Shape-controlled palladium nanowires and nanoparticles electrodeposited on carbon electrodes

Corduneanu, Oana; Diculescu, Victor C.; Chiorcea-Paquim, Ana-Maria; Oliveira-Brett, Ana Maria

doi:10.1016/j.jelechem.2008.07.034

Cited by 39 publications

(29 citation statements)

References 54 publications

(87 reference statements)

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“…These voltammetric features provide evidence for the nucleation and growth of Pd at the HOPG surface, with the magnitude and nature of the features strongly dependent on the voltammetric conditions, timescale and concentration of the Pd precursor in solution. 37,39 This electrochemical behavior is consistent with previous reports of Pd electrodeposition at the macroscale, 31,37 highlighting that the microscale measurements do not introduce any new features or perturb this system compared to macroscopic studies. Potential step chronoamperometry is the preferred technique for monitoring electrochemical nucleation and growth processes, as this provides a constant (but controllable) driving force for electrodeposition, with the current-time behavior considered to inform on the rate and mechanism.…”

Section: Experimental Methodssupporting

confidence: 87%

“…37,38 In the second cycle, the reduction peak of Pd electrodeposition was broadened (also due to concomitant oxide reduction), and the onset potential was shifted significantly positive to 0.37 V, as expected for the growth of Pd on preformed Pd rather than on the carbon substrate. 37,39 In addition, the current magnitudes of two oxidation peaks were increasedparticularly the more cathodic peak, corresponding to the formation of Pd oxide -and shifted slightly negative to 0.36 V and 0.51 V, respectively. These voltammetric features provide evidence for the nucleation and growth of Pd at the HOPG surface, with the magnitude and nature of the features strongly dependent on the voltammetric conditions, timescale and concentration of the Pd precursor in solution.…”

Section: Experimental Methodssupporting

confidence: 55%

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Nucleation and Aggregative Growth of Palladium Nanoparticles on Carbon Electrodes: Experiment and Kinetic Model

Kim¹,

Lai

McKelvey³

et al. 2015

J. Phys. Chem. C

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The mechanism and kinetics of the electrochemical nucleation and growth of Pd nanoparticles (NPs) on carbon electrodes have been investigated using a microscale meniscus cell on both highly oriented pyrolytic graphite and a carbon coated transmission electron microscopy (TEM) grid. Using a microscale meniscus cell, it is possible to monitor the initial stage of electrodeposition electrochemically, while the ability to measure directly on a TEM grid allows subsequent high resolution microscopy characterization which provides detailed nanoscopic and kinetic information. TEM analysis clearly shows that Pd is electrodeposited in the form of NPs (approximately 1 − 2 nm diameter) that aggregate into extensive nanocrystaltype structures comprised of NPs. This gives rise to a high NP density. This mechanism is shown to be consistent with double potential step chronoamperometry measurements on HOPG, where a forward step generates electrodeposited Pd and the reverse step oxidizes the surface of the electrodeposited Pd to Pd oxide. The charge passed in these transients can be used to estimate the amounts of NPs electrodeposited and their size. Good agreement is found between the electrochemically determined parameters and the microscopy measurements. A model for electrodeposition based on the nucleation of NPs that aggregate to form stable structures isproposed that is used to analyze data and extract kinetics. This simple model reveals considerable information on the NP nucleation rate, the importance of aggregation in the deposition process and quantitative values for the aggregation rate.

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Section: Experimental Methodssupporting

confidence: 87%

Section: Experimental Methodssupporting

confidence: 55%

Nucleation and Aggregative Growth of Palladium Nanoparticles on Carbon Electrodes: Experiment and Kinetic Model

Kim¹,

Lai

McKelvey³

et al. 2015

J. Phys. Chem. C

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“…Both spatial and size control can be easily achieved by the fine tuning of electrochemical parameters. 21 The major advantage associated with the electrochemical synthesis of nanoscale metal particles is that it does not require toxic reducing/stabilizing agents and sophisticated equipment. Moreover, the particles can be directly deposited on conducting platforms for microelectronic and micro fuel-cell applications.…”

Section: Introductionmentioning

confidence: 99%

Pt-Pd nanoelectrocatalyst of ultralow Pt content for the oxidation of formic acid: Towards tuning the reaction pathway

Ghosh

Raj

2015

J Chem Sci

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Synthesis of highly efficient functional electrocatalyst that favours the electrochemical oxidation of formic acid via CO-free dehydrogenation pathway is required for direct formic acid fuel cells. Traditional catalysts favour the dehydration pathway involving the generation of poisonous CO. Herein we demonstrate the superior electrocatalytic performance of Pt-Pd bimetallic nanoelectrocatalyst of ultralow Pt content and tuning the reaction pathway by controlling the Pt content. Bimetallic nanoparticles of Pt 4 Pd 96 , Pt 7 Pd 93 and Pt 47 Pd 53 compositions are synthesized by electrochemical co-deposition method in aqueous solution. The nanoparticles of ultralow Pt content, Pt 4 Pd 96 , favour the CO-free dehydrogenation pathway for formic acid oxidation with an onset potential of 0 V (SHE) whereas the Pt 47 Pd 53 nanoparticles favour the dehydration pathway involving the formation of CO at high positive potential. The Pt content of the bimetallic nanoparticles actually controls the oxidation peak potential and catalytic activity. Significant negative shift (∼350 mV) in the oxidation peak potential and remarkable enhancement in the current density (2.6 times) are observed for Pt 4 Pd 96 nanoparticles with respect to Pt 47 Pd 53 . The absence of three adjacent Pt and Pd atoms could be the reason for the suppression of CO pathway. The electrochemical impedance measurements indirectly support the CO-free pathway for the formic acid oxidation on Pt 4 Pd 96 nanoparticles.

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“…6 are shown successive CVs starting at E i = 0.00 V in the positive direction until E 1 = +1.40 V then going in the negative direction to progressively more negative applied potential limits. The CVs recorded showed that when the negative applied potential reaches E 2 = − 0.50 V a complex electrochemical behaviour is observed, characteristic of the electrodeposition of palladium at the surface of the electrode [30,31].…”

Section: Voltammetric Characterization Of Pd(ii)-spm and Pd(ii)-spdmentioning

confidence: 99%

“…Indeed Pd(II)-Spd has three palladium atoms, which increase the spontaneous adsorption onto HOPG [30,31], and two Spd molecules, vs. two palladium and one Spm in the case of Pd(II)-Spm. Additionally the larger Pd(II)-Spd complexes lead to the formation of larger and higher molecular clusters, Fig.…”

Section: Afm Characterization Of Spontaneously Adsorbed Pd(ii)-spm Anmentioning

confidence: 99%

Polynuclear palladium complexes with biogenic polyamines: AFM and voltammetric characterization

Corduneanu

Chiorcea-Paquim

Fiuza

et al. 2010

Bioelectrochemistry

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Polynuclear Pd(II) complexes with biogenic polyamines present great potential clinical importance, due to their antiproliferative and cytotoxic activity coupled to less severe side-effects. The adsorption process and the redox behaviour of two polynuclear palladium chelates with spermine (Spm) and spermidine (Spd), Pd(II)-Spm and Pd(II)-Spd, as well as of their ligands Spm and Spd, were studied using atomic force microscopy (AFM) and voltammetry at highly oriented pyrolytic graphite and glassy carbon electrodes. AFM revealed different adsorption patterns and degree of surface coverage, correlated with the chelate structure, concentration of the solution, applied potential and voltammetric behaviour of the Spm, Spd, Pd(II)-Spm and Pd(II)-Spd systems. The voltammetric study of Spm and Spd showed that these biogenic polyamines undergo an irreversible and pH-dependent oxidation. In acid medium the polyamines are fully protonated, rendering their oxidation more difficult. With increasing pH the oxidation potential for both Spm and Spd is shifted to less positive values, indicating a greater ease of oxidation in alkaline medium. The Pd(II)-Spm and Pd(II)-Spd complexes dissociate at high negative or high positive potentials. The application of a positive potential induced the oxidation of these Pd complexes and the formation of mixed layers of palladium oxides, Spm/Spd and Pd(II)-Spm/Pd(II)-Spd.

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Shape-controlled palladium nanowires and nanoparticles electrodeposited on carbon electrodes

Cited by 39 publications

References 54 publications

Nucleation and Aggregative Growth of Palladium Nanoparticles on Carbon Electrodes: Experiment and Kinetic Model

Nucleation and Aggregative Growth of Palladium Nanoparticles on Carbon Electrodes: Experiment and Kinetic Model

Pt-Pd nanoelectrocatalyst of ultralow Pt content for the oxidation of formic acid: Towards tuning the reaction pathway

Polynuclear palladium complexes with biogenic polyamines: AFM and voltammetric characterization

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