Lab-made biosilica (SiO2) nanoparticles were obtained from waste biomass (rice husks) and used as eco-friendly fillers in the production of nickel matrix composite films via the co-electrodeposition technique. The produced biosilica nanoparticles were characterized using XRD, FTIR, and FE-SEM/EDS. Amorphous nano-sized biosilica particles with a high SiO2 content were obtained. Various current regimes of electrodeposition, such as direct current (DC), pulsating current (PC), and reversing current (RC) regimes, were applied for the fabrication of Ni and Ni/SiO2 films from a sulfamate electrolyte. Ni films electrodeposited with or without 1.0 wt.% biosilica nanoparticles in the electrolyte were characterized using FE-SEM/EDS (morphology/elemental analyses, roundness), AFM (roughness), Vickers microindentation (microhardness), and sheet resistance. Due to the incorporation of SiO2 nanoparticles, the Ni/SiO2 films were coarser than those obtained from the pure sulfamate electrolyte. The addition of SiO2 to the sulfamate electrolyte also caused an increase in the roughness and electrical conductivity of the Ni films. The surface roughness values of the Ni/SiO2 films were approximately 44.0%, 48.8%, and 68.3% larger than those obtained for the pure Ni films produced using the DC, PC, and RC regimes, respectively. The microhardness of the Ni and Ni/SiO2 films was assessed using the Chen-Gao (C-G) composite hardness model, and it was shown that the obtained Ni/SiO2 films had a higher hardness than the pure Ni films. Depending on the applied electrodeposition regime, the hardness of the Ni films increased from 29.1% for the Ni/SiO2 films obtained using the PC regime to 95.5% for those obtained using the RC regime, reaching the maximal value of 6.880 GPa for the Ni/SiO2 films produced using the RC regime.
