Local-made electrospun machine is firstly constructed. Poly Vinyl Alcohol/ Zinc acetate (PVA/Zinc acetate) composite fibres, different molarities of (0.2 M, 0.3 M, 0.4 M, 0.5 M) are formed on Al-foil substrate by electrospinning technique. Electrospum Poly Vinyl Alcohol/Zinc Oxide (PVA?ZnO) submicron fibres of (0.2 M, 0.5 M) are successfully formed by calcinations at high temperature. Scanning Electron Microscopy (SEM) analysis is carried out to examine the fibre diameter and microstructural properties of both submicron fibres