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Rational synthesis of bimetallic alloy nanocrystals (NCs) is still a great challenge. Especially, spatially uniform alloy NCs are very difficult to achieve because of the different reduction rates of the individual alloy components. Herein we propose a facile wet chemical synthetic strategy to prepare uniform bimetallic alloy NCs with tunable composition by controlling the growth of alloy NCs under diffusion controlled conditions. Using this strategy, we successfully synthesized trisoctahedral (TOH) Au–Pd alloy NCs enclosed by {hhl} high-index facets with uniform spatial distributions and different compositions. Significantly, using our strategy, the composition of the as-prepared Au–Pd alloy NCs is identical to the ratio of the two metal precursors in the reaction solution over a wide range. Investigation of the composition-dependent electrochemical behavior of the as-prepared TOH Au–Pd alloy NCs showed that the TOH Au–Pd alloy NCs containing 14.1 atom% Pd exhibited the best activity.
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