A study of the combustion processes of Ti/CuO and Ti/CuO/NC nanothermites prepared via electrospraying was conducted in this work. For this purpose, the compositions were thermally conditioned at 350, 550 and 750 °C, as selected based on our initial differential scanning calorimetry-thermogravimetry (DSC/TG) investigations. The tested compositions were analysed for chemical composition and morphology using SEM-EDS, Raman spectroscopy and XRD measurements. Additionally, the thermal behaviour and decomposition kinetics of compositions were explored by means of DSC/TG. The Kissinger and Ozawa methods were applied to the DSC curves to calculate the reaction activation energy. SEM-EDS analyses indicated that sintering accelerated with increasing equivalence ratio and there was a strong effect on the sintering process due to cellulose nitrate (NC) addition. The main combustion reaction was found to start at 420-450 °C, as confirmed by XRD and Raman study of samples annealed at 350 °C and 550 °C. Moreover, increasing the fuel content in the composition led to lower Ea, higher reaction heats and a more violent combustion process. Conversely, the addition of NC had an ambiguous effect on Ea. Finally, a multi-step combustion mechanism was proposed and is to some extent in line with the more general reactive sintering (RS) mechanism. However, unusual mass transfer was observed, i.e., to the fuel core, rather than the opposite, which is typically observed for Al-based nanothermites.