Solid oxide electrochemical cells (SOCs) consisting of solid oxide fuel cells (SOFCs) and solid oxide electrolysis cells (SOECs) are widely studied for the development of high-efficiency energy generation and storage devices. To investigate the effect of precursor particle size on the microstructural and morphological properties of the electrode, glycine nitrate process and solid-state reaction ball-milling were utilized as synthesis methods for Nickel oxide-scandia stabilized zirconia (NiO-ScSZ) powders. The synthesized powders were then screen-printed on commercial YSZ solid electrolyte substrates. The structure and morphology of the sintered electrodes were investigated. Particle size analysis (PSA) revealed that NiO-ScSZ precursor powders obtained from GNP ball-milled had a smaller average particle size than solid-state reaction ball-milled powders. For the sintered NiO-ScSZ films, cubic structures of both NiO and ScSZ have been observed from the X-ray diffraction (XRD) patterns. A better porous morphology with less agglomeration and better dispersion of NiO and ScSZ phases was revealed by the scanning electron microscopy (SEM) micrographs and elemental mapping for the GNP-ball-milled synthesized powders.