In the present study, manganese monoxide (MnO) which is hard to prepare because of the chemical activity of the manganese metal has been synthesized in nanofibrous form. An electrospun manganese acetate/poly(vinyl alcohol) nanofiber mats have been hydrothermally treated by novel strategy. The treatment process was based on producing of water gas (Co and H(2)) to eliminate the polymer and reduced the manganese acetate to manganese monoxide. The process was carried out by heating the dried nanofiber mates at 400 degrees C for 3 h in an especial designed reactor in which a stream of water vapor was passing through a bed of an activated carbon. The obtained physiochemical characterization results indicated that the proposed hydrothermal treatment process does have the ability to produce pure MnO nanofibers with good crystallinity. (C) 2009 Elsevier B.V. All rights reserved.