Electrothermal-Chemical Synthesis (ETCS) is a relatively new process for the synthesis of nanocrystalline powders. With ETCS nanoparticles are formed through the controlled chemical reaction of a metal plasma, produced by cathode erosion, with a gas. By controlling the quench rate of the plasma precisely, the average particle size can be varied from as small as 6–8 nm up to 100 nm and above. The process is quite versatile and can be used to produce a wide variety of nanopowders including metals, oxides, and nitrides. However, before the nanoparticles produced by this process (or any other process for that matter) can find wide scale commercial acceptance, their physical properties must be characterized. Among many characterization techniques, electron microscopy can provide structural, chemical, and morphological information on nanoparticles. In this paper, we will discuss the SEM and TEM characterization of metal and metal oxide nanoparticles powders produced by ETCS.