We report the fabrication of porous titanium nitride (TiN) monoliths through the ammonolysis of porous TiO 2 monoliths prepared via the sol-gel process accompanied by phase separation. The obtained TiN monoliths possess good mechanical strength as well as excellent electric conductivity with a superconducting transition at T c ∼5.0 K. We have investigated the electrochemical properties of the porous TiN monoliths as an electrode using various electrolytes. The results reveal that the pseudocapacitance of TiN increases in the order of K + < Na + < Li + contrary to the case of EDL capacitance in neutral aqueous electrolytes. It is also found that acidic and strongly basic electrolytes are not suitable due to high corrosivity, while there is no significant deterioration when neutral aqueous electrolytes and organic electrolytes are used.Titanium nitride (TiN) exhibits significant potential in various electrochemical applications 1-8 owing to the unique intrinsic features such as excellent electric conductivity, high mechanical strength, and good chemical and thermal stabilities. One of the promising electrode applications of TiN electrodes is pseudocapacitors. 3-5 Meanwhile, the previous efforts devoted to the study on TiN materials disclose that the slightly oxidized layer is formed on TiN surface, 9-11 which indicates the oxidized surface significantly contributes to the interfacial reaction between electrolyte and electrode involving surface corrosion by polarization. Hence, fundamental understandings of the electrochemistry and stability of TiN surface are indispensable for the practical use of TiN pseudocapacitors. Nevertheless, there are only a few studies reported on the electrochemistry of TiN associated with surface corrosion chemistry. 9,12-14 The research from a longitudinal perspective, which is of importance from an application perspective, is especially limited to the investigation in KOH aqueous solution. 3,13 The recent upsurge of interest in TiN electrodes therefore desires comprehensive studies on the electrochemistry of TiN in a variety of electrolytes.In most cases, composite electrodes prepared from slurry composed of active materials, binders and conductive additives (generally carbon) are employed. However, the composite electrodes are not suitable for the fundamental studies, because the additives and the mixing process to prepare the slurry may change various properties, such as morphology and surface chemistry, of the electrode materials, which makes it difficult to obtain intrinsic information on the active material itself. On the other hand, porous monolithic electrodes [15][16][17][18] can overcome these issues, as they consist of a single piece of bulk electrode without any binders. In order to fabricate the monolithic electrodes, the control of pore properties is crucial, because porous structures are indispensable to allow the electrolyte to penetrate inside of the monolithic electrodes. 19 To date, we have developed the phase-separation method, a sol-gel process accompanied by spinod...