scholarly journals Oxygen Reduction Reaction of Carbon Nanotubes Supported Polypyrrole Doped Toluene Sulfonic Acid in Alkaline Medium

2019 ◽  
Vol 7 (4.14) ◽  
pp. 473
Author(s):  
Rika Sri Utami ◽  
Wai Yin Wong ◽  
Edy Herianto Majlan ◽  
Kee Shyuan Loh

In this study, polypyrrole/toluene sulfonic acid-based nitrogen doped carbon nanotube (NCNT) is synthesized via chemical oxidative polymerization followed by high-temperature heat treatment under N2 atmosphere. The structure, morphology and composition of the NCNT catalyst are investigated with X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectroscopy. Different N species including pyridinic, pyrrolic, graphitic, and oxidized-N are quantitatively determined by X-ray photoelectron spectroscopy (XPS). The electrocatalytic activity of NCNT towards oxygen reduction reaction (ORR) in alkaline condition is evaluated with cyclic voltammetry (CV) and rotating disk electrode (RDE). The globular and tubular structure of NCNT can be clearly seen from SEM images. The typical Raman spectrum for NCNT showed two prominent bands around 1348 cm-1 (D band) and 1568 cm-1 (G band). High-resolution XPS spectrum of N 1s for NCNT showed that graphitic-N has the highest percentage (39.36%), whereas the pyridinic-N (26.54%), pyrrolic-N (18.88%) and oxidized-N (15.22%). The ORR electrocatalytic activity of the NCNT in 0.1 M KOH has the onset potential of -0.154 V vs. Ag/AgCl, the current density 0.455 mA/cm2, and electron transfer number of n ≈ 4.  

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3858
Author(s):  
Monica Dan ◽  
Adriana Vulcu ◽  
Sebastian A. Porav ◽  
Cristian Leostean ◽  
Gheorghe Borodi ◽  
...  

Four N-doped graphene materials with a nitrogen content ranging from 8.34 to 13.1 wt.% are prepared by the ball milling method. This method represents an eco-friendly mechanochemical process that can be easily adapted for industrial-scale productivity and allows both the exfoliation of graphite and the synthesis of large quantities of functionalized graphene. These materials are characterized by transmission and scanning electron microscopy, thermogravimetry measurements, X-ray powder diffraction, X-ray photoelectron and Raman spectroscopy, and then, are tested towards the oxygen reduction reaction by cyclic voltammetry and rotating disk electrode methods. Their responses towards ORR are analysed in correlation with their properties and use for the best ORR catalyst identification. However, even though the mechanochemical procedure and the characterization techniques are clean and green methods (i.e., water is the only solvent used for these syntheses and investigations), they are time consuming and, generally, a low number of materials can be prepared, characterized and tested. In order to eliminate some of these limitations, the use of regression learner and reverse engineering methods are proposed for facilitating the optimization of the synthesis conditions and the materials’ design. Thus, the machine learning algorithms are applied to data containing the synthesis parameters, the results obtained from different characterization techniques and the materials response towards ORR to quickly provide predictions that allow the best synthesis conditions or the best electrocatalysts’ identification.


Author(s):  
Chakkrapong Chaiburi ◽  
Bernd Cermenek ◽  
Birgit Elvira Pichler ◽  
Christoph Grimmer ◽  
Viktor Hacker

This paper describes electrocatalysts for the oxygen reduction reaction (ORR) in alkaline direct ethanol fuel cells (ADEFCs), using the non-noble metal electrocatalyst Ag/C, MnO2/C and AgMnO2/C. These electrocatalysts showed tolerance toward ethanol in alkaline media and therefore resistance to ethanol crossover in ADEFCs. Transmission electron microscopy, X-ray spectroscopy (EDX), cyclic voltammetry, and rotating disk electrode (RDE) were employed to determine the morphology, composition, and electrochemical activity of the catalysts. The herein presented results confirm that the AgMnO2/C electrocatalyst significantly outperforms the state-of-the art ORR catalyst platinum.


Catalysts ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 799 ◽  
Author(s):  
Rehan Anwar ◽  
Naseem Iqbal ◽  
Saadia Hanif ◽  
Tayyaba Noor ◽  
Xuan Shi ◽  
...  

Metal-organic frameworks (MOFs) have been at the center stage of material science in the recent past because of their structural properties and wide applications in catalysis. MOFs have also been used as hard templates for the preparation of catalysts. In this study, highly active CuPt/NC electrocatalyst was synthesized by pyrolyzing Cu-tpa MOF along with Pt precursor under flowing Ar-H2 atmosphere. The catalyst was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and X-ray powder diffraction (XRD). Rotating disk electrode study was performed to determine the oxygen reduction reaction (ORR) activity for CuPt/NC in 0.1 M HClO4 at different revolutions per minute (400, 800, 1200, and 1600) and it was also compared with commercial Pt/C catalyst. Further the ORR performance was evaluated by K-L plots and Tafel slope. CuPt/NC shows excellent ORR performance with onset potential of 0.9 V (vs. RHE), which is comparable with commercial Pt/C. The ORR activity of CuPt/NC is demonstrated as an efficient electrocatalyst for fuel cell.


2011 ◽  
Vol 14 (2) ◽  
pp. 81-85 ◽  
Author(s):  
M. A. Garcia-Contreras ◽  
S. M. Fernandez-Valverde ◽  
J. R. Vargas-Garcia

CoNi and PtNi film electrocatalysts were prepared by Metal-Organic Chemical Vapour Deposition (MOCVD) and their electrocatalytic activity for the oxygen reduction reaction (ORR) in 0.5 M KOH was investigated by cyclic voltammetry and Rotating Disk Electrode techniques. Experiments included working electrodes of Co, Ni and Pt prepared also by MOCVD for comparison. The film electrocatalysts were characterized by X-ray diffraction, Scanning Electronic Microscopy and Energy dispersive X-ray analysis. Films thickness was about 200-250 nm and nanocrystallites were found in the range of 12 to 30 nm. In the same experimental conditions, the overpotential for the ORR at a current density of 1 mA cm-2 for PtNi film was 120 mV lower than the overpotential of Pt film electrocatalyst, and an enhanced activity was observed on PtNi with respect to Pt. The electrochemical response for the oxygen reduction reaction on CoNi film was higher than those of elemental Ni and Co films obtained by MOCVD. A good stability was obtained in a chronoamperometry test for the PtNi electrode, only affected by oxygen flow variations.


2018 ◽  
Vol 18 (44) ◽  
pp. 36-40
Author(s):  
Oyunbileg G ◽  
Batnyagt G ◽  
Enkhsaruul B ◽  
T Takeguchi

The oxygen reduction reaction (ORR) is a characteristic reaction which determines the performance of fuel cells which convert a chemical energy into an electrical energy. Aims of this study are to synthesize Au-based nanostars (AuNSs) and determine their preliminary electro-catalytic activities towards ORR by a rotating-disk electrode method in alkaline electrolyte. The images obtained from a scanning electron microscope (SEM) and a transmission electron microscope (TEM) analyses confirm the formation of the star-shaped nanoparticles. Among the investigated nanostar catalysts, an AuNS5 with smaller size and a few branches showed the higher electrocatalytic activity towards ORR than other catalysts with a bigger size. In addition, the electron numbers transferred for all the catalysts are approximately two. The present study results infer that the size of the Au-based nanostars may influence greatly on their catalytic activity. The present study results show that the further improvement is needed for Au-based nanostar catalysts towards the ORR reaction.


Materials ◽  
2021 ◽  
Vol 14 (7) ◽  
pp. 1662
Author(s):  
Antonia Sandoval ◽  
Edgar Borja ◽  
Lorena Magallón ◽  
Javier Su

A simple and rapid synthesis of a CoFeRu-based electrocatalyst by a microwave-assisted method (using water as the microwave absorbing solvent) is reported in this work. Agglomerates with different sizes and shapes are observed by scanning electron microscopy technique. The energy dispersive X-ray spectroscopy shows a low atomic percentage of Co and similar atomic percentage of Fe and Ru. However, the X-ray diffraction exhibits only the presence of metallic Ru and Fe2O3 (hematite) phases. The oxygen reduction without and with 2 mol L−1 methanol is studied using the rotating disk electrode technique. The electrochemical kinetic parameters obtained are compared to a similar electrocatalyst reported in the literature, which was synthesized using a mixture of an organic solvent with DI water as the microwave absorbing solvent. An improvement on the activity of the electrocatalyst synthesized is observed, where high Tafel slopes are not observed. The electrocatalyst also showed tolerance to the presence of methanol during the oxygen reduction reaction.


Author(s):  
Balamurugan Arumugam ◽  
Guru Prasad Kuppuswamy ◽  
S. Yuvaraj

Abstract We report electrocatalytic oxygen reduction reaction (ORR) at silver nanoparticle (AgNPs) electrodes. The AgNPs was obtained in a general one-pot synthesis using 5-amino 2-naphthalene-sulfonic acid (ANS) as a reducing agent in aqueous and room-temperature conditions. The simultaneous formation of AgNPs and an oxidation of ANS were monitored by UV-vis spectroscopy. Surface morphology of AgNPs was characterized by transmission electron microscopy, which revealed that AgNPs appeared as a sphere. The average size of AgNPs was found to be 162 nm. Furthermore, the chemical identity of the nanostructures was established using X-ray photoelectron spectroscopy and X-ray diffraction. The prepared AgNPs showed electrocatalytic activity for reduction of oxygen in neutral pH. Rotating disk electrode voltammetry was used to elucidate kinetics of ORR at AgNPs electrode. These results reveal that oxygen reduction reaction at AgNPs-PANS electrode involved direct four electron pathways.


Author(s):  
Alan Lima ◽  
Alex Lima ◽  
Gabriel Meloni ◽  
Carla Santos ◽  
Mauro Bertotti

In this work, La0.6M0.4Ni0.6Cu0.4O3 (M = Ag, Ba, and Ce, denoted as LANC, LBNC, and LCNC, respectively) electrocatalysts were synthesized by the Pechini method at 1023 K for two hours in air. Rietveld refinement allowed the identification of the crystallographic phases present in all oxides. The electrocatalytic performance of these oxides towards the oxygen reduction reaction (ORR) was examined in alkaline medium by rotating disk electrode (RDE) technique and scanning electrochemical microscopy (SECM) in the redox competition mode. The results indicate that the best performance was found with the LANC electrocatalyst prepared with carbon as a conducting agent (LANC/Carbon), which showed good catalytic activity towards the ORR via a pseudo fourelectron transfer pathway. The enhanced electrocatalytic activity of LANC is probably a result of the presence of a Ag phase, which improves the synergistic effect between the perovskite and carbon added to increase the conductivity, thus leading to a higher ORR performance when compared to other materials.


2020 ◽  
Vol 16 (4) ◽  
pp. 625-638
Author(s):  
Leila Samiee ◽  
Sedigheh Sadegh Hassani

Background: Porous carbon materials are promising candidate supports for various applications. In a number of these applications, doping of the carbon framework with heteroatoms provides a facile route to readily tune the carbon properties. The oxygen reduction reaction (ORR), where the reaction can be catalyzed without precious metals is one of the common applications for the heteroatom-doped carbons. Therefore, heteroatom doped catalysts might have a promising potential as a cathode in Microbial fuel cells (MFCs). MFCs have a good potential to produce electricity from biological oxidization of wastes at the anode and chemical reduction at the cathode. To the best of our knowledge, no studies have been yet reported on utilizing Sulfur trioxide pyridine (STP) and CMK-3 for the preparation of (N and S) doped ordered porous carbon materials. The presence of highly ordered mesostructured and the synergistic effect of N and S atoms with specific structures enhance the oxygen adsorption due to improving the electrocatalytic activity. So the optimal catalyst, with significant stability and excellent tolerance of methanol crossover can be a promising candidate for even other storage and conversion devices. Methods: The physico-chemical properties of the prepared samples were determined by Small Angle X-ray Diffraction (SAXRD), N2 sorption-desorption, Transmission Electron Microscopy (TEM), Field Emission Scanning Electron Microscopy (FESEM) and X-ray Photoelectron Spectroscopy (XPS). The prepared samples were further applied for oxygen reduction reaction (ORR) and the optimal cathode was tested with the Microbial Fuel Cell (MFC) system. Furthermore, according to structural analysis, The HRTEM, and SAXRD results confirmed the formation of well-ordered hexagonal (p6mm) arrays of mesopores in the direction of (100). The EDS and XPS approved that N and S were successfully doped into the CMK-3 carbon framework. Results: Among all the studied CMK-3 based catalysts, the catalyst prepared by STP precursor and pyrolysis at 900°C exhibited the highest ORR activity with the onset potential of 1.02 V vs. RHE and 4 electron transfer number per oxygen molecule in 0.1 M KOH. The high catalyst durability and fuel-crossover tolerance led to stable performance of the optimal cathode after 5000 s operation, while the Pt/C cathode-based was considerably degraded. Finally, the MFC system with the optimal cathode displayed 43.9 mW·m-2 peak power density showing even reasonable performance in comparison to a Pt/C 20 wt.%.cathode. Conclusions: The results revealed that the synergistic effect of nitrogen and sulfur co-doped on the carbon substrate structure leads to improvement in catalytic activity. Also, it was clearly observed that the porous structure and order level of the carbon substrate could considerably change the ORR performance.


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