The application of microwave diamond-based HBAR as a sensor of microwave acoustic attenuation α was considered, using the Mo film as an object of research. A multilayered piezoelectric structure, as the Al/Al0.73Sc0.27N/Mo/(100) diamond/Mo, was produced using aluminum–scandium nitride composition, and was studied in detail for a number of the Mo films with different thicknesses obtained by magnetron deposition. The operational frequency band of 3.3 … 18 GHz was used. It was found that the dependence of the resonant frequency shift vs. theh(Mo) thickness for all the overtones to be investigated was linear. For a given sensor, it was found that the mass sensitivity per unit arearmwas equal to −26 × 10−12and −8.7 × 10−12g/(cm2∙Hz) at 6.0 GHz and 18.3 GHz, respectively. The frequency dependencies of quality factorQ, which changed as a result of Mo film deposition, were considered as the basic experimental data. A method for extracting the α(Mo) values was proposed. TheQ-factor under the complete deposition of Mo film was 936 nm, and dropped moderately to ~25%. Such values were enough for an aim of the given experiment. The α(f) in molybdenum was obtained, and demonstrated a dependence that was close to quadratic, corresponding to the Akhiezer attenuation law.