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The compositional microstructure of a zinc sample that has been subjected to aqueous oxidation has been investigated using a data‐constrained modelling (DCM) approach combined with multi‐energy X‐ray micro computed tomography (CT) data. High‐resolution X‐ray CT data sets were acquired at the Shanghai Synchrotron Radiation Facility (SSRF) at beam energies of 9 and 10.5 keV. CT images were used to reconstruct the three dimensional chemical compositional distribution via the DCM approach, with spatial resolution at the order of a micron. The results indicate that the interface between zinc and zinc oxide is characterized by a triple layer where the innermost layer consists of zinc and zinc oxide and the outer layers of zinc oxide with differing density.