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We have adapted the two-phase Brust method to synthesize large quantities of AuPd alloy nanoparticles with diameter of 1.86 ± 0.40 nm. When the particles were spread at the air/water interface of a Langmuir–Blodgett (LB) trough, they exhibited a distinct pressure area isotherm curve. The X-ray reflectivity (XRR) shows the formation of an incompressible monolayer with uniform thickness of 1.16 ± 0.02 nm at low pressures which collapses to form a second layer with 2.13 nm thickness at higher pressures. High resolution transmission electron microscopy (HRTEM) imaging of the monolayer indicates that the particles are highly crystalline, with well-defined atomic planes and self-assembly into a hexagonal structure. Extended X-ray absorption fine structure (EXAFS) analysis of the LB lift-off films only shows Au–Au and Au–Pd configurations, consistent with the formation of random alloy rather than core–shell …