Preparation of Ta2O5 nanoparticles by using cathode glow discharge electrolysis

Tantalum pentoxide nanoparticles (Ta2O5 NPs) were fabricated by cathode glow discharge electrolysis (CGDE) generated between a needle-like platinum wire cathode and a tantalum foil anode in 6 g L−1 Na2SO4 electrolyte solution containing 5 mL hydrofluoric acid (HF) and 0.075 g cetyltrimethyl ammonium bromide (CTAB). The chemical structure, composition and morphology of the obtained powder were analyzed by using XRD, FT-IR, SEM/EDS, XPS and UV-vis DRS. The results found that Ta2O5 NPs with orthorhombic structure and wide band gap (3.6 eV) are successfully fabricated at 500 V discharge voltage in about 3 h. CTAB as a stabilizing agent can reduce the agglomeration due to forming CTA+ and attaching the surface of the synthetic products. A possible preparation mechanism of Ta2O5 NPs is proposed. Firstly, the tantalum foil anode is oxidized to form a compact Ta2O5 layer. Then, Ta2O5 surface is etched to form soluble [TaF7]2− complexes in the presence of HF. After that, soluble [TaF7]2− complexes can react with H2O to form Ta(OH)5. Finally, Ta(OH)5 is further converted to Ta2O5 from plasma-liquid interface into solution.

Structural Evolution of Pt, Au, and Cu Anodes by Electrolysis up to Contact Glow Discharge Electrolysis in Alkaline Electrolytes

<div>Applying a voltage to metal electrodes in contact with aqueous electrolytes results in the electrolysis of water at low voltages and plasma formation in the electrolyte at high voltages referred to as contact glow discharge electrolysis (CGDE). While several studies explore parameters that lead to changes in the I-U characteristics in this voltage range, little is known about the evolution of the structural properties of the electrodes. Here we study this aspect on materials essential to electrocatalysis, namely Pt, Au, and Cu. The stationary I-U characteristics are almost identical for all electrodes. Detailed structural characterization by optical microscopy, scanning electron microscopy, and electrochemical approaches reveal that Pt is stable during electrolysis and CGDE, while Au and Cu exhibit a voltage-dependent oxide formation. More importantly, oxides are reduced when the Au and Cu electrodes are kept in the electrolysis solution. We suspect that H₂O₂(formed during electrolysis) is responsible for the oxide reduction. The reduced oxides (which are also accessible <i>via</i> electrochemical reduction) form a porous film, representing a possible new class of materials in energy storage and conversion studies.</div>

Structural Evolution of Pt, Au, and Cu Anodes by Electrolysis up to Contact Glow Discharge Electrolysis in Alkaline Electrolytes

<div>Applying a voltage to metal electrodes in contact with aqueous electrolytes results in the electrolysis of water at low voltages and plasma formation in the electrolyte at high voltages referred to as contact glow discharge electrolysis (CGDE). While several studies explore parameters that lead to changes in the I-U characteristics in this voltage range, little is known about the evolution of the structural properties of the electrodes. Here we study this aspect on materials essential to electrocatalysis, namely Pt, Au, and Cu. The stationary I-U characteristics are almost identical for all electrodes. Detailed structural characterization by optical microscopy, scanning electron microscopy, and electrochemical approaches reveal that Pt is stable during electrolysis and CGDE, while Au and Cu exhibit a voltage-dependent oxide formation. More importantly, oxides are reduced when the Au and Cu electrodes are kept in the electrolysis solution. We suspect that H₂O₂(formed during electrolysis) is responsible for the oxide reduction. The reduced oxides (which are also accessible <i>via</i> electrochemical reduction) form a porous film, representing a possible new class of materials in energy storage and conversion studies.</div>

Contact Glow Discharge Electrolysis: Effect of Electrolyte Conductivity on Discharge Voltage

Contact glow discharge electrolysis (CGDE) can be exploited in environmental chemistry for the degradation of pollutants in wastewater. This study focuses on the employment of cheap materials (e.g., steel and tungsten) as electrodes for experiments of CGDE conducted in electrochemical cells with variable electrolytic composition. A clear correlation between breakdown voltage (VB)/discharge (or midpoint) voltage (VD) and the conductivity of the electrolyte is shown. Regardless of the chemical nature of the ionogenic species (acid, base or salt), the higher the conductivity of the solution, the lower the applied potential required for the onset of the glow discharge. Concerning practical application, these salts could be added to poorly conductive wastewaters to increase their conductivity and thus reduce the ignition potential necessary for the development of the CGDE. Such an effect could render the process of chemical waste disposal from wastewaters more economical. Moreover, it is evidenced that both VB and VD are practically independent on the ratio anode area to cathode area if highly conductive solutions are employed.