This study addresses a scientific challenge by elucidating the influence of calcination temperature on the properties and electromagnetic wave absorption capabilities of NiCo2O4, a material whose performance is inherently tied to its preparation process. Specifically, we systematically investigate how varying calcination temperatures not only diversify the material’s composition and morphology but also enhance its electromagnetic wave absorption properties. By controlling the calcination temperature, we not only achieve the successful synthesis of NiCo2O4 but also unravel intricate correlations among calcination conditions, material composition, and wave absorption performance. Notably, NiCo2O4 sample calcined at 400 °C exhibits remarkable electromagnetic wave absorption, marked by an exceptional maximum reflection loss of −53.93 dB and a broad absorption bandwidth spanning 6.24 GHz. These insights contribute to advancing the frontiers of NiCo2O4 utilization, particularly in the realm of electromagnetic wave absorption and beyond, underscoring the novelty and impact of our research.