This paper compares the photoelectrochemical performances of nickel oxide (NiO) thin films processed using two different sintering procedures: rapid discharge sintering (RDS) and conventional furnace sintering (CS). Prior to sintering, NiO nanoparticles were sprayed onto substrates to form loosely adherent nanoparticulate coatings. After RDS and furnace sintering the resultant NiO coatings were sensitized with erythrosine B dye and corresponding p-type dyesensitized solar cells were fabricated and characterized. NiO electrodes fabricated using the RDS technique exhibited a fourfold enhancement in electroactivity compared to CS electrodes. A possible explanation is the smaller sintered grain size and more open mesoporous structure achieved using the microwave plasma treatments.