The study focuses on the influence of Ni and Bi on alkaline ethanol oxidation reaction (EOR) activities, stabilities and structure characteristics of carbon supported Pd-based nanocatalysts (Pd/C, Pd 60 Ni 40 /C, Pd 60 Bi 40 /C, Pd 60 Ni 20 Bi 20 /C) by cyclic voltammetry/chronoamperometry using rotating disk electrode and various physico-chemical methods such as X-ray powder diffraction, X-ray photoelectron spectroscopy, transmission electron microscopy coupled with energy dispersive X-ray spectroscopy and inductively coupled plasma optical emission spectrometry. Nickel generates more adsorbed OH on the Pd catalyst surface than Bi and promotes the oxidation of adsorbed ethanol species. This results in a low onset potential toward ethanol oxidation with high current density. The presence of Bi facilitates high tolerance toward various reaction intermediates resulting from the incomplete ethanol oxidation, but might also initiate the agglomeration of Pd nanoparticles. The novel Pd 60 Ni 20 Bi 20 /C nanocatalyst displays exceptional byproduct tolerance, but only satisfying catalytic activity toward ethanol oxidation in an alkaline medium. Therefore, the EOR performance of the novel carbon supported ternary Pd x Ni y Bi z anode catalyst with various atomic variations (Pd 70 Ni 25 Bi 5 /C, Pd 70 Ni 20 Bi 10 /C, Pd 80 Ni 10 Bi 10 /C and Pd 40 Ni 20 Bi 40 /C) using the common instant reduction synthesis method was further optimized for the alkaline direct ethanol fuel cell. The carbon supported Pd:Ni:Bi nanocatalyst with atomic ratio of 70:20:10 displays outstanding catalytic activity for the alkaline EOR compared to the other Pd x Ni y Bi z /C nanocatalysts as well as to the benchmarks Pd/C, Pd 60 Ni 40 /C and Pd 60 Bi 40 /C. The synergy and the optimal content in consideration of the oxide species of Pd, Ni and Bi are crucial for the EOR kinetic enhancement in alkaline medium.
A series of novel cross-linked highly quaternized chitosan and quaternized poly (vinyl alcohol) membranes were successfully synthesized to be applied in alkaline direct ethanol fuel cells. Cross-linking was accomplished using two different cross-linking agents and an additional thermal process to improve both chemical and thermal properties. Equivalent blends of chitosan and poly (vinyl alcohol) membranes with various degrees of cross-linking were prepared by using different amounts of glutaraldehyde and ethylene glycol diglycidyl ether as cross-linkers. To investigate their applicability in direct ethanol fuel cells, the membranes were characterized in terms of their structural properties, chemical, thermal and alkaline stability, ion transport and ionic properties using following methods: Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy, scanning electron microscopy, thermogravimetric analysis, water uptake by mass change, ethanol permeability in the diffusion cell, back titration method (ion exchange capacity) and electrochemical impedance spectroscopy (anion conductivity). Despite the high degree of quaternization of the applied materials and regardless of the thin film thickness of the blend membranes, the novel cross-linked products displayed outstanding mechanical stability. The lower crosslinked membranes exhibited the best transport and ionic properties with a high anion conductivity of 0.016 S cm-1 and a high ion exchange capacity of 1.75 meq g-1 , whereas membranes with a higher degree of cross-linking performed superior in terms of reduced ethanol permeability of 3.30•10-7 cm 2 s-1 at 60°C. The blend membranes-chemically and thermally cross-linked-provide excellent thermal stability with an onset degradation temperature above 280°C and superb alkaline stability in 1.0 M KOH at 60°C for 650 h. Therefore, these composite membranes exhibit high potential for application as alkaline electrolytes in fuel cells.
Many antioxidants can be electrochemically oxidized using graphite-based electrodes; nevertheless problems arise due to the strong adsorption of redox species at the sensing area. We have demonstrated that boron doped diamond (BDD) electrodes do not show this property, which can be exploited for the design of a new amperometric sensor for the quantification of antioxidants as “total antioxidant capacity” (AOC). As reference substances hydroquinone (HQ) and 6-hydroxy-2,5,7,8-tetramethylchromane-2-carboxylic acid (Trolox) were studied in more detail. The supporting electrolyte was a phosphate buffer solution (PBS, 0.1 mol/L, pH 7.0). The limits of detection (LOD) were 1.5 mg/L and 2.5 mg/L for HQ and Trolox, respectively. The repeatability was 3 % RSD for concentration of 200 mg/L HQ. The method could be applied for the determination of AOC in different berry samples, such as strawberry, blueberry, grape and bramble. A comparison with a standard photometric assay showed good correlation between both methods. The BDD sensor features good reproducibility without fatiguing over at least two months of operation
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