The　Au-Ni　bimetal　nanoparticles　were　prepared　by　coreduction　in　aqueous　solution　and　post-heat-treatment　process.　In　this　synthesis　approach,　NaBH4　was　used　as　reductive　reagent　and　sodium　dodecyl　sulfate　was　added　as　surfactant　to　control　the　size　and　the　morphology　of　the　nanoparticles.　Post-heat-treatment　was　performed　to　further　remove　the　oxide　species　on　the　surface　of　the　nanoparticles.　Structural　and　compositional　evolution　analysis　of　the　nanostructured　bimetals　are　performed　by　scanning　electron　microscopy　(SEM),　transmission　electron　microscopy　(TEM),　X-ray　diffraction　(XRD)　and　X-ray　photoelectron　spectrometry　(XPS)　measurements.　The　Au-Ni　electrocatalysts　for　electro-oxidation　of　formic　acid　in　acidic　media　were　investigated.　(C)　2009　Elsevier　B.V.　All　rights　reserved.