In this chapter, the author will review several advanced microscopy techniques developed at the N"S" Glenn Research Center in the last years. Topical areas include unconventional approach to investigate the fine nanoporous structure of aerogels by scanning electron microscopy, new limits for transmission electron microscopy investigation of dispersion and chirality of single-walled carbon nanotubes within a polymer matrix, the importance of microstructure of porous tin dioxide nanostructure that lead to first time detection of methane at room temperature without doping or catalyst, in situ SEM methods to study the thermal stability of nanoparticles on Graphene/Cu based materials, electron beam irradiation effects on carbon nanotube yarns electrical properties, and nanoindentation work of multiphase thermoelectric material.Keywords: Electron microscopy, "erogels, CNT, SnO , Graphene/Cu, WSi /SiGe . Introduction Nanomaterials can have a direct impact on N"S" missions in areas of engineered materials and structures, devices, electronics, energy generation and storage, and sensors among others [ ]. Nanomaterials can offer up to percent weight savings, and thus cost [ ]. This chapter will review several advanced microscopy techniques developed and applied to cutting-edge nanomaterials research at N"S" Glenn Research Center GRC in the last years [ ]. The first © 2015 The Author(s). Licensee InTech. This chapter is distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.topic investigates the examination of the nanoporous structure of aerogels with a scanning electron microscopy SEM technique. "erogels are emerging materials with the promise of unusually high strength for some cases , thermal insulation, and damping capability combined with very light weight. "ecause of these properties, aerogels have been used in several N"S" missions to collect comet dust particles and provide thermal insulation of components in Mars rovers, for instance [ ]. Other current applications include thermal insulation for inflatable reentry decelerators and extra-vehicular activity suits [ ]. Many of the outstanding physical properties of aerogels depend on their porous structure. SEM is a commonly used technique to estimate the pore size in aerogels, but is hampered by charging, the accumulation of electrons on the surface of the sample. The common solution employed to minimize charging effects is to deposit a layer of a conducting material on the sample. However, this technique can drastically mask the intrinsic porous structure of the aerogel. Here it is shown that negative charging effects on aerogels can be dissipated using nitrogen gas [ -].The second subject will be carbon nanotube CNT /polymer nanocomposites, which have excellent promise for improved strength and light weight and are being actively researched in a number of N"S" projects. Rec...