We report a sonochemical synthesis of homogeneous PtCu 3 nanoparticles. Ultra-sonication during reduction in a non-aqueous solution is compared with synthesis under identical conditions in the absence of sonication (to form a Rieke alloy). X-ray diffraction (XRD) measurements suggest that the sonochemical procedure produces an amorphous, uniformly alloyed nanomaterial having a composition consistent with the PtCu 3 stoichiometry, while the Rieke alloy is polyphasic. Energy dispersive X-ray (EDX) analysis indicates that the composition of the sonochemically prepared PtCu 3 material reflects the nominal values. EDX and XRD analyses also provide evidence for the inhibition of oxide formation on sonochemically prepared PtCu 3 nanoparticles, but oxide is readily apparent in the Rieke alloy. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images of the sonochemically prepared sample show particles with diameters of $2 to 3 nm. As-synthesized PtCu 3 particles were activated using an electrochemical de-alloying procedure to prepare an oxygen reduction electrocatalyst. The de-alloyed catalyst consisted of a Pt-rich surface layer, over a core indicated as having a Pt 3 Cu composition. The de-alloyed sample exhibited $3 to 6 fold enhancements in oxygen reduction reaction (ORR) activity when compared to commercial Pt catalysts.
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