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Rapid Synthesis and Correlative Measurements of Electrocatalytic Nickel/Iron Oxide Nanoparticles



Kavita M. Jeerage, Stephanie L. Candelaria, Samuel M. Stavis


Electrocatalytic nanoparticles, such as nickel/iron oxides for oxygen evolution (OER) in alkaline electrolytes, require rapid synthesis and measurement for practical use. To address this issue, we investigated a novel process of adding Ni(II) species to Fe nanoparticles immediately after synthesis, which we expected to yield Ni-rich shells around Fe-rich cores. Cyclic voltammetry showed that the overpotential decreased as the molar ratio of Ni to Fe in the synthesis vessel increased from 0.2 mol Ni : 1 mol Fe to 1.5 mol Ni : 1 mol Fe, consistent with an increase of Ni composition. Unexpectedly, the overpotential increased abruptly at 2.0 mol Ni : 1 mol Fe. X-ray photoelectron spectroscopy revealed that this synthesis ratio resulted in less Ni at the nanoparticle surfaces than lower synthesis ratios. These results demonstrate the sensitivity of rapid electrochemical measurements to surface composition, and the limits of Ni(II) adsorption and reduction to rapidly form Ni-rich shells around Fe-rich cores. Cyclic voltammetry also showed that the onset of methanol oxidation (MOR) correlates with the oxidation of Ni(OH)2 to NiOOH. Therefore, tuning materials to improve performance as OER catalysts also improves their performance as MOR catalysts.
Scientific Reports


core-shell nanoparticles, cyclic voltammetry, methanol oxidation, oxygen evolution, X-ray photoelectron spectroscopy


Jeerage, K. , Candelaria, S. and Stavis, S. (2018), Rapid Synthesis and Correlative Measurements of Electrocatalytic Nickel/Iron Oxide Nanoparticles, Scientific Reports, [online], (Accessed May 29, 2024)


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Created March 15, 2018, Updated November 10, 2018