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Ni substituted lanthanum manganite of LaMn1−XNiXO3 (x = 0.2, 0.4, 0.5, 0.6, 0.7) of a single phase perovskite structure was synthesised through sol-gel technique. The effect of Ni substitution by varying Ni and Mn amount ratios over LaMn1−XNiXO3 materials were studied. The physio-chemical characteristics like crystallinity were confirmed by XRD, surface area by BET analysis, metallic surface area by CO chemisorption. The optimal level of Ni substitution increases surface area, pores volume and metallic surface area, which leads highly stability. The oxygen vacancies and rapid migration of lattice oxygen from the bulk toward the surface was observed over LaMn0.4Ni0.6O3 compared to other perovskite materials. The LaMn0.4Ni0.6O3 perovskite materials show high surface area, metallic area with absorbed oxygen due to threshold Ni and Mn ratio leads the perfect synergic balance.