Brillouin spectroscopy was used to probe the hypersonic properties of Ca-modified lead titanate between the pure amorphous and the coarse grained state. The samples were thin films rf sputtered onto (100)-silicon wafer at ambient temperature, followed by an annealing process in the range from 673 to 873 K. An elastic instability of the longitudinally polarized sound mode suggests the existence of a discontinuous structural transformation from the amorphous to the nanostructured state. [S0031-9007(97)02610-0] PACS numbers: 81.05. Ys, 68.35.Rh, 68.60.Bs, 78.35. + c Against the background of an increasing interest in nanostructured materials (nsM) the physical properties of the intermediate metastable structures between the pure amorphous and the microcrystalline states require special attention. One possible way to realize such intermediate states is to produce sputtered amorphous (dielectric) films and to anneal these films successively in an appropriate way. It is likely that the annealing-induced transformation from the initial amorphous state to the final coarse grained state may pass through one or more so-called metastable nanocrystallized states (e.g. [1][2][3][4][5]). It is a matter of current physical interest (i) whether these intermediate nanostructured states (nsS) can be fixed, (ii) how the transformation from the amorphous to the microcrystalline states takes place, and (iii) what are the properties of these intermediate states. Although the amorphous state as well as the nsS are metastable, the possibility of a structural phase transformation between the crystalline and the amorphous states has been proposed in the literature [1,5]. Based on free-energy simulations, Wang et al. [6], only recently, have predicted a phase transition from the nanocrystalline to the glassy state. A hint for the existence of such a transition may be drawn from the work of Rehn et al. [1]. These authors have reported an elastic shear instability for ion damaged Zr 3 Al.It is well established now that the evolution of the nsS is accompanied by an anomalous behavior in the elastic properties when compared to the amorphous and the microcrystalline reference states [2,4,7,8]. Experimental and theoretical results indicate a significant influence in the size of nanoparticles on the elastic properties of the consolidated nsM (e.g., [2,4,[9][10][11][12][13]). In turn, the elastic properties are expected to reflect the predicted transition from the amorphous to the nsS. The aim of the current paper is to show evidences for such a transformation in rf-sputtered films of Ca-modified lead-titanate ͑Pb 0.76 Ca 0.24 ͒TiO 3 (PTC) at a critical annealing temperature ͑T ca ഠ 823 K͒. As a sensitive probe we used the lon-gitudinally polarized acoustic phonon mode as detected by high resolution Brillouin spectroscopy (BS).PTC is -in the single or coarse grained polycrystalline state-a ferroelectric perovskite with a phase transition from the paraelectric to the ferroelectric state at T c ഠ 530 K [14]. At room temperature, the material is t...