The doctoral thesis discusses the measurement of parameters of piezoelectric (PZT) materials and the influence of temperature on their stability. In the introductory sections, the author briefly explains the piezoelectric effect and its use; simultaneously, methods for the preparation of piezoelectric materials and the measurement of their properties are presented to illustrate the analyzed problem. The experimental part of the thesis describes the procedure of measuring and calculating the complete matrix of material coefficients from samples of PZT ceramics. The applied set of piezoelectric samples complying with relevant European and world standards was made in the form of thin plates, thin discs and cylinders, via gradual modification of the large disc. The NCE51 and/or the older PCM51 ceramics obtained from the company Noliac Ceramics were used in determining the complete matrix and describing the measurement method. Both these types are soft piezoceramics composed from a solid solution of lead zirconate and lead titanate with the general chemical formula of Pb(Zr1-x,Tix)O3. The real crystallographic structure and chemical composition of the samples were confirmed by X-ray diffraction spectroscopy and energy dispersive spectroscopy (EDS), respectively. The frequency method was used for the measurement and calculation of all material coefficients. An Agilent 4294A impedance analyzer and a set of measuring tweezers marketed as “Tweezers Contact Test Fixture 16334A” were used in the process. Fast determination of the entire matrix of coefficients without any special requirement for the preparation of the samples to be measured was tested and verified. The charge coefficients of the piezoelectric material were confirmed by direct methods including the laser interferometer technique, the vibrometric method, and the procedure utilizing changes of the force applied to the sample. The advantages and disadvantages of the methods were compared and defined based on measurements and their results. The main part of thesis was focused on the behavior of piezoelectric material at high temperatures near the Curie point. Depolarization performed by means of a high temperature approaching the Curie point constitutes a significant yet hardly measurable material property of PZT ceramics. Commonly available vibrometric methods (d33-meters) do not appear to be suitable for the measurement of temperature dependencies, and for that reason the frequency technique was used. The piezoelectric charge coefficient, whose value can be effectively measured via the above-discussed frequency method, was selected as the indicator showing the depolarization state in the applied piezoelectric ceramics. The accuracy of the procedure was verified via comparison of the vibrometric method in cylinders of the NCE51 ceramics with different sizes, which are designed for the longitudinal length mode. The result is an optimized measurement methodology which facilitates accurate determination of the Curie temperature, namely phase transition to the cubic crystallographic structure. The experiment also proved the applicability of progressive, controlled depolarization of PZT ceramics via high temperature, and it also enabled us to define the temperature limits at which there occur irreversible changes of the piezoelectric properties of piezoceramics. In the measured NCE51 and PCM51 materials, the limit for the irreversible changes was equal to 95% of the Curie temperature.