Lead zirconium titanate (PZT) is a ubiquitous piezoelectric ceramic material used in sensing/actuation, with appli cations such as in electronics or energy harvesting. Its functionality at low temperature is less explored, although piezoelectric materials have potential applications in deep space and low temperature/cryogenic environments. Non-destructive X-ray imaging of PZT, at room and low temperature, remains unexplored and is challenging due to its lead (Pb) content. To overcome this, high energy X-ray photons were used to investigate commercial hard and soft PZT ceramics and their microstructures at 300 K and 77 K. The results show a clear variation in the porosity between the soft and hard PZT, with the former having higher porosity. At low temperature, the materi als thermally contract by about 4-8 & micro;m, straining the microstructures. Combined with electrical characterization, the results show that in addition to the material's pyroelectric behavior, a large thermal contraction and mate rial porosity can also impact the polarization switching behavior at low temperatures. The results provide new insights on the effects of processing and microstructure on the ferroelectric response in PZT, using synchrotron Xray microtomography, and can potentially be used as another tool in the microstructural and domain engineering of Pb and non-Pb based piezoelectric/ferroelectric materials.

In this work, we present the area-selective growth of zinc oxide nanowire (NW) arrays on patterned surfaces of a silicon (Si) substrate for a piezoelectric nanogenerator (PENG). ZnO NW arrays were selectively grown on patterned surfaces of a Si substrate using a devised microelectromechanical system (MEMS)-compatible chemical bath deposition (CBD) method. The fabricated devices measured a maximum peak output voltage of ~7.9 mV when a mass of 91.5 g was repeatedly manually placed on them. Finite element modeling (FEM) of a single NW using COMSOL Multiphysics at an applied axial force of 0.9 nN, which corresponded to the experimental condition, resulted in a voltage potential of −6.5 mV. The process repeated with the same pattern design using a layer of SU-8 polymer on the NWs yielded a much higher maximum peak output voltage of ~21.6 mV and a corresponding peak power density of 0.22 µW/cm3, independent of the size of the NW array. The mean values of the measured output voltage and FEM showed good agreement and a nearly linear dependence on the applied force on a 3 × 3 µm2 NW array area in the range of 20 to 90 nN.

The use of piezoelectric nanomaterials combined with ultrasound stimulation is emerging as a promising approach for wirelessly triggering the regeneration of different tissue types. However, it has never been explored for boosting chondrogenesis. Furthermore, the ultrasound stimulation parameters used are often not adequately controlled. In this study, we show that adipose-tissue-derived mesenchymal stromal cells embedded in a nanocomposite hydrogel containing piezoelectric barium titanate nanoparticles and graphene oxide nanoflakes and stimulated with ultrasound waves with precisely controlled parameters (1 MHz and 250 mW/cm2, for 5 min once every 2 days for 10 days) dramatically boost chondrogenic cell commitment in vitro. Moreover, fibrotic and catabolic factors are strongly down-modulated: proteomic analyses reveal that such stimulation influences biological processes involved in cytoskeleton and extracellular matrix organization, collagen fibril organization, and metabolic processes. The optimal stimulation regimen also has a considerable anti-inflammatory effect and keeps its ability to boost chondrogenesis in vitro, even in an inflammatory milieu. An analytical model to predict the voltage generated by piezoelectric nanoparticles invested by ultrasound waves is proposed, together with a computational tool that takes into consideration nanoparticle clustering within the cell vacuoles and predicts the electric field streamline distribution in the cell cytoplasm. The proposed nanocomposite hydrogel shows good injectability and adhesion to the cartilage tissue ex vivo, as well as excellent biocompatibility in vivo, according to ISO 10993. Future perspectives will involve preclinical testing of this paradigm for cartilage regeneration.

The search for a synthesis method to create longer ZnO NWAs with high-quality vertical alignment, and the investigation of their electrical properties, have become increasingly important. In this study, a hydrothermal method for growing vertically aligned arrays of ZnO nanowires (NWs) using localized heating was utilized. To produce longer NWs, the temperature environment of the growth system was optimized with a novel reaction container that provided improved thermal insulation. At a process temperature above ~90 °C, ZnO NWs reached a length of ~26.8 µm within 24 h, corresponding to a growth rate of 1.1 µm/h, nearly double the rate of 0.6 µm/h observed in traditional chemical bath growth using a glass reactor. The densely grown NWs (~1.9/µm2), with a diameter of ~0.65 µm, exhibited a preferred hexagonal c-axis orientation and were vertically aligned to the (100) silicon (Si) substrate. These NW structures have multiple applications, e.g., in piezotronic strain sensors, gas sensing, and piezoelectric energy harvesting. As proof of concept, a piezoelectric nanogenerator (PENG) was fabricated by embedding the NWs in an S1818 polymer matrix over a 15 mm × 15 mm area. Under repeated impulse-type compressive forces of 0.9 N, a maximum peak output voltage of ~95.9 mV was recorded, which is higher by a factor of four to five than the peak output voltage of 21.6 mV previously obtained with NWs measuring ~1.8 µm in length.

Engineering materials through the introduction of point defects has resulted in significant advances in semiconductor processing and, more recently, the observation of novel phenomena such as large reconfigurable strains in ferroelectrics as a result of defect dipole complexes. Up to 0.8% strain has been demonstrated in BaTiO3 crystals dilutely doped with iron. However, the defect dipole pinning sites and the corresponding achievable strains are found to degrade as the crystal is electrically cycled as part of the measurement process. The strain degradation rate is dependent on the applied field values but shows an exponential change in materials properties regardless of the electric field. This behavior, plus a change in impedance with number of times cycled, suggests these changes are due to electric field induced oxygen migration—similar to the cause of the resistance degradation effect. Despite this, effective piezoelectric coefficients of over 4700 pm/V were recorded with 1.5 kV/cm fields, one of the largest values for a lead-free piezoelectric material thus far. In addition, the defect dipole-aligned state and the high strains can be repeatably recovered by a subsequent heat treatment step after cycling. Potential paths to exploiting the defect dipole induced effects and large piezoelectric coefficient in these dilutely doped systems are proposed.

A novel methodology is presented for identifying and distinguishing between structural phases in multi-phasic systems, such as piezoelectric materials like PMN-PT [Pb(Mg1/3Nb2/3)O3-PbTiO3], PIN-PMN-PT [Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3] and PZT [Pb(Zr,Ti)O3], using diffuse multiple scattering and Kossel line diffraction techniques. The method exploits the splitting of triple line intersections from special coplanar reflections combined with logical constraints to generate a splitting fingerprint for robust crystallographic phase determination and discrimination.

This study focuses on the exploration of electromechanical properties of polyvinylidene fluoride (PVDF) using a new characterization tool for piezoelectric polymers. The theoretical background is briefly described, then the experimental setup is shown, results are presented and discussed. The study puts emphasis on the temperature and humidity dependency of d 31 of PVDF. Finally, a short conclusion is given.

Electrical switching of ferroelectric domains and subsequent domain wall motion promotes strong piezoelectric activity, however, light scatters at refractive index discontinuities such as those found at domain wall boundaries. Thus, simultaneously achieving large piezoelectric effect and high optical transmissivity is generally deemed infeasible. Here, it is demonstrated that the ferroelectric domains in perovskite Pb(In1/2 Nb1/2 )O3 -Pb(Mg1/3 Nb2/3 )O3 -PbTiO3 domain-engineered crystals can be manipulated by electrical field and mechanical stress to reversibly and repeatably, with small hysteresis, transform the opaque polydomain structure into a highly transparent monodomain state. This control of optical properties can be achieved at very low electric fields (less than 1.5 kV cm-1 ) and is accompanied by a large (>10 000 pm V-1 ) piezoelectric coefficient that is superior to linear state-of-the-art materials by a factor of three or more. The coexistence of tunable optical transmissivity and high piezoelectricity paves the way for a new class of photonic devices.

Abstract Osteoarthritis implies a progressive degeneration of the whole joint. Cartilage is particularly affected, with inflammation playing a pivotal role1. In recent years, cartilage regeneration has been pursued through several bioengineering strategies and using different stem cell types2-6. Adipose -derived mesenchymal stromal cells (ASCs) constitute an intriguing and minimally invasive option. However, the use of ASCs for cartilage regeneration is hampered by a relatively inefficient expression of key chondrogenic markers7. Thus, new strategies to boost both in situ targeting and chondrogenesis of ASCs are highly desirable. Here we show that ASCs embedded in a nanocomposite hydrogel including piezoelectric nanomaterials and graphene oxide nanoflakes, and stimulated with ultrasound waves with precisely controlled parameters (1 MHz and 250 mW/cm2, for 5 min once every two days for a period of 10 days) dramatically boost cell chondrogenic commitment. Furthermore, this stimulation regimen also has a considerable anti-inflammatory effect. The proposed nanocomposite hydrogel also shows excellent biocompatibility in vivo. Our results show for the first time the chondrogenic potential of the combined piezoelectric nanoparticle-ultrasound stimulus; the proposed paradigm has the potential to trigger cartilage regeneration in osteoarthritis, focal cartilage defects and other pathological conditions involving cartilage lesions and degeneration. Future efforts should expand preclinical data, and target clinical applications of this therapeutic strategy.

Piezoelectric energy harvesting has in recent years technologically advanced and gained excellent momentum due to its enormous energy efficiency and numerous environmental benefits. Zinc oxide (ZnO), on the other hand, continues to remain afloat as a material of choice for the manufacture of a wide range of energy harvesting devices as well as self-powered sensors. In this work, a low-temperature (<100 deg C) aqueous solution growth of uniformly aligned ZnO nanowire arrays (NWAs) on a cost-effective, easy synthesis and compatible silicon (Si) substrate is realized. Compared to its counterparts such as bulk or layers, NWAs have the advantage of being miniaturized and integrated with other devices. On the other hand, the power density of NWAs is higher due to the small active thickness. Furthermore, their higher piezoelectric coefficient and larger elastic deformation when tiny external stimulus are applied for piezo potential generation, makes ZnO NWAs the material of choice. The ZnO NWAs in our experiment were selectively grown on patterned Si substrate surfaces by a devised Microelectromechanical System (MEMS)-compatible chemical-bath deposition (CBD) method. The patterned nanowire growth has the advantage of improved output performance and independent working mode of each region. To facilitate nucleation between the ZnO NWs and the Si substrate, a low- temperature, low-cost direct-current (DC) sputtering of Zn thin film was employed for seed layer deposition. The sputtered Zn thin film was annealed in air at a temperature of 600 deg C for 60 min for oxidation to obtain a crystalline ZnO seed layer. Scanning Electron Microscopy (SEM) images of the fabricated ZnO NWAs taken shows that the NWs are well aligned with diameters and lengths of (200 ± 53) nm and (1800 ± 99) nm, respectively. This study, therefore, demonstrates the potential for MEMS fabrication of ZnO-based piezoelectric nanogenerator (PENG) on Si substrate. The proposed device, with a measured output voltage of 8 mV for a patterned region when finger-pressed, is intended to be able to provide the power needs for health-care monitoring devices’ application. The demonstration of this concept paves way for the fabrication of a state-of-the-art ZnO-based PENG on a flexible polymer substrate in our future work.

Demonstrating both the intrinsic and extrinsic nature of the giant piezoelectric effect (GPE) in complex solid solutions, near the morphotropic phase boundary, has been extremely challenging until now, because such materials exhibit multiple phases on the order of tens of microns across, meaning important information is lost due to averaging when using established high resolution diffraction techniques to extract three dimensional structural information. We have used a different approach proposed by Nisbet et al. [Acta Crystallogr. Sect. A 71, 20 (2015)], which has been adapted to differentiate between spatially adjacent phases and simultaneously track the evolution of those phases in response to electric fields. As a result, we have identified three environment specific GPEs. The first of these is a GPE which is an order of magnitude greater than previously reported for a given change in field. This is observed during a tetragonal-monoclinic transition in a multiphasic environment. A secondary, large GPE is observed in the neighboring, nontransitioning, monoclinic phase due to stress biasing, and a more typical GPE is observed when the system becomes monophasic. Our results demonstrate the simultaneous and complex interplay of intrinsic and extrinsic factors contributing to the GPE which is likely to have implications for device manufacture and miniaturization.

Combining and coupling both magnetic and electric properties in one single phase multiferroic material has attracted high interest recently to enable a broad range of novel devices and applications. To evaluate one potential route toward new multiferroics, we have studied 0.5% Fe-doped BaTiO3 single crystals and measured the ferroelectric, magnetic, and multiferroic properties. X-ray absorption spectroscopy shows the presence of Fe3+, and magnetic measurements confirmed that this has a significant impact on the magnetic properties. Doping of iron introduces paramagnetism from lone iron atoms as well as what appears to be a weak ferromagnetism. Multiferroicity and magnetoelectric (ME) coupling were observed in the polarization-electric field hysteresis loops with an applied magnetic field, yet there was no direct evidence that ME coupling persists when the sample was in the defect dipole-aligned state.

In this work, we present a grazing incidence X-ray diffraction study of the surface of a 0.24Pb(In1/2Nb1/2)O-3-Pb(Mg1/3Nb2/3)O-3-PbTiO3(PIN-PMN-PT) [011] poled rhombohedral single crystal. The near surface microstructure (the top several tens to hundreds of unit cells) was measured in situ under an applied electric field. The strains calculated from the change in lattice parameters have been compared to the macroscopic strain measured with a strain gauge affixed to the sample surface. The depth dependence of the electrostrain at the crystal surface was investigated as a function of temperature. The analysis revealed hidden sweet spots featuring unusually high strains that were observed as a function of depth, temperature and orientation of the lattice planes.

In this work, we demonstrate that xPb(In1/2Nb1/2)O3-(1-x-y)Pb(Mg1/3Nb2/3)O3-yPbTiO3 [110]-poled domain-engineered relaxor single crystals can be dynamically and reversibly driven through a ferroelectric–ferroelectric phase transition exhibiting a highly enhanced piezoelectric response in a wide range of frequencies. Realization of this phase switching requires an applied compressive stress close to the critical values for the inter-ferroelectric phase transition, which can then be induced by a relatively small electric field (≤0.2 kV/mm). The required critical stress was established by in situ stress and x-ray diffraction measurements. The effective d32 coefficient measured dynamically up to 70 Hz was shown to be consistently twice that of the linear piezoelectric mode measured below the phase transformation region. The crystal was installed into a prototype transducer based on a Tonpilz configuration. The performance of the transducer was tested in water and showed up to 15 dBSPL higher acoustic power radiated when the crystal was driven through the phase transition than when operating in the linear piezoelectric regime.

Multiferroics that simultaneously exhibit ferroelectricity and ferromagnetism have recently attracted great attention due to their potential application in next generation electronic devices. However, only a few single-phase multiferroic materials exhibit ferroelectric and ferromagnetic orders at room temperature. Recently, some bismuth layer-structured Aurivillius compounds were reported as multiferroics at room temperature, but the origin of their magnetic property is still under debate because the net magnetization may originate from the presence of secondary phases that are not easily detected by laboratory XRD diffractometers. Here, textured Aurivillius phase Bi5.25La0.75FeCoTi3O18 ceramics were prepared by Spark Plasma Sintering. The ferromagnetic character of the ceramics was indicated by the magnetic field-induced reversible intensity changes of a certain set of crystalline planes belonging to the Aurivillius phase, as measured by in situ neutron diffraction under the applied magnetic field. The first principles calculations indicate that the ferromagnetism originates from double exchange interactions Fe3+–O–Fe3+, Co3+–O–Co3+, and Fe3+–O–Co3+ in the ferro-toroidal main phase. The magnetic-controlled ferroelectric domain switching was observed by piezoelectric force microscopy at room temperature. The prepared Aurivillius phase ceramics, with Co/Fe contributing to magnetization and polarization at the same time, can be considered an intrinsic room-temperature multiferroic.

A new single phase Aurivillius structured ceramic shows room temperature multiferroic behavior.