Co-Tm nano-spinel ferrite with chemical formula CoTmxFe2-xO4 (0.0 <= x <= 0.08) NPs were prepared via sonochemical approach. X-ray powder diffraction patterns, microscopic images (SEM and TEM) and infrared spectra proved the formation of Co spinel ferrite. The effect of Tm3+ substituted on spinal structure was evaluated by lattice parameters, tetrahedral and octahedral bond length and cationic distribution. The band gap energy (Eg) of samples were estimated by performing UV-Vis percent diffuse reflectance (% DR) and applying the Kubelka-Munk theory. Eg values are in an interval between 1.33 eV and 1.64 eV. The analyses of magnetization were performed at room (300 K; RT) and low (10 K) temperatures. Different magnetic parameters including coercivity H-c, saturation magnetization M remanence M-r, squareness ratio (SQR = M-r/M-s) and magnetic moment n(B) were deduced and discussed. The results showed superparamagnetic (SPM) nature at RT for x = 0.00 and 0.02 samples. However, the other products exhibit ferromagnetic (FM) nature. At 10 K, all synthesized NPs display FM behavior. An amazing increase in the magnitudes of M-s, M-r and H-c was observed at 10 K in comparison to RT, which is principally due to the reduced thermal fluctuations of magnetic moments at lower temperatures. The Tm3+ substitution affects considerably the magnetizations data. An enhancement in the M M-r, and n(B) was detected on increasing the Tm3+ concentration. The SQR values at RT are found to be smaller than 0.5 postulating a single domain nature with uniaxial anisotropy for all produced ferrites. However, SQRs are in the range 0.66-0.76 at 10 K, suggesting the multi magnetic domain at low temperature, except the x = 0.02 product where the SQR = 0.47 indicating the single magnetic domain. The obtained magnetic results were investigated deeply with relation to structural and microstructural properties.