The development of nanocomposite for magnetic fluid hyperthermia applications is in high demand and has captivated the interest of researchers in recent years. Herein, we report the synthesis by sol–gel method, heating ability, and the characterization of γ-Fe2O3@ZnO/Al nanocomposite with several techniques, including X-ray diffraction, Fourier transformer Infrared, Transmission electron microscopy, energy dispersive spectroscopy and vibrating sample magnetometer. X-ray diffraction and Rietveld analysis showed the formation of the nanocomposite with the presence of maghemite (γ-Fe2O3) and ZnO. The nanocomposite exhibits high crystallinity, small sizes, and superparamagnetic behavior. Langevin’s paramagnetism theory and the law of approach to saturation have been used to confirm superparamagnetism and to calculate the effective anisotropy constant, respectively. Heating ability was investigated as a function of concentration and field amplitude in an alternating magnetic field. We found that the nanocomposite rapidly reached the hyperthermia temperature (42 °C) under an alternating magnetic field in 160 s, and it could rise to 66 °C in 900 s with a specific absorption rate equal to 119 W · g−1 and intrinsic loss power equal to 1.95 nHm2 kg−1. The high crystallinity and intrinsic loss power values appear to be in the range of the reported commercial ferrofluids (0.20–3.10 nHm2 kg−1), strongly suggesting that the synthesized nanocomposite is a promising candidate for the application of photo/magnetic fluid hyperthermia.