The staff of US Nanocorp, Inc. are developing unique nanostructured materials for a wide range of applications in the areas of energy storage (batteries and ultracapacitors) and energy conversion (fuel cells and thermoelectric) devices. Many of the preparations of these materials exploit a wet synthesis process (patent pending) that is scaleable to large volume manufacturing and anticipated to be low in cost. Specifically, both the β-form of nickel hydroxide and the hollandite form of manganese dioxide have been synthesized. The hexagonal Ni(OH) 2 is anticipated to significantly boost energy densities in nickel-alkaline batteries, including nickel/cadmium, nickel/metal hydride and nickel/zinc. The nanophase MnO 2 microstructure exhibits an unusual tunnelled tubular geometry within a bird's nest superstructure, and is expected to be of interest as an intercalation cathode material in lithium-ion systems as well as a catalyst for fuel cells. Characterization of these materials has been by the techniques of high resolution SEM and TEM, as well as XRD. Both Hg porosimetry and BET surface measurements for conventional and spherical nickel hydroxides are summarized. Pore distribution and electrochemical activity for the nanophase materials will be examined in the future.