Composites of synthesized reduced graphene oxide (rGO) and titanium dioxide nanotubes (TNTs) were examined and combined at different mass proportions (3:1, 1:1, and 1:3) to develop an electrochemical double layer capacitor (EDLC) nanocomposite. Three different combination methods of synthesis—(1) TNT introduction during GO reduction, (2) rGO introduction during TNT formation, and (3) TNT introduction in rGO sheets using a microwave reactor—were used to produce nanocomposites. Among the three methods, method 3 yielded an EDLC nanomaterial with a highly rectangular cyclic voltammogram and steep electrochemical impedance spectroscopy plot. The specific capacitance for method 3 nanocomposites ranged from 47.26–165.22 F/g while that for methods 1 and 2 nanocomposites only ranged from 14.03–73.62 F/g and 41.93–84.36 F/g, respectively. Furthermore, in all combinations used, the 3:1 graphene/titanium dioxide-based samples consistently yielded the highest specific capacitance. The highest among these nanocomposites is 3:1 rGO/TNT. Characterization of this highly capacitive 3:1 rGO/TNT EDLC composite revealed the dominant presence of partially amorphous rGO as seen in its XRD and SEM with branching crystalline anatase TNTs as seen in its XRD and TEM. Such property showed great potential that is desirable for applications to capacitive deionization and energy storage.

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The capability of novel 3:1 reduced graphene oxide/titanium dioxide nanotubes (rGO/TiONTs) composite to desalinate using capacitive deionization (CDI) employing highly concentrated NaCl solutions was tested in this study. Parameters such as material wettability, electrosorption capacity, charge efficiency, energy consumption, and charge-discharge retention were tested at different NaCl initial concentrations—100 ppm, 2000 ppm, 15,000 ppm, and 30,000 ppm. The rGO/TiONTs composite showed good material wettability before and after CDI runs with its contact angles equal to 52.11° and 56.07°, respectively. Its two-hour electrosorption capacity during CDI at 30,000 ppm NaCl influent increased 1.34-fold compared to 100 ppm initial NaCl influent with energy consumption constant at 1.11 kWh per kg with NaCl removed. However, the percentage discharge (concentration-independent) at zero-voltage ranged from 4.9–7.27% only after 30 min of desorption. Repeated charge/discharge at different amperes showed that the slowest charging rate of 0.1 A·g−1 had the highest charging time retention at 60% after 100 cycles. Increased concentration likewise increases charging time retention. With this consistent performance of a CDI system utilizing rGO/TiONTs composite, even at 30,000 ppm and 100 cycles, it can be a sustainable alternative desalination technology, especially if a low charging current with reverse voltage discharge is set for a longer operation.