ABSTRACT The study of the ultrasonic acoustic response of materials is of increasing interest for the characterisation of high-frequency applications. In this work, some elastic properties (acoustic velocity and acoustic attenuation) and some physical properties (thickness and density), together with the phase shift of the transducer, are estimated via one method. Scanning acoustic microscopy was performed via an innovative and different method using a high-frequency (50 MHz) planar wave transducer. In addition, the Debye series model (DSM) was used to model the acoustic response of the bilayer structure of the glass substrate and the resin‒epoxy sample. The inverse problem of estimating the acoustic parameters that results in a DSM reflected echo that matches the experimental signal is solved by proposing an innovative step-by-step curve fitting algorithm. The algorithm for solving the inverse problem is then optimised via relative mean square error (RMSE) curves, resulting in a robust method for assessing the uniqueness of the multiparameter solution.