NiO doped  catalytic fibres were prepared by coating electrospun  catalytic fibres by wet impregnation using three types of nickel salts,    and  each at three concentrations so as to yield final dry weight ratios of Ni : Si of 7 : 3, 8 : 2 and 9 : 1, prior to calcination at 500°C to form NiO crystalline coatings. Scanning electron micrograph based analysis of all nine different sets of fibres revealed that the surface roughness of the NiO-coated electrospun  (catalyst) fibres increased with an increase in the Ni : Si weight ratio. The X-ray diffractograms revealed that the structure of NiO appears on catalyst fibres that were prepared from  and  but not from  Similarly, X-ray fluorescence analysis of the fibres indicated that the percentage of NiO formed on the catalyst fibres increased with as the % (w/w) Ni composition increased. There was no NiO formed on catalyst fibres prepared from  solution.