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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.

International audience; The fabrication of low-resistance and thermally stable Ohmic contacts is essential for the realization of reliable GaN power devices. In the particular case of p-type GaN, a thin Ni/Au bilayer is commonly used for Ohmic contacts. However, Au metal contacts are quite expensive, are incompatible with the complementary metal oxide–semiconductor foundries, and also have poor thermal stability. Thus, seeking an alternative that is affordable and thermally stable is crucial. In the present study, we investigate Au-free Ohmic contact formation on p-type GaN using a bilayer Ni/Al-doped ZnO (AZO) thin film. Careful studies were focused on identifying the role of process parameters such as annealing parameters: temperature, time, and atmosphere in order to obtain an excellent Ohmic contact on p-GaN. Our results show that the contact resistance can be significantly reduced using a Ni/AZO bilayer with a suitable rapid thermal process. We demonstrate that the specific contact resistance for Ni/AZO on p-GaN can reach the lowest value of 1.85 × 10–4 Ω·cm2 for a sample with a 5 nm Ni layer annealed at 500 °C in air for 5 min. Our work demonstrates that the bilayer Ni/AZO contact could be suitable for efficient GaN power diodes or transistors.

International audience; The weak ferroelectric contribution to the polarization of antiferroelectric lead zirconate (PZO) thin films has been investigated using PUND (Positive Up Negative Down) pulse measurements and hysterons decomposition by First Order Reversal Curves (FORC) technique. The PUND allows decomposing the measured current, obtained from the polarization-electric field loop measurements, into a switching and a non-switching contribution. We show that the weak ferroelectric phase is enhanced when a large electric field has been previously applied to the material, in order to switch from the antiferroelectric to the ferroelectric phase. Using the PUND measurement at fields below the antiferroelectric to ferroelectric phase transition, the polarization loop corresponding only to the ferroelectric switching contribution has been determined revealing that this contribution to the overall polarization is small. FORC measurements, however, indicate that the ferroelectric phase is present at different fields. At low fields, a quite homogeneous distribution of hysterons exists and at large field, a high concentration of hysterons at a field near to the antiferroelectric to ferroelectric phase transition can be seen. Moreover, when changing the delay between pulses of the PUND and the FORC measurements, we show that this weak ferroelectricity contribution is metastable and decreases with time.

International audience

International audience; Sintering is a very important process in materials science and technological applications. Despite breakthroughs in achieving optimized piezoelectric properties, fundamentals of K$_{0.5}$Na$_{0.5}$NbO$_3$ (KNN) sintering are not yet fully understood, facing densification versus grain growth competition. At present, microscale events during KNN sintering under reducing atmospheres are real-time monitored using a High Temperature-Environmental Scanning Electron Microscope. A two contacting KNN particles model satisfying the Kingery and Berg's bulk diffusion model is reported. Dynamic events like individual grain growth and grain elimination process are explored through a postanalysis of recorded image series. The diffusion coefficient for oxygen vacancies of 10$^{−8}$ cm$^2$ s$^{−1}$ and average boundary mobility of 10$^{−9}$ cm$^4$ J$^{−1}$ s$^{−1}$ are reported for the KNN ceramics. Moreover, the local pore shrinkage is consistent with the Kingery and François's concept of pore stability except that pore curvatures are not all concave, convex or flat due to anisotropic grain-boundary energies. The global grain growth kinetics are described using parabolic and/or cubic laws. The effect of atmospheres and microstructure evolution on the intrinsic and extrinsic contributions to the dielectric response using Rayleigh's law is also explored. These results bring a new breath for KNN sintering studies in order to adapt the sintering process.

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.

The miniaturization of electronic devices and power systems requires the fabrication of functional components in the form of micrometer-sized thick films. A major challenge is the integration of functional ceramics with metals, which are considered incompatible with high-temperature ceramic processing. To overcome the integration barrier, an aerosol deposition (AD) spray-coating method based on room temperature deposition can be used. By employing the AD method, we were able to deposit relaxor-ferroelectric 0.65Pb(Mg1/3Nb2/3)O3–0.35PbTiO3 ceramic thick films on low-cost stainless-steel substrates. The as-deposited films were dense, with ∼97% of the theoretical density. Moreover, the post-deposition annealing at 500 °C did not result in any microstructural changes. Compared to the as-deposited films, the annealed films exhibit improved energy storage and electromechanical properties. The annealed thick films achieve a recoverable energy density of 15.1 J⋅cm−3 at an electric field of 1350 kV⋅cm−1 and an electric-field cycling stability of 5 million cycles. A piezoelectric response was detected through the entire film thickness by piezoelectric force microscopy. Macroscopic displacement measurements revealed a maximum relative strain of 0.38% at 1000 kV⋅cm−1, corresponding to inverse effective piezoelectric coefficient of ∼40 pm⋅V−1. In this study, we overcame the integration challenges and demonstrated the multifunctionalization of future ceramic-metal structures, as the deposited thick films on stainless steel exhibit energy storage capability and piezoelectric properties.

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.