In this study, an abundant and eco-friendly photocatalytic material, Fe 2 O 3 particles were synthesized by sonochemical method. Morphological and microstructural investigations of synthesized undoped and Ni, Co-doped Fe 2 O 3 particles were performed. The effect of particle morphology and microstructure on its photocatalytic performance was further investigated. Comparative studies for evaluating particle crystallite sizes were conducted by Williamson-Hall (W-H) method and modified Debye-Scherrer (MDS). Crystallite sizes and lattice strains of Fe 2 O 3 induced by process parameters were calculated by W-H method based on uniform deformation model (UDM). The crystallite sizes of the synthesized powders were calculated in the range of 200 nm and 76 nm by Williamson-Hall analysis. In addition to structural investigation, dislocation density of the synthesized particles was calculated by Williamson-Smallman relation. Afterwards, photocatalytic performance of Fe 2 O 3 particles was investigated in detail. The photodegradation of methylene blue solutions in the presence of light in 20 min with samples 3,4, and 5 in 20 min were 0.937, 0.896, and 0.855, respectively. Moreover, the photodegradation of methylene blue solution with sample 5 for 15, 30, and 45 min were 0.9, 0.828, and 0.757, respectively. A photocatalytic activity of 24.25% has been observed under optimum conditions for the time interval of 45 min.