An attempt was made to synthesize coiled carbon fibers over nickel catalyst using acetylene as a carbon source at 700 degreesC by microwave technique. X-ray diffraction (XRD) and temperature-programmed oxidation (TPO) studies showed presence of disordered carbon in these materials. Highly coiled carbon fibers were observed by scanning electron microscopy (SEM). From a transmission electron microscopy (TEM) study, the average diameter of the fiber was measured approximate to200 nm. A Raman spectra of microcoiled carbon fiber was also recorded at room temperature under a nitrogen atmosphere. It has been observed that the surface area of the microwave derived microcoiled carbon was 62 m(2) g(-1). This value of surface area of microcoiled carbon was found to decrease with increasing temperature. (C) 2002 Elsevier Science B.V. All rights reserved.