In this study, carbon-supported MnO₂ nanocomposites have been prepared using the microwave-assisted heating method followed by two different approaches. The MnO₂/C nanocomposite, labeled as sample S1, was prepared directly by the microwave-assisted synthesis of mixed KMnO₄ and carbon powder components. Meanwhile, the other MnO₂/C nanocomposite sample labeled as S2 was prepared indirectly via a two-step procedure that involves the microwave-assisted synthesis of mixed KMnO₄ and MnSO₄ components to generate MnO₂ and subsequent secondary microwave heating of synthesized MnO₂ species coupled with graphite powder. Field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and inductively coupled plasma optical emission spectroscopy have been used for characterization of MnO₂/C nanocomposites morphology, structure, and composition. The electrochemical performance of nanocomposites has been investigated using cyclic voltammetry and galvanostatic charge/discharge measurements in a 1 M Na₂SO₄ solution. The MnO₂/C nanocomposite, prepared indirectly via a two-step procedure, displays substantially enhanced electrochemical characteristics. The high specific capacitance of 980.7 F g⁻¹ has been achieved from cyclic voltammetry measurements, whereas specific capacitance of 949.3 F g⁻¹ at 1 A g⁻¹ has been obtained from galvanostatic charge/discharge test for sample S2. In addition, the specific capacitance retention was 93% after 100 cycles at 20 A g⁻¹, indicating good electrochemical stability.

This study focuses on fabricating cobalt particles deposited on graphitic carbon nitride (Co/gCN) using annealing, microwave-assisted and hydrothermal syntheses, and their employment in hydrogen and oxygen evolution (HER and OER) reactions. Composition, surface morphology, and structure were examined using inductively coupled plasma optical emission spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction. The performance of Co-modified gCN composites for the HER and OER were investigated in an alkaline media (1 M KOH). Compared to the metal-free gCN, the modification of gCN with Co enhances the electrocatalytic activity towards the HER and OER. Additionally, thermal annealing of both Co(NO₃)₂ and melamine at 520 °C for 4 h results in the preparation of an effective bifunctional Co₃O₄/gCN catalyst for the HER with the lower E_onset of −0.24 V, a small overpotential of −294.1 mV at 10 mA cm⁻², and a low Tafel slope of −29.6 mV dec⁻¹ in a 1.0 M KOH solution and for the OER with the onset overpotential of 286.2 mV and overpotential of 422.3 mV to achieve a current density of 10 mA cm⁻² with the Tafel slope of 72.8 mV dec⁻¹.

The production of high-purity hydrogen from hydrogen storage materials with further direct use of generated hydrogen in fuel cells is still a relevant research field. For this purpose, nickel-molybdenum-plated copper catalysts (NiMo/Cu), comprising between 1 and 20 wt.% molybdenum, as catalytic materials for hydrogen generation, were prepared using a low-cost, straightforward electroless metal deposition method by using citrate plating baths containing Ni²⁺–Mo⁶⁺ ions as a metal source and morpholine borane as a reducing agent. The catalytic activity of the prepared NiMo/Cu catalysts toward alkaline sodium borohydride (NaBH₄) hydrolysis increased with the increase in the content of molybdenum present in the catalysts. The hydrogen generation rate of 6.48 L min⁻¹ g_cat⁻¹ was achieved by employing NiMo/Cu comprising 20 wt.% at a temperature of 343 K and a calculated activation energy of 60.49 kJ mol⁻¹ with remarkable stability, retaining 94% of its initial catalytic activity for NaBH₄ hydrolysis following the completion of the fifth cycle. The synergetic effect between nickel and molybdenum, in addition to the formation of solid-state solutions between metals, promoted the hydrogen generation reaction.

The perfect strategy for the generation of green and renewable hydrogen (H₂) fuels is the direct electrocatalytic splitting of plentiful seawater rather than scarce freshwater. One of the half-reactions taking place during the electrocatalytic splitting of seawater is oxygen evolution (OER). However, the OER is affected by slow four-electron transfer kinetics as well as competitive chlorine evolution reactions (CERs) in seawater. To overcome the kinematic and competitive barriers of seawater splitting and achieve an excellent overall performance of seawater splitting, we herein report a facile, low-cost, one-step fabrication procedure of 3D structured nickel–manganese (NiMn) coatings using a dynamic hydrogen bubble template (DHBT) technique. The electrocatalytic activities of the thus synthesized catalytic materials for OER in simulated seawater (0.5 M NaCl + 1 M KOH, denoted as SSW) and alkaline natural seawater (natural seawater + 1 M KOH, denoted as ASW) were investigated using linear sweep voltammetry (LSV) at varying temperatures from 25 to 75 °C. Scanning electron microscopy (SEM) and inductively coupled plasma–optical emission spectroscopy (ICP–OES) were used to examine the surface morphology and composition of the prepared catalysts. It was found that the prepared NiMn/Ti-1 catalyst in a plating bath containing a molar ratio of 1:1 Ni²⁺:Mn²⁺ and having the lowest Mn loading of 13.43 µg cm⁻² exhibited quite reasonable activity for OER in Cl⁻ ion rich SSW and ASW. To achieve the benchmark current density of 10 mA cm⁻² in SSW and ASW, the NiMn/Ti-1 electrocatalyst requires overpotentials of 386 and 388 mV, respectively. In addition, this optimal bimetallic electrocatalyst also demonstrated superior long-run stability at 1.81 V (vs. RHE) and 10 mA cm⁻² for 24 h in both working electrolytes. Impressively, the two-electrode electrolyzer—NiMn/Ti-5₍₋₎||NiMn/Ti-1₍₊₎—needs only 1.619 V to deliver 10 mA cm⁻² current density for overall alkaline seawater electrolysis, which is even 0.075 V lower than the noble metal-based electrolyzer (Pt₍₋₎||NiMn/Ti-1₍₊₎).

In this work, 3D nickel-manganese (NiMn) bimetallic coatings have been studied as electrocatalysts for both hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) in alkaline (1.0 M KOH) media and the HER in acidic (0.5 M H₂SO₄) media. The catalysts have been deposited on a titanium substrate (1 × 1 cm²) using low-cost and facile electrochemical deposition method through a dynamic hydrogen bubble template technique. The electrocatalytic performance of these fabricated catalysts was investigated by using Linear Sweep Voltammetry (LSV) for HER and OER at different temperatures ranging from 25 up to 75 °C and also was characterized by scanning electron microscopy (SEM) and inductively coupled plasma optical emission spectroscopy (ICP-OES). It was found that fabricated NiMn/Ti-5 electrocatalyst with Ni²⁺/Mn²⁺ molar ratio of 1:5 exhibits excellent HER activity in alkaline media with overpotential of 127.1 mV to reach current density of 10 mA cm⁻². On the contrary, NiMn/Ti-1 electrocatalyst that fabricated with Ni²⁺/Mn²⁺ molar proportion of 1:1 and lowest Mn-loading of 13.43 µgcm⁻² demonstrates exceptional OER activity with minimum overpotential of 356.3 mV to reach current density of 10 mA cm⁻². The current densities increase ca. 1.8–2.2 times with an increase in temperature from 25 °C to 75 °C for both HER and OER investigation. Both catalysts also have exhibited excellent long-term stability for 10 h at constant potentials as well as constant current density of 10 mA cm⁻² that assure their robustness and higher durability regarding alkaline water splitting.