In this study, Iron oxide nanoparticles (Fe₂O₃ NPs) were synthesized using iron chloride hexahydrate (FeCl·6HO) and ammonia solution through a straightforward co-precipitation method. The nanoparticles were annealed at temperatures of 100 °C, 300 °C, 500 °C, 700 °C, and 900 °C, with one sample left unannealed. Comprehensive analyses were performed using X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Zeta potential, Dynamic Light Scattering (DLS), Scanning Electron Microscopy (SEM), and UV-Vis Spectrophotometry. The XRD patterns confirmed the presence of both Maghemite (γ-FeO) and Hematite (α-FeO) phases, with a phase transition observed between 100 °C and 300 °C, and the most pronounced transition occurring at 500 °C. At this optimal temperature, the crystallite size was 19.14 nm, the average particle size was 37.36 nm, and the band gap energy was measured at 1.76 eV. SEM images revealed that nanoparticles formed clusters as the annealing temperature increased. The zeta potential measurements showed a range from 6.12 mV at 100 °C to -1.9 mV at 900 °C, indicating changes in particle stability. DLS analysis indicated a size increase from 86.81 nm at 300 °C to 1577 nm at 900 °C, reflecting aggregation trends. The reduction in band gap energy with higher temperatures is attributed to enhanced crystallinity and increased particle size. The magnetic properties of Fe₂O₃ NPs were evaluated using a Physical Property Measurement System (PPMS), revealing an increase in magnetic response with rising annealing temperatures. The transition from superparamagnetic γ-Fe₂O₃ to weakly ferromagnetic α-Fe₂O₃ was confirmed through changes in the hysteresis loop area and shape. These findings suggest that 500 °C is the optimal annealing temperature for producing Fe₂O₃ NPs with desirable properties for applications in targeted drug delivery, MRI contrast enhancement, and environmental remediation. This research advances the engineering of Fe₂O₃ NPs, paving the way for their use in various technological applications.