Reliable quantification of 3D results obtained by X-ray Energy Dispersive Spectroscopy (XEDS) tomography is currently hampered by the presence of shadowing effects and poor spatial resolution. Here, we present a method that overcomes these problems by synergistically combining quantified XEDS data and High Angle Annular Dark Field -Scanning Transmission Electron Microscopy (HAADF-STEM) tomography. As a proof of principle, the approach is applied to characterize a complex Au/Ag nanorattle

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... d through a galvanic replacement reaction. However, the technique we propose here is widely applicable to a broad range of nanostructures.