In this research, we succeeded in designing a new strategy to synthesize a unique thin film structured of nitrogen doped graphene (NGr) composite combined with coupled NiO/TiO2 hollow nanospheres using a synergistic hydrothermal method. The NGr@NiO/TiO2 composite characteristics are demonstrated by several rational characterization techniques such as the morphological shape of NiO/TiO2 hollow nanospheres which are evenly distributed on the surface of N-graphene with particle distribution in the range 79.78-362.13 nm with an average diameter of 130 nm. In addition, the crystal structures of carbon from NGr, NiO, and TiO2 (anatase and rutile) have been confirmed and proven by spectra showing the presence of C-N stretching primary amides (1400 cm− 1), Ni-O stretching (700 cm− 1) and Ti-O-Ti bond (425 cm− 1), respectively. The electrochemical test was carried out by optimizing the performance of cyclic voltammetry (CV) through parameters such as the influence of composition, scan rate, and cycle with the best conditions, namely composite ratio 80:10:10 (wt%), scan rate 50 mV/s, condition stable cycle and also calculated the high specific capacity value of 839.83 F/g. Based on this, it is revealed that NGr@NiO/TiO2 composites can explore the potential and be fully applied in the development of alkaline metal ion (AIB) batteries such as Li/Na/K.