IR results showed that all the organic molecules could be removed completely from PVA/nickel acetate composite fibres after calcination at 700 C, and a new peak around 442 cm 1 assigned to m of nickel oxide (NiO) appeared [17,18], indicating that the fibres obtained at this temperature were pure inorganic NiO species. Fig. 1 gave the WAXD curve for various fibres samples.