. Zhou, L. Mai, Adv. Energy Mater. 1703237 (2018)