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Practical aspects of preparation and prospects for practical use of a series of the metal oxide whiskers were studied. The procedures for the synthesis were proposed, and the phase composition, micromorphology, and electrochemical and sensor characteristics of the macroscopic (up to 5–10 mm long) whiskers in the Ba-V-O, Ba-Mn-O, and Sn-O systems were analyzed. The electroconducting BaV8O21-δ whiskers were prepared by the hydrothermal treatment. These whiskers possess stable electrochemical characteristics appropriate for the development of novel secondary current sources. The protonated form of the Ba6Mn24O48 whiskers produced by the isothermal vaporization of chloride fluxes is a mixed conductor with the proton and electron conductivity at a level of mS units at 25 °C. A new procedure by the thermal disproportionation of tin(ii) oxide under nitrogen was proposed for the growth of SnO2 whiskers of various morphology. The produced whiskers have substantial sensor sensitivity toward a series of toxic components of the gaseous medium, such as nitrogen dioxide.