In this study, we investigate the effect of K 2 feo 4 , as a new and soluble fe salt at alkaline conditions, on oxygen-evolution reaction (oeR) of ni oxide. Both oxidation and reduction peaks for ni in the presence and absence of fe are linearly changed by (scan rate) 1/2. immediately after the interaction of [feo 4 ] 2with the surface of the electrode, a significant increase in OER is observed. This could be indicative of the fact that either the [feo 4 ] 2on the surface of ni oxide is directly involved in oeR, or, it is important to activate Ni oxide toward OER. Due to the change in the Ni(II)/(III) peak, it is hypothesized that Fe impurity in KOH or electrochemical cell has different effects at the potential range. At low potential, [FeO 4 ] 2− is reduced on the surface of the electrode, and thus, is significantly adsorbed on the electrode. Finally, oxygenevolution measurements of K 2 feo 4 and ni 2 o 3 are investigated under chemical conditions. K 2 feo 4 is not stable in the presence of Ni(II) oxide, and OER is observed in a KOH solution (pH ≈ 13).
Polypyrrole (PPy) and Polypyrrole-ZnO (PPy-ZnO) nanocomposites were electrodeposited on mild steel and its corrosion protection ability was studied by Tafel and Impedance techniques in 3.5% NaCl solution. Pure Polypyrrole film was not found to protect the mild steel perfectly but the coating with nano-sized ZnO (PPyZnO) has dramatically increased the corrosion resistance of mild steel. Electrochemical Impedance Spectroscopy (EIS) measurements indicated that the coating resistance (R coat ) and corrosion resistance (R corr ) values for the PPyZnO nanocomposite coating was much higher than that of pure PPy coated electrode.
The design of molecular oxygen-evolution reaction (OER) catalysts requires fundamental mechanistic studies on their widely unknown mechanisms of action. To this end, copper complexes keep attracting interest as good catalysts for the OER, and metal complexes with TMC (TMC = 1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane) stand out as active OER catalysts. A mononuclear copper complex, [Cu(TMC)(H2O)](NO3)2 (TMC = 1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane), combined both key features and was previously reported to be one of the most active copper-complex-based catalysts for electrocatalytic OER in neutral aqueous solutions. However, the functionalities and mechanisms of the catalyst are still not fully understood and need to be clarified with advanced analytical studies to enable further informed molecular catalyst design on a larger scale. Herein, the role of nanosized Cu oxide particles, ions, or clusters in the electrochemical OER with a mononuclear copper(II) complex with TMC was investigated by operando methods, including in situ vis-spectroelectrochemistry, in situ electrochemical liquid transmission electron microscopy (EC-LTEM), and extended X-ray absorption fine structure (EXAFS) analysis. These combined experiments showed that Cu oxide-based nanoparticles, rather than a molecular structure, are formed at a significantly lower potential than required for OER and are candidates for being the true OER catalysts. Our results indicate that for the OER in the presence of a homogeneous metal complex-based (pre)catalyst, careful analyses and new in situ protocols for ruling out the participation of metal oxides or clusters are critical for catalyst development. This approach could be a roadmap for progress in the field of sustainable catalysis via informed molecular catalyst design. Our combined approach of in situ TEM monitoring and a wide range of complementary spectroscopic techniques will open up new perspectives to track the transformation pathways and true active species for a wide range of molecular catalysts.
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