Galvanic Displacement Reaction Research Articles

Development of inexpensive, simple and environment-friendly solar selective absorber using copper nanoparticle

Abstract Concentrating solar power is the most challenging and expensive yet highly efficient source of thermal energy from solar power. This is mainly due to the intermittency of the sun rays and expensive materials used to harness its energy. One of the main components adding to the cost is the solar selective absorber materials which are simply put spectrally selective coatings on a receiver system to capture maximum heat from the sun. These materials add to a large extent to the efficiency of converting the sun’s energy to thermal energy and in turn electricity. An ideal solar selective absorber possesses the property of absorbing maximum radiations in the solar spectrum and emit minimum in the thermal energy spectrum. In the current study, an inexpensive, simple and environment-friendly solar selective absorber is fabricated by a galvanic displacement reaction of copper nanoparticles on galvanised metal substrates. These copper nanoparticles have high absorptivity (0.8–0.9) by virtue of plasmon resonance property. The emissivity is low due to the highly reflective metal substrate. By varying size of the copper nanoparticles from 100 nm to 2 μm emissivity and absorptivity can be varied. However, achieving low emissivity and high absorptivity requires some optimising. The size depends on the concentration of precursor solution and immersion time of substrate. One of the remedies for controlling the deposition rate to tune the nanoparticle size and microstructure of deposited copper nanoparticle is by addition of a deposition inhibitor (e.g. Polyethylene glycol).

Bismuth coated graphite felt modified by silver particles for selective electroreduction of CO2 into formate in a flow cell

A 3D porous Ag-Bi electrode was developed to achieve the highly selective reduction of CO2 into formate. Ag particles were deposited on Bi coated graphite felt by galvanic displacement reaction. The selectivity of the reduction was enhanced with the Ag-Bi electrode compared with Bi coated graphite felt. The bimetallic catalytic system converted CO2 into formate with a high selectivity of 88% at -1.6 VSCE. The highly porous structure and large surface area of the electrode facilitated the mass transport, leading to a high surface current density of 76 mA cm−2 and a production rate of 8.1 ± 0.4 mmol cm−3 h−1 (62 ± 3 mg cm−2 h−1). These results are very promising in the context of the electrochemical conversion of CO2.

Gold nanoparticles plated porous silicon nanopowder for nonenzymatic voltammetric detection of hydrogen peroxide

A voltammetric approach was developed for the selective and sensitive determination of hydrogen peroxide using Au plated porous silicon (PSi) nanopowder modified glassy carbon electrode (GCE). The AuNPs-PSi hybrid structure was synthesized via stain etching procedure followed by an immersion plating method to deposit AuNPs onto PSi via a simple galvanic displacement reaction with no external reducing agent to convert Au3+ to Au0. The as-fabricated AuNPs-PSi catalyst was successfully characterized by XRD, Raman, FTIR, XPS, SEM, TEM and EDS techniques. Well crystalline nature of the as-fabricated hybrid structure with AuNPs size ranging from 5 to 40 nm was observed. The specific surface area and total pore volume for both PSi and AuNPs plated PSi were evaluated using N2 adsorption isotherm technique. Cyclic voltammetry and electrochemical impedance spectroscopy techniques were applied to investigate the catalytic efficiency of AuNPs-PSi modified electrode compared to pure PSi/GCE and unmodified GCE. The sensing performance of the active material modified GCE was thoroughly examined with linear sweep voltammetry (LSV) and square wave voltammetry (SWV) techniques. The AuNPs-PSi/GCE exhibited a remarkable linear dynamic range between 2.0 and 13.81 mM (for LSV) and 0.5–6.91 mM for (SWV) with high sensitivity and low detection limit of 10.65 μAmM−1cm−2 and 14.84 μM for LSV, whereas 10.41 μAmM−1cm−2 and 15.16 μM using SWV techniques, respectively. The fabricated sensor electrode showed excellent anti-interfering ability in the presence of several common biomolecules as well as demonstrated good operational stability and reproducibility with low relative standard deviation. Moreover, the modified electrode showed acceptable recovery of H2O2 in a real sample analysis. Thus, the developed AuNPs-PSi hybrid nanomaterial represents an excellent electrocatalyst for the efficient detection and quantification of H2O2 by the electrochemical approach.

Consequence of Galvanic Displacement Reaction on Digital Photocorrosion of GaAs/Al0.35Ga0.65As Nanoheterostructures

GaAs/AlGaAs semiconductor nanoheterostructures have found attractive application in the field of biosensing based on the effect of digital photocorrosion (DIP). The sensitivity of semiconductor–nanoheterostructure-based biosensors depends on the precision of controlling the process of DIP, which is highly sensitive to the surface presence of electrically charged biomolecules. To explore further this process, we have investigated the role of a galvanic displacement (GD) reaction on DIP of GaAs/Al0.35Ga0.65As (001) nanoheterostructures. Deposition of ionic gold on the GaAs surface induces spontaneous electron transfer between the semiconductor and ionic gold, which affects the photocorrosion of GaAs/AlGaAs layers observed simultaneously with the photoluminescence effect. The immediate consequence of the electron transfer from GaAs toward Au3+ is a significantly increased rate of DIP. At the same time, the formation of neutralized gold nanoparticles and Au–Ga alloy takes place on the surface of photocorroding nanoheterostructures. In the presence of 2.8% solution of ammonia and 0.1 mM gold chloride, a significantly reduced rate of deposition of gold nanoparticles is observed. This allows achieving layer-by-layer removal of the investigated material, which is sensitive to perturbations induced by surface immobilized electrically charged molecules. We have elaborated various factors stimulating photocorrosion of the GaAs/Al0.35Ga0.65As nanoheterostructures and we demonstrate the biosensing potential of an innovative GD-based DIP sensor.

Deposition of FeOOH layers onto porous PbO2 by galvanic displacement and their use as electrocatalysts for oxygen evolution reaction

Abstract The galvanic displacement reaction between sacrificial PbO2 layers and Fe(II) ions has been carried out in mildly acid acetate solutions. The effect of experimental variables, like morphology of the PbO2 layers, solution pH, temperature and concentration of Fe(II) ions, has been investigated by combining electrochemical methods, SEM-EDS, XRD and XPS. The reaction between PbO2 and Fe(II) ions produced secondary dual layers, consisting of an inner amorphous FeOOH film and an outer crystalline γ-FeOOH deposit, respectively. This peculiar behavior was in contrast with analogous reactions involving other transition metal ions, which yielded only continuous amorphous secondary oxide layers. PbO2/FeOOH layers were tested as anodes for the oxygen evolution reaction in basic media.

Surface-Enhanced Raman Scattering Spectra of Non-Fluorescent 4-Mercaptobenzoic Acid and Human Red Blood Cells on Carnation-Shaped Silver Meso-Flowers Monolayer

The development of new surface-enhanced Raman scattering (SERS) substrates is primarily motivated by designing synthetic substrates to obtain the significant signal enhancement. In this paper, a large-scale carnation-shaped Ag meso-flowers monolayer with sufficient “hot spots” has been synthesized on copper foil without using any capping agent. In dimethyl sulfoxide, AgNO3 is reduced by Cu for 60 min at 35 °C through the galvanic displacement reaction, and carnation-shaped Ag meso-flowers with good crystallinity and high purity are obtained. The as-fabricated carnation-shaped Ag meso-flowers monolayer is used as novel SERS substrates. Non-fluorescent 4-mercaptobenzoic acid is selected as the probe molecule to test the SERS activity, uniformity and enhancement factors (EF) of the monolayer. Experimental results show that the EF of the carnation-shaped Ag meso-flowers monolayer is up to 7.06×108 and the limit of detection is 10-11 M. Meanwhile, the biocompatibility of the carnation-shaped silver meso-flowers monolayer is tested for red blood cells detection. SERS measurements demonstrate that the carnation-shaped silver meso-flowers monolayer has good activity, uniformity and biocompatibility, and can be used as an outstanding SERS substrate, which has a broad application prospect in numerous chemical and biochemical sensing applications.

One-Step Rapid Synthesis of Al-Based Ag Dendrites for Highly Active and Cost Effective SERS Plasmonic Substrates

Highly active Al-based Ag dendrites SERS plasmonic substrates have been rapidly synthesized by the one-step galvanic displacement reaction without the use of any surfactants and templates. The as-prepared SERS substrates were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman spectroscopy. XRD measurements confirmed the metallic nature of the formed Ag dendrites. None of the organic additives were used in the synthesis process, which ensures the substrates surfaces are completely clean and avoiding the introduction of organic contaminants. The innovative rough bionic substrates yield a final silver dendritic structure that offers large specific surface area and high-density hotspots. Using malachite green as a model target, the Al-based Ag dendrites SERS substrates exhibited acceptable reproducibility (relative standard deviation of 23.8%) and high enhancement capacities (pushed the detection limit down to 10 pM). Importantly, these Ag dendrites could potentially be employed as highly active and cost effective flexible SERS sensors for label-free ultrasensitive detection of biomolecules.

PVP‐mediated galvanic replacement growth of AgNPs on copper foil for SERS sensing

Herein, the authors present a simple and cost-effective silver nanoparticles (AgNPs)-based surface-enhanced Raman scattering (SERS) sensor based on galvanic displacement reaction using AgNO3 and copper foil as precursors. With the mediation of polyvinyl pyrrolidone (PVP), AgNPs grow in-situ on the surface of copper foil at room temperature. AgNPs-based SERS sensor was prepared with optimised AgNO3 concentration of 50 mM, the mass ratio of AgNO3 to PVP of 2:1 and characterised using scanning electron microscopy and X-ray diffraction. As-fabricated SERS sensor exhibited a high Raman signal enhancement factor of 3.5 × 105 in the detection of Rhodamine 6G (R6G). Furthermore, a decent linear relationship for methyl parathion sensing was obtained in the range from 1 × 10−6 to 1 × 10−4 M, with an actual detection limit of 1 × 10−6 M. Recoveries of methyl parathion-spiked lake water samples ranging from 93.64 to 106.16% were obtained, suggesting the feasibility of the SERS sensor. These features demonstrated that the AgNPs-based SERS sensor can potentially be used in sensing a trace amount of chemicals in surface water for environmental protection.

Pt deposition on Ni-based superalloy via a combination of galvanic displacement reaction and chemical reduction

We demonstrate the deposition of Pt film on a nickel-based superalloy (CMSX-4) via a combination of galvanic displacement reaction and chemical reduction. The aqueous plating bath contains an optimized mixture of Pt precursor (H2PtCl6), pH adjuster (NaOH), and reducing agent (HCHO). Both time-evolved UV–Vis and X-ray absorption spectra on the plating bath indicate a sequential chemical reduction of Pt4+ → Pt2+ → Pt. In addition, a parasitic galvanic displacement reaction occurs in which Ni, Al, and Co from the CMSX-4 suffer from corrosive dissolution whereas the Pt4+ ions from the plating bath are reduced directly. This surface-mediated galvanic displacement reaction produces numerous Pt nanoparticles serving as the nucleation sites for chemical reduction of Pt4+ from HCHO. Therefore, typical sensitization and activation steps for electroless plating are not necessary in our plating bath. From X-ray diffraction pattern, the Pt film adopts a fcc polycrystalline structure. Images from scanning electron microscope confirm the formation of a dense and continuous Pt film with 1 μm thickness.

Synthesis dynamics of silver nanowires galvanically displaced by platinum salts: a fabrication route for oxygen reduction electrocatalysts and metal electrodeposition electrodes

The advancement of conductive and flexible thin films is relevant to an assortment of energy applications ranging from organic photovoltaics, fuel cells, lithium ion batteries, and dynamic windows. Here, we develop an inexpensive, fast, and adjustable method to yield nanowire arrays on flexible polyethylene terephthalate substrates for the alkaline oxygen reduction reaction and for reversible metal electrodeposition. Ag nanowires serve as a non-sacrificial template for Pt deposition and allow for the synthesis of bimetallic Pt/Ag nanowires. When not properly controlled, the galvanic displacement reaction occurring at the solid–liquid interface between Ag nanowires and aqueous Pt ions results in nonuniform nucleation and growth profiles, which creates micron-sized gaps in the nanowire arrays. These gaps, which result in poorly conducting thin films, increase in prevalence when immersion length and Pt concentration are increased. Multiple cycles of 10-min immersions in 10 mM K2PtCl4 yield bimetallic Pt/Ag nanowires that maintain the high aspect ratios and conductivities of the initial Ag nanowires, while the added Pt improves electrocatalytic performance and electrochemical durability.

Facile Synthesis of Co3O4@CoO@Co Gradient Core@Shell Nanoparticles and Their Applications for Oxygen Evolution and Reduction in Alkaline Electrolytes.

We demonstrate a facile fabrication scheme for Co3O4@CoO@Co (gradient core@shell) nanoparticles on graphene and explore their electrocatalytic potentials for an oxygen evolution reaction (OER) and an oxygen reduction reaction (ORR) in alkaline electrolytes. The synthetic approach begins with the preparation of Co3O4 nanoparticles via a hydrothermal process, which is followed by a controlled hydrogen reduction treatment to render nanoparticles with radial constituents of Co3O4/CoO/Co (inside/outside). X-ray diffraction patterns confirm the formation of crystalline Co3O4 nanoparticles, and their gradual transformation to cubic CoO and fcc Co on the surface. Images from transmission electron microscope reveal a core@shell microstructure. These Co3O4@CoO@Co nanoparticles show impressive activities and durability for OER. For ORR electrocatalysis, the Co3O4@CoO@Co nanoparticles are subjected to a galvanic displacement reaction in which the surface Co atoms undergo oxidative dissolution for the reduction of Pt ions from the electrolyte to form Co3O4@Pt nanoparticles. With commercial Pt/C as a benchmark, we determine the ORR activities in sequence of Pt/C > Co3O4@Pt > Co3O4. Measurements from a rotation disk electrode at various rotation speeds indicate a 4-electron transfer path for Co3O4@Pt. In addition, the specific activity of Co3O4@Pt is more than two times greater than that of Pt/C.

Hematite/M (M = Au, Pd) Catalysts Derived from a Double-Hollow Prussian Blue Microstructure: Simultaneous Catalytic Reduction of o- and p-Nitrophenols.

Present study deals with hematite/M (M = Au, Pd) catalysts converted from a double-hollow Prussian blue microstructure (DHPM). The unique Prussian blue (PB) microstructure (MS) is prepared by a template-free solvothermal synthetic route in a single-step reaction. An amine-functionalized silicate sol-gel matrix (SSG) has served as the structure-directing agent cum stabilizer for making DHPM. Synthesized DHPM is having a unique structure: a hollow core and an in situ etched porous surface. Growth mechanism is explored and revealed by analyzing several experimental parameters such as HCl concentration, Fe source, effect of the added EtOH, silane concentration, and role of silanes' amine groups. It is identified that the superstructure consisted of well-aligned PB cubes growing radially from the core of the superstructure. Metal (Au and Pd) nanoparticles (NPs) are deposited on both interior and exterior of the PB MS through galvanic displacement reaction, and thus metal NP-loaded hematite phase iron oxide (α-Fe2O3) nanomaterials were derived by annealing them in air. Catalytic activities of the hematite/M(M = Au, Pd) MS are investigated toward simultaneous catalytic reduction of o-nitrophenol and p-nitrophenol. The resultant hematite/Pd MS showed high structural stability and catalytic active sites than the hematite/Au MS, which enhances the catalytic properties for the simultaneous catalytic reduction of both nitrophenols.

Investigation on the oxide-oxide galvanic displacement reactions employed in the preparation of electrocatalytic layers

Galvanic displacement reactions between sacrificial oxide layers and metal cations, leading to the formation of secondary oxide layers, have been studied with the aim of collecting new experimental evidence on their mechanism. The study has been carried out by combining electrochemical methods, SEM-EDS and XPS depth profiling. Both porous and compact PbO2 layers have been used as sacrificial oxides and reacted, in different experiments, with: (i) a single low-valent cation, (ii) two cations in sequential exchange reactions or (iii) two cations simultaneously. The experimental results converged to show (i) a lack of correlation between the reaction driving force and the secondary oxide growth rate, (ii) the incorporation of cations from solution at the secondary oxide/electrolyte interface, (iii) the transport of Pb species through the growing secondary oxide layer and (iv) a major effect of mass transport on the growth rate.

Formation Mechanism and Gram-Scale Production of PtNi Hollow Nanoparticles for Oxygen Electrocatalysis through In Situ Galvanic Displacement Reaction.

Galvanic displacement reaction has been considered a simple method for fabricating hollow nanoparticles. However, the formation of hollow interiors in nanoparticles is not easily achieved owing to the easy oxidization of transition metals, which results in mixed morphologies, and the presence of surfactants on the nanoparticle surface, which severely deteriorates the catalytic activity. In this study, we developed a facile gram-scale methodology for the one-pot preparation of carbon-supported PtNi hollow nanoparticles as an efficient and durable oxygen reduction electrocatalyst without using stabilizing agents or additional processes. The hollow structures were evolved from sacrificial Ni nanoparticles via an in situ galvanic displacement reaction with a Pt precursor, directly following a preannealing process. By sampling the PtNi/C hollow nanoparticles at various reaction times, the structural formation mechanism was investigated using transmission electron microscopy with energy-dispersive X-ray spectroscopy mapping/line-scan profiling. We found out that the structure and morphology of the PtNi hollow nanoparticles were controlled by the acidity of the metal precursor solution and the nanoparticle core size. The synthesized PtNi hollow nanoparticles acted as an oxygen reduction electrocatalyst, with a catalytic activity superior to that of a commercial Pt catalyst. Even after 10 000 cycles of harsh accelerated durability testing, the PtNi/C hollow electrocatalyst showed high performance and durability. We concluded that the Pt-rich layers on the PtNi hollow nanoparticles improved the catalytic activity and durability considerably.

Effect of an Organic Additive, N-Dimethyldithiocarbamic acid Ester Sodium salt, on Properties of Bismuth Telluride thin Films Fabricated by Galvanic Displacement Reaction of Electroplated Cobalt thin Films

Effect of an Organic Additive, N-Dimethyldithiocarbamic acid Ester Sodium salt, on Properties of Bismuth Telluride thin Films Fabricated by Galvanic Displacement Reaction of Electroplated Cobalt thin Films

Fabrication of fully covered Cu–Ag core–shell nanoparticles by compound method and anti-oxidation performance

Cu–Ag core–shell nanoparticles with a size of 8 nm were synthesized by the compound method of replacement reaction and chemical reduction reaction. A fully covered Cu–Ag core–shell structure was obtained by controlling the two different silver sources and electroless silver plating time. The optimum condition uses silver ammonia reacted for 14 h. The process of electroless silver plating uses the mixed growth model of layered growth and island growth. Silver atoms firstly attach to the surface of the as-prepared copper nanoparticles to form the dotted Ag atom structure by galvanic displacement reaction between Cu and [Ag(NH3)2]+, and then more silver atoms, reduced by sodium citrate, gradually deposit on the copper surface to form a fully covered structure. The morphology and core–shell structure of the nanoparticles was observed by scanning electron microscopy, transmission electron microscopy and x-ray diffraction. The simultaneous thermal analyzer results confirmed that the weight gain of Cu–Ag core–shell nanoparticles was 2.2% when heated up to 400 °C, which was lower than pure Cu nanoparticles. According to the x-ray photoelectron spectroscopy results, the Cu–Ag core–shell nanoparticles exhibited good anti-oxidation performance compared with the pure copper nanoparticles after being stored for one month under the ambient conditions.

Rational construction of Au–Ag bimetallic island-shaped nanoplates for electrocatalysis

Active electrocatalysts are the key to water splitting for hydrogen production through the electrolysis. In this paper, 50 nm silver nanoplates were used as templates for synthesis of Au–Ag island-shaped nanoplates by controlling the surface chemistry. The guiding mechanism of polyvinylpyrrolidone (PVP, Mw = 40 000) to Au–Ag island-shaped nanoplates crystal was also further investigated. It is found that the surface energy of Ag nanoplates between (100) and (111) crystal planes can be regulated by varying the amount of PVP in the system. Then a uniform Au-Ag triangular island nanostructure was obtained. Compared with the Ag nanoplates catalysts, the Au–Ag island nanoplates catalysts show the superior catalytic performances in hydrogen evolution electrocatalysis (HER). These results demonstrate a new surface chemistry modification by PVP and a galvanic displacement reaction for designing the active electrocatalysts. More importantly, the Au–Ag island-shaped nanoplates show an unconventional growth mode of preserving the original Ag nano-triangular crystal structure. The enhanced performance in electrocatalysis can be mainly attributed to Au–Ag alloy structure, which allows the appearance of synergistic effects. The present work demonstrates the crucial roles of surface chemistry in catalysts synthesis, which may guide the design of active bimetallic catalysts.

Plasmonic biosensors fabricated by galvanic displacement reactions for monitoring biomolecular interactions in real time

Optical sensors are prepared by reduction of gold ions using freshly etched hydride-terminated porous silicon, and their ability to specifically detect binding between protein A/rabbit IgG and asialofetuin/Erythrina cristagalli lectin is studied. The fabrication process is simple, fast, and reproducible, and does not require complicated lab equipment. The resulting nanostructured gold layer on silicon shows an optical response in the visible range based on the excitation of localized surface plasmon resonance. Variations in the refractive index of the surrounding medium result in a color change of the sensor which can be observed by the naked eye. By monitoring the spectral position of the localized surface plasmon resonance using reflectance spectroscopy, a bulk sensitivity of 296 nm ± 3 nm/RIU is determined. Furthermore, selectivity to target analytes is conferred to the sensor through functionalization of its surface with appropriate capture probes. For this purpose, biomolecules are deposited either by physical adsorption or by covalent coupling. Both strategies are successfully tested, i.e., the optical response of the sensor is dependent on the concentration of respective target analyte in the solution facilitating the determination of equilibrium dissociation constants for protein A/rabbit IgG as well as asialofetuin/Erythrina cristagalli lectin which are in accordance with reported values in literature. These results demonstrate the potential of the developed optical sensor for cost-efficient biosensor applications.Graphical abstract

Pd–Cu alloy catalyst synthesized by citric acid-assisted galvanic displacement reaction for N2O reduction

In this study, the composition-optimized Pd–Cu catalyst for electrochemical N2O reduction in highly alkaline solution was prepared by a galvanic displacement method. The atomic ratio of Pd to Cu in Pd–Cu bimetallic catalyst, which has been known to be hardly controlled using galvanic displacement, was tailored by varying the concentration of citric acid in galvanic displacement bath. With increasing citric acid concentration, the decreased grain size, characterized by X-ray diffraction, and the increased amount of carbon in Pd–Cu catalyst, measured by energy-dispersive X-ray spectrometry, revealed the incorporation of citric acid into the catalyst, which was attributed to the tunable catalyst composition. The incorporation of citric acid into Pd–Cu deposit restrained the diffusion of Cu from Cu substrate to deposit, leading to decrease in the Cu content in Pd–Cu. The electrocatalytic activity for N2O reduction was strongly dependent on the Pd/Cu composition in Pd–Cu catalysts. Among the investigated Pd–Cu catalysts with different compositions, the highest electrocatalytic activity was obtained with Pd60Cu40 with a Tafel slope of 0.096 V dec−1. Moreover, the Pd60Cu40 catalyst showed remarkably enhanced mass-specific activity for N2O reduction, compared with a commercial Pd/C. The density functional theory (DFT) calculations revealed that the highest N2O reduction activity of Pd60Cu40 could be attributed to the facilitation of an adsorption/desorption balance for N2O reduction, resulting from the appropriately lowered d-band center of catalyst.

Applications of cathodic Co100-XNiX (x = 0, 30, 70, and 100) electrocatalysts chemically coated with Pt for PEM fuel cells

The present work comprises a study about the synthesis, characterization, and performance evaluation of four Co100-X-NiX (x = 0, 30, 70, and 100) electrocatalysts coated with Pt with potential catalytic activity towards ORR. Electrocatalysts were prepared through a two-stage process combining the versatile high-energy ball milling synthesis and the galvanic displacement method. On a first stage, high-energy ball milling was used to produce nanoparticles of non-noble transition metals, (M = Co100 and Ni100) and (BM = Co30Ni70and Co70Ni30). On a second stage, galvanic displacement reactions via chemical reflux treatment were employed to promote a Pt coating over the milled nanoparticles. The four electrocatalysts were dispersed on Vulcan carbon maintaining a metal:carbon (wt.%) ratio of 50:50 each one. The result was two type of systems: (M-Pt/C = Co100–Pt/C and Ni100–Pt/C) and (BM-Pt/C = Co30Ni70–Pt/C and Co70Ni30–Pt/C). All the electrocatalysts presented a final composition: ~10 wt%. of Pt, ~40 wt% of Co100-xNix, and ~50 wt% of Vulcan carbon. Physical characterization of the synthesized electrocatalysts involved XRD, STEM, AAS-ICP-MS and EDS-SEM studies confirming the formation of homogeneously-distributed metallic nanoparticles on the carbon. The electrochemical evaluation, through cyclic voltammetry and steady-state polarization curves using rotating disk electrode technique, was performed for the four synthesized electrocatalysts and for a commercial platinum-loaded carbon black (Pt Etek 20 wt%) catalysts. All four synthesized electrocatalysts were electroactive for ORR. Moreover, the Ni100–Pt/C electrocatalyst presented the highest mass activity whereas Co30Ni70–Pt/C electrocatalyst showed the major stability after 3000 cycles of accelerated degradation test than the others. Two membrane electrode assemblies (MEAs) for PEM fuel cell were fabricated with the synthesized Ni100–Pt/C and Co30Ni70–Pt/C electrocatalysts used as cathodes. Results under single-fuel cell operation showed the same performance trend for those materials that observed under electrochemical glass cell conditions.