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In this work, we present facile synthesis of amorphous Ni/Fe mixed (oxy)hydroxide (NiFe(H)) nanoparticles (NPs) and their electrocatalytic performance for oxygen evolution reaction (OER) in alkaline media. a-NiFe(H) NPs have received lots of attention as OER electrocatalysts with many desirable properties. By using a simple sonochemical route, we prepared amorphous Ni and Fe-alkoxide (NiFe(A)) NPs whose composition can be controlled in the entire composition range (NiFe, 0≤x≤1). These samples are composed of extremely small NiFe(A) NPs with Ni and Fe atoms homogeneously distributed. NiFe(A) NPs are readily converted into corresponding electrocatalytically active NiFe(H) NP by a simple electrochemical treatment. Electrochemical analysis data show that the OER activity of amorphous NiFe(H) samples follows the volcano-type trend when plotted against the Fe content. NiFe(H) sample showed the lowest overpotential of 292mV at 10mAcm and the lowest Tafel slope of 30.4mVdec, outperforming IrO/C (326mV, 41.7mVdec). Our samples are highly durable based on the chronopotentiometry data at the current density of 10mAcm for 2h which show that NiFe sample maintains the steady-state potential, contrary to the time-varying IrO/C.

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