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In this paper, the field-induced residual ferroelectricity in antiferroelectric lead zirconate thin films has been studied by impedance measurements together with a hyperbolic law analysis, which permits us to extract the different contributions to the material’s complex permittivity. By measuring the Rayleigh coefficient αr, it appears that the residual ferroelectricity is considerably enhanced when the sample has been previously exposed to an electric field close to the antiferroelectric to ferroelectric transition field. This indicates that a part of the material remains ferroelectric after the antiferroelectric–ferroelectric backward transition, which constitutes an additional contribution to polarization. Consequently, a higher domain wall density and mobility can be observed. Measurements after exposition to thermal treatment show that this ferroelectric response is metastable.

In this paper, the nanolamination of a ZrO2 insulator by Al2O3 for metal insulator metal capacitor applications has been studied. The insulating layers (ZrO2 and Al2O3) were deposited by atomic layer deposition and the electrodes were made of TiN. Different configurations of ZrO2 and Al2O3 alternations were studied, including 1 to 16 Al2O3 inclusions in the ZrO2 layer. X-ray diffraction of the insulator configurations showed that with four or more Al2O3 inclusions, the structure loses its crystalline orientation and becomes amorphous. Electrical characterizations have been conducted to study the capacitance, breakdown field, and leakage current for every insulator configuration. The capacitance density significantly decreases as the number of Al2O3 layers increases, except when an amorphous transition occurs; at this point, a local maximum of 17 nF/mm2 was found. A 19% increase of the breakdown field of samples with two or more Al2O3 inclusions has been correlated with an increase of leakage current explained by the emergence of the Fowler–Nordeim conduction mechanism at electrical fields higher than 4 MV/cm.

In this work, the effects of thermal annealing at 500 °C on aerosol-deposited 0.65Pb(Mg1/3Nb2/3)O3-0.35PbTiO3 thick films on stainless-steel substrates are investigated using two complementary methods at high and low applied external electric fields. The first one is the positive up negative down method, which allows us to obtain information about the switching and non-switching contributions to the polarization. It shows that the as-deposited film is ferroelectric before annealing, since it has a switching contribution to the polarization. After annealing, both the switching and non-switching contributions to polarization increased by a factor of 1.6 and 2.33, respectively, indicating a stronger ferroelectric behavior. The second method is based on impedance spectroscopy coupled with Rayleigh analysis. The results show that post-deposition thermal annealing increases the reversible domain wall contribution to the dielectric permittivity by a factor of 11 while keeping the threshold field similar. This indicates that, after annealing, domain wall density is larger while domain wall mobility remains similar. These two complementary characterization methods show that annealing increases the ferroelectric behavior of the thick film by increasing the domain wall density, and its influence is visible both on polarization vs electric field loop and dielectric permittivity.

International audience; In this study, two different methods have been used in order to characterize leadzirconate anti-ferroelectric thin film elaborated by a modified sol-gel process: First-Order Reversal Curves (FORC) measurements and impedance spectroscopy coupled to hyperbolic law analysis. Approaches at low and high applied electric fields allow concluding on the presence of a weak residual ferroelectric behavior even if this contribution is not visible on the polarization-electric field loops. Moreover, the weak ferroelectric phase seems to switch only when the phase of the antiferroelectric cells is modified and no coalescence of ferroelectric domains at low field occurs due to a well distribution of small residual ferroelectric clusters in the material. The main goal of this paper is to show that FORC distribution measurements and impedance spectroscopy coupled to the hyperbolic law analysis are very sensitive and complementary methods.