This paper describes the result of investigation on PVA/FeCl3 nano composites fibres prepared by the electrospinning process. The effects of instrument parameters including solution concentration, electric voltage, tip-target distance, flow rate parameters on the morphology of electrospun PVA/FeCl3 fibres were evaluated. The produced composite fibres were characterized by scanning electron microscopy (SEM) and transmission electron microscope (TEM). Fibre mats of (PVA)/FeCl3 composite thin fibres, in the diameter of 500-1100 nm, were prepared by electrospinning. These microscopies show detailed morphologies of PVA/FeCl3 nano composites incorporating magnetic power. These novel composite fibres could be used in biomedical, catalyst and magnetic purpose.