scholarly journals Electro-Oxidation of Ammonia over Copper Oxide Impregnated γ-Al2O3 Nanocatalysts

Coatings ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 313
Author(s):  
Safia Khan ◽  
Syed Sakhawat Shah ◽  
Mohsin Ali Raza Anjum ◽  
Mohammad Rizwan Khan ◽  
Naveed Kausar Janjua

Ammonia electro-oxidation (AEO) is a zero carbon-emitting sustainable means for the generation of hydrogen fuel, but its commercialization is deterred due to sluggish reaction kinetics and the poisoning of expensive metal electrocatalysts. With this perspective, CuO impregnated γ-Al2O3 (CuO/γ-Al2O3) hybrid materials were synthesized as effective and affordable electrocatalysts and investigated for AEO in alkaline media. Structural investigations were performed via different characterization techniques, i.e., X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and electrochemical impedance spectroscopy (EIS). The morphology of γ-Al2O3 support as interconnected porous structures rendered the CuO/γ-Al2O3 nanocatalysts with robust activity. The additional CuO impregnation resulted in the enhanced electrochemical active surface area (ECSAs) and diffusion coefficient and spiked the electrocatalytic performance for NH3 electrolysis. Owing to good values of diffusion coefficient for AEO, low bandgap, and availability of ample ECSA at higher CuO to γ-Al2O3 ratio, these proposed electrocatalysts were proved to be effective in AEO. Due to good reproducibility, electrochemical stability, and higher activity for ammonia electro-oxidation, CuO/γ-Al2O3 nanomaterials are proposed as efficient promoters, electrode materials, or catalysts in ammonia electrocatalysis.

2010 ◽  
Vol 113-116 ◽  
pp. 1810-1813
Author(s):  
Fang Xiao ◽  
You Long Xu

MnO2 films were electrodeposited on the Ti substrates by galvanostatic method in various plating solutions, which was MnCl2, Mn(NO3)2, MnSO4 and Mn(CH3COO)2 solutions, respectively. On X-ray diffraction test, Crystal structures of all MnO2 films were associated to α-MnO2 of tetragonal crystal system. Scanning electron microscopy results show that morphologies of MnO2 films were clearly different. Among them, MnO2 film prepared in Mn(CH3COO)2 solution presented a lot of cracks and holes. According to electrochemical impedance spectrum analysis, this MnO2 film presents the lowest charge-transfer resistance. Additionally, electrochemical active surface areas of MnO2 films were calculated on the basis of equivalent circuit model for impedance data. The result was found that MnO2 film prepared in Mn(CH3COO)2 solution showed the biggest electrochemical active surface area, which was about 382 cm2. Cyclic voltammograms were carried out for all the samples. MnO2 film formed in Mn(CH3COO)2 solution showed the highest special capacitance of 230 F g-1. The results suggest that Mn(CH3COO)2 solution is suitable for electrodepositing MnO2 film using supercapacitor electrode materials.


2015 ◽  
Vol 228 ◽  
pp. 219-224
Author(s):  
Magdalena Popczyk ◽  
Julian Kubisztal ◽  
Bożena Łosiewicz ◽  
A. Budniok

The Ni+Cr+Si, Ni+Mo+Si and Ni+W+Si composite coatings were obtained by electrodeposition of crystalline nickel from an electrolyte containing suspension of suitable metallic and non-metallic components (Cr, Mo, W and Si). These coatings were obtained galvanostatically at the current density of jdep = -0.100 A cm-2 and at the temperature of 338 K. Chemical composition of the coatings was determined by energy dispersive spectroscopy (EDS). The electrochemical activity of these electrocatalysts was studied in the process of hydrogen evolution reaction (HER) in 5 M KOH solution using steady-state polarization and electrochemical impedance spectroscopy (EIS) methods. The kinetic parameters of the HER on particular electrode materials were determined. It was found that Ni+Mo+Si composite coatings are characterized by enhanced electrochemical activity towards the HER as compared with Ni+W+Si and Ni+Cr+Si coatings due to the presence of Mo and increase in electrochemically active surface area.


Author(s):  
Sabarinathan Ravichandran ◽  
Narayanamoorthy Bhuvanendran ◽  
Kai Peng ◽  
Weiqi Zhang ◽  
Qian Xu ◽  
...  

Abstract The Pt–Fe2O3 nanoparticles embedded over N, P-doped carbon (Pt–Fe2O3/NPC) was successfully synthesized by chemical reduction method demonstrating an enhanced electrocatalytic efficacy in alkaline media toward oxygen reduction reaction (ORR). The surface morphology of Pt–Fe2O3/NPC has been characterized by electron microscopy scanning, X-ray diffraction, electron microscopy transmission, Raman spectra, and X-ray photoelectron spectroscopy. The ORR electrocatalytic activity of Pt–Fe2O3/NPC was found to be the superior mass activity of 0.120 mA µg−1, which are almost twice higher than those for Pt–Fe2O3/VC (0.068 mA µg−1) and Pt/C (0.061 mA µg−1) catalysts. The durability tests revealed that the Pt–Fe2O3/NPC exhibited enhanced stability observed from the order of electrochemical active surface area (ECA) loss determined as Pt–Fe2O3/NPC (45.67%) <Pt–Fe2O3/VC (62.5%) <(Pt/C (72.13%) after 5000 cycles. This present investigation unveiled a facile approach to develop the number of active sites with the combination between P–Fe2O3 and N, P-doped carbon for improved electrocatalytic performance toward ORR.


Coatings ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 257
Author(s):  
Mariam Khan ◽  
Naveed Kausar Janjua ◽  
Safia Khan ◽  
Ibrahim Qazi ◽  
Shafaqat Ali ◽  
...  

An Ag2O(x)−PrO2(y)/γ-Al2O3 electrocatalyst series (X:Y is for Ag:Pr from 0 to 10) was synthesized, to use synthesized samples in electrochemical applications, a step in fuel cells advancements. Ag2O(x)−PrO2(y)/γ-Al2O3/Glassy-Carbon was investigated for electrochemical oxidation of ammonia in alkaline medium and proved to be highly effective, having high potential utility, as compared to commonly used Pt-based electrocatalysts. In this study, gamma alumina as catalytic support was synthesized via precipitation method, and stoichiometric wt/wt.% compositions of Ag2O−PrO2 were loaded on γ-Al2O3 by co-impregnation method. The desired phase of γ-Al2O3 and supported nanocatalysts was obtained after heat treatment at 800 and 600 °C, respectively. The successful loadings of Ag2O−PrO2 nanocatalysts on surface of γ-Al2O3 was determined by X-rays diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), and energy dispersive analysis (EDX). The nano-sized domain of the sample powders sustained with particle sizes was calculated via XRD and scanning electron microscopy (SEM). The surface morphology and elemental compositions were examined by SEM, transmission electron microscopy (TEM) and EDX. The conductive and electron-transferring nature was investigated by cyclic voltammetry and electrochemical impedance (EIS). Cyclic voltammetric profiles were observed, and respective kinetic and thermodynamic parameters were calculated, which showed that these synthesized materials are potential catalysts for ammonia electro-oxidation. Ag2O(6)−PrO2(4)/γ-Al2O3 proved to be the most proficient catalyst among all the members of the series, having greater diffusion coefficient, heterogeneous rate constant and lesser Gibbs free energy for this system. The catalytic activity of these electrocatalysts is revealed from electrochemical studies which reflected their potentiality as electrode material in direct ammonia fuel cell technology for energy production.


2019 ◽  
Vol 10 ◽  
pp. 62-70 ◽  
Author(s):  
Yong Li ◽  
Peng Yang ◽  
Bin Wang ◽  
Zhongqing Liu

Bimetallic phosphides have been attracting increasing attention due to their synergistic effect for improving the hydrogen evolution reaction as compared to monometallic phosphides. In this work, NiCoP modified hybrid electrodes were fabricated by a one-step electrodeposition process with TiO2 nanotube arrays (TNAs) as a carrier. X-ray diffraction, transmission electron microscopy, UV–vis diffuse reflection spectroscopy, X-ray photoelectron spectroscopy and scanning transmission electron microscopy/energy-dispersive X-ray spectroscopy were used to characterize the physiochemical properties of the samples. The electrochemical performance was investigated by cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy. We show that after incorporating Co into Ni–P, the resulting Ni x Co y P/TNAs present enhanced electrocatalytic activity due to the improved electron transfer and increased electrochemically active surface area (ECSA). In 0.5 mol L−1 H2SO4 electrolyte, the Ni x Co y P/TNAs (x = 3.84, y = 0.78) demonstrated an ECSA value of 52.1 mF cm−2, which is 3.8 times that of Ni–P/TNAs (13.7 mF cm−2). In a two-electrode system with a Pt sheet as the anode, the Ni x Co y P/TNAs presented a bath voltage of 1.92 V at 100 mA cm−2, which is an improvment of 79% over that of 1.07 V at 10 mA cm−2.


2019 ◽  
Vol 25 (6) ◽  
pp. 1394-1400 ◽  
Author(s):  
Sumit Majumder ◽  
Sangam Banerjee

AbstractHere, a well crystalline 3D flower-like structured MoS2 (~420 nm) has been successfully synthesized on a large scale by a simple hydrothermal technique. The evolution of morphology in the formation process has also been investigated. The crystallinity, purity, and morphology of the sample are characterized by powder X-ray diffraction, Fourier-transform infrared spectroscopy, fieldemission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM) techniques. The FESEM and TEM images reveal that the sample exhibits a uniform 3D flower-like microsphere shape with folded nanosheets, which are stretched out along the edge of the microsphere. The electrochemical performance of the sample has been investigated by cyclic voltammogram, galvanostatic charge–discharge, and electrochemical impedance spectroscopy studies. The results of the electrochemical analysis suggest that the material delivers a maximum specific capacitance (Csp) of 350 F/g at a discharge current density of 0.25 A/g with energy density 17.5 Wh/kg. It also exhibits good capability and excellent cyclic stability (94% capacity retention after 1,000 cycles in 1 A/g) owing to the coupling effect of electrical conductivity with the interesting morphology and larger active surface area. Hence, the sample may be used as a promising electrode material for high-performance energy storage devices.


2011 ◽  
Vol 399-401 ◽  
pp. 1926-1931 ◽  
Author(s):  
Yi Wang ◽  
Gang Chen ◽  
Wei Dong Liu ◽  
Qiong Yu Zhou ◽  
Qing Dong Zhong

Fe + Si coatings were prepared by iron deposition from a bath containing a suspension of silicon powders. These coatings were obtained at galvanostatic conditions, at the current density of jdep=−0.020 A cm−2 and at the temperature of 338 K. For determination of the influence of phase composition and surface morphology of these coatings on changes in the corrosion resistance, these coatings were modified in an argon atmosphere by thermal treatment at 873 K for 2h. A scanning electron microscope was used for surface morphology characterization of the coatings. The chemical composition of the coatings was determined by EDS and phase composition investigations were conducted by X-ray diffraction. It was found that the as-deposited coatings consist of a two-phase structure, i.e., iron and silicon. The phase composition for the Fe + Si coatings after thermal treatment is markedly different. The main peaks corresponding to Fe and Si coexist with the new phases: FeSi. Electrochemical corrosion resistance investigations were carried out in 3.5wt% NaCl, using potentiodynamic and electrochemical impedance spectroscopy (EIS) methods. On the basis of these investigations it was found that the Fe + Si coatings after thermal treatment are more corrosion resistant in 3.5wt% NaCl solution than the as-deposited coatings. The reasons for this are a reduction in the amount of free iron and silicon, the presence of new phases (in particular silicides), and a decrease of the active surface area of the coatings after thermal treatment.


2020 ◽  
Vol 20 (8) ◽  
pp. 4854-4859 ◽  
Author(s):  
Lei Chen ◽  
Xu Chen ◽  
Yaqiong Wen ◽  
Bixia Wang ◽  
Yangchen Wu ◽  
...  

Nitrogen-enriched reduced graphene oxide electrode material can be successfully prepared through a simple hydrothermal method. The morphology and microstructure of ready to use electrode material is measured by field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD). Physical characterizations revealed that nitrogen-enriched reduced graphene oxide electrode material possessed high specific surface area of 429.6 m2 · g−1, resulting in high utilization of electrode materials with electrolyte. Electrochemical performance of nitrogen-enriched reduced graphene oxide electrode was also investigated by cyclic voltammetry (CV), galvanostatic charge/discharge measurements and electrochemical impedance spectroscopy (EIS) in aqueous in 6 M KOH with a three-electrode system, which displayed a high specific capacitance about 223.5 F · g−1 at 1 mV · s−1. More importantly, nitrogenenriched reduced graphene oxide electrode exhibited outstanding stability with 100% coulombic efficiency and with no specific capacitance loss under 2 A · g−1 after 10000 cycles. The supercapacitive behaviors indicated that nitrogen-enriched reduced graphene oxide can be a used as a promising electrode for high-performance super-capacitors.


Crystals ◽  
2021 ◽  
Vol 12 (1) ◽  
pp. 14
Author(s):  
Sajid Ali Ansari ◽  
Nazish Parveen ◽  
Mohd Al Saleh Al-Othoum ◽  
Mohammad Omaish Ansari

The design and development of electrode materials for energy-storage applications is an area of prime focus around the globe because of the shortage of natural resources. In this study, we developed a method for preparing a novel three-dimensional binder-free pseudocapacitive NiZn2O4 active material, which was grown directly over nickel foam (NiZn2O4@3D-NF), using a simple one-step hydrothermal process. The material was characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Cyclic voltammetry, galvanostatic charge–discharge, and electrochemical impedance spectroscopy techniques were employed to evaluate the pseudocapacitive performance of the NiZn2O4 active material in a three-electrode assembly cell. The prepared NiZn2O4@3D-NF electrode exhibited an excellent specific capacitance, of 1706.25 F/g, compared to that of the NiO@3D-NF (1050 F/g) electrode because it has the bimetallic characteristics of both zinc and nickel. The NiZn2O4@3D-NF electrode showed better cyclic stability (87.5% retention) compared to the NiO@3D-NF electrode (80% retention) after 5000 cycles at a fixed current density, which also supports the durability of the NiZn2O4@3D-NF electrode. The characteristics of NiZn2O4@3D-NF include corrosion resistance, high conductivity, an abundance of active sites for electrochemical reaction, a high surface area, and synergism between the bimetallic oxides, which make it a suitable candidate for potential application in the field of energy storage.


Author(s):  
Nicholas Schwartz ◽  
Jason Harrington ◽  
Kirk J Ziegler ◽  
Philip Cox

Abstract The direct electrochemically driven separation of CO2 from a humidified N2, O2, and CO2 gas mixture was conducted using an asymmetric membrane electrode assembly (MEA). The MEA was fabricated using a screen-printed ionomer bound Pt cathode, an anion exchange membrane (AEM), and ionomer bound IrO2 anode. Electrocatalyst materials were physically and chemically characterized prior to inclusion within the electrode. Electrochemical impedance spectroscopy (EIS) and linear sweep voltammetry (LSV) measurements using a rotating disk electrode (RDE) were used to quantify the catalytic activity and determine the effects of the catalyst-to-ionomer ratio. Catalysts were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer–Emmett–Teller (BET) surface analysis, and (dynamic light scattering) DLS to evaluate catalyst structure, active surface area, and determine the particle size and bulk particle size distribution (PSD). The electrocatalyst layer of the electrodes were fabricated by screen printing a uniformly dispersed mixture of catalyst, dissolved anionic ionomer, and a solvent system onto an electrode supporting gas diffusion layer (GDL). Pt IrO2 MEAs were fabricated and current-voltage relationships were determined using constant-current measurements over a range of applied current densities and flow rates. Baseline reaction kinetics for CO2 separation were established with a standard set of Pt-IrO2 MEAs.


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