Electrochemical reduction of CO2 to formic acid is a good strategy to address both environmental and energy issues. However, some drawbacks including low activity, selectivity, and stability of electrocatalysts must be overcome. We propose a method for tailoring Bi2O2CO3-coated carbon fiber electrodes with higher selectivity and stability for electrochemical CO2 reduction to formic acid. We evaluated the effect of Bi2O2CO3 and Nafion contents on the electrocatalysts performance for CO2 reduction reaction (CO2RR). All electrodes produced only HCOO− in the liquid phase with a maximum faradaic efficiency (FE) of 69%. The electrocatalysts were stable under 24 h of continuous CO2RR operation. The FE increased with the increasing electrolyte concentration and cation radius size, which indicates that the anion stabilization in solution is critical for adequate formate generation. The CO2RR mechanism was proposed with basis on the literature. The structural carbonate of Bi2O2CO3 acts as an intermediate species in the formate production from CO2.

Electrochemical liquid cell transmission electron microscopy (TEM) is a unique technique for probing nanocatalyst behavior during operation for a range of different electrocatalytic processes, including hydrogen evolution reaction (HER), oxygen evolution reaction (OER), oxygen reduction reaction (ORR), or electrochemical CO2 reduction (eCO2R). A major challenge to the technique's applicability to these systems has to do with the choice of substrate, which requires a wide inert potential range for quantitative electrochemistry, and is also responsible for minimizing background gas generation in the confined microscale environment. Here, we report on the feasibility of electrochemical experiments using the standard redox couple Fe(CN)63−/4− and microchips featuring carbon-coated electrodes. We electrochemically assess the in situ performance with respect to flow rate, liquid volume, and scan rate. Equally important with the choice of working substrate is the choice of the reference electrode. We demonstrate that the use of a modified electrode setup allows for potential measurements relatable to bulk studies. Furthermore, we use this setup to demonstrate the inert potential range for carbon-coated electrodes in aqueous electrolytes for HER, OER, ORR, and eCO2R. This work provides a basis for understanding electrochemical measurements in similar microscale systems and for studying gas-generating reactions with liquid electrochemical TEM.

In this work, a N-doped CsTi2NbO7@g-C3N4 (NTCN) heterojunction nanocomposite was synthesized by a simple one-step calcination method. The as-prepared samples were characterized by means of X-ray diffraction patterns, scanning electron microscopy, high-angle annular dark-field scanning transmission electron microscopy, and Fourier transformed infrared spectroscopy. The results showed that g-C3N4 was formed both on the surface and within the interlayers of CsTi2NbO7, in which CsTi2NbO7 was in situ doped by nitrogen atoms to form N–CsTi2NbO7. The NTCN composite displayed higher electrocatalytic activity toward the detection of nitrite than pure CsTi2NbO7 and g-C3N4. The main reasons could be attributed to the synergistic effects of morphology engineering, N-doping, and layered heterojunction. The NTCN-based electrochemical sensor expressed a good linear relationship range from 0.0999 to 3.15 mmol/L with a detection limit of 2.63 × 10−5 mol/L. The good recovery, stability, and reproducibility of this biosensor showed the potential application in environmental monitoring.

Ni was surface-alloyed with Si by ion implantation. The material was examined for its redox and electrocatalytic behavior in NaOH by cyclic voltammetry. The surface was characterized by x-ray photoelectron spectroscopy, x-ray and electron diffraction, and electron and atomic force microscopy. The ion implantation enhanced activity toward the redox conversion of Ni(OH)2 ↔ NiOOH and the anodic oxidation of glucose reached about 3.5 times and about 2.8 times, respectively. The material is an amorphous mixed oxide of Ni and Si. The effect is discussed considering the true surface area and the generation of active surface sites in relation to the oxygen evolution.

In this paper we describe the synthesis and characterisation of La1-xAxCoO3 (A=Ca, Sr) (0 < x < 0,5) of different morphologies using pulsed laser deposition, ceramic methods and alternative soft-chemistry techniques. Furthermore the potential use of a La1-xCaxCoO3/carbon nanotube composite material for oxygen electrodes is discussed.