This paper introduces a novel method for fabricating copper (Cu) oxide/activated carbon fibre (ACF) through the aerosol palladium (Pd) activation for use in electroless Cu deposition and heat treatment of Cu deposited ACF with nitric monoxide (NO) gas injection. Electroless Cu deposition was initiated by catalytically activating the ACF surface with spark generated Pd aerosol nanoparticles. The catalytically activated ACF was placed into a solution used for the electroless Cu deposition. Subjecting the Cu deposited ACF to a heat treatment in a NO/nitrogen (N 2) gas injection (1000 ppm NO) resulted in changes to the morphology of the Cu particles. As the temperature increased from 100 to 500 • C, the relative mass fraction of oxygen in the Cu particles increased from 3.6% to 14.2% and the fraction of Cu decreased from 41.2% to 34.1%, which was caused by the formation of Cu oxides (Cu 2 O and CuO). The corresponding surface area and pore volume of the ACF decreased from 1019 m 2 g −1 to 401 m 2 g −1 and from 0.40 cm 3 g −1 to 0.18 cm 3 g −1 , respectively. The morphological evolution and decrease in porosity were attributed to volume expansion of Cu particles during oxidation.