Search Results (44)

In the present manuscript, the influence of reaction time on the hexagonal-to-monoclinic phase transition in hydroxyapatite (HAp) nanofibers synthesized via a low-temperature modified hydrothermal method at 100 °C is investigated. The resulting nanofibers were highly crystalline and stoichiometric, with a Ca/P ratio of approximately 1.67. Comprehensive structural and functional characterization, combining X-ray diffraction with Rietveld refinement, Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, transmission electron microscopy (TEM), and resonance-tracking piezoresponse force microscopy (RT-PFM), was employed to elucidate the role of the non-centrosymmetric monoclinic P2₁/b phase in governing HAp’s structural and piezoelectric properties. The analyses indicated a time-dependent phase evolution from hexagonal (P6₃/m) to monoclinic (P2₁/b), with exclusive formation of the hexagonal phase at 6 h and a clearly dominant monoclinic fraction (73.56%) after 24 h. Nanofibers synthesized for 48 h comprised approximately 98% monoclinic HAp and exhibited elongated morphologies with an average length of 354.82 nm and diameter of 45 nm. RT-PFM measurements confirmed a pronounced piezoelectric response associated with the monoclinic phase, yielding an effective piezoelectric coefficient (d_eff) of 19.85 pm/V. In vitro MTT assays demonstrated that the high monoclinic content did not compromise biocompatibility, as cell viability and cytotoxicity met the requirements of ISO 10993 and ASTM F895 standards. These findings offer new insights into how monoclinic ordering governs the piezoelectric behavior of HAp and suggest a promising strategy for enhancing its performance in biomedical applications. Full article

Lead-free transparent ferroelectric ceramics with integrated opto-electro-mechanical functionalities are pivotal for next-generation multifunctional devices. In this study, K_0.48Na_0.52NbO₃-xLa₂O₃ (KNN-xLa, x = 0.005 − 0.04) ceramics were fabricated via a conventional solid-state route to investigate the La³⁺-induced multiscale structural evolution and its modulation of optical and electrical properties. La³⁺ substitution drives a critical structural transition from an anisotropic orthorhombic phase (Amm2) to a high-symmetry pseudocubic-like tetragonal phase (P4mm) for x ≥ 0.025, characterized by minimal lattice distortion (c/a = 1.0052). This enhanced structural isotropy, coupled with submicron grain refinement (<1 μm) driven by ${\mathrm{V}}_{\mathrm{A}}^{\prime }$-mediated solute drag, effectively suppresses light scattering. Consequently, a high-transparency plateau (T₇₈₀ ≈ 53–58%, T₁₇₀₀ ≈ 70–72%) is achieved for 0.025 ≤ x ≤ 0.035. Simultaneously, the system undergoes a crossover from normal ferroelectric (FE) to relaxor (RF) state, governed by an FE–RF boundary at x = 0.015. While x = 0.005 exhibits robust piezoelectricity (d₃₃ ≈ 92 pC/N), the x = 0.015 composition facilitates a transitional polar state with large strain (0.179%) and high polarization (P_m ≈ 33.3 μC/cm², P_r ≈ 15.8 μC/cm²). Piezoresponse force microscopy (PFM) confirms the domain evolution from lamellar macro-domains to speckle-like polar nanoregions (PNRs), elucidating the intrinsic trade-off between optical transparency and piezoelectricity. This work underscores La³⁺ as a potent structural modifier for tailoring phase boundaries and defect chemistry, providing a cost-effective framework for developing high-performance transparent electromechanical materials. Full article

This paper considers the uniaxial orientation effect on the structure and piezoelectric properties of vinylidene fluoride-tetrafluoroethylene copolymer ferroelectric films. The films were exposed to uniaxial orientation stretching in a temperature range from 20 °C to 60 °C; then, they were contact polarized under normal conditions. The temperature dependence of the electric strength was determined. The longitudinal piezoelectric coefficient d₃₃ values were measured by the quasi-static Berlincourt method. The piezoresponse force microscopy (PFM) method was used to investigate the film domain structure before and after polarization, and the local piezoelectric coefficient values were also calculated. Phase composition was studied using differential scanning calorimetry and infrared spectroscopy with the Fourier transform. It was found that uniaxial orientation stretching contributed to an increase in the piezoelectric coefficient d₃₃ from 5 pC/N to 16–20 pC/N. The results obtained indicate the importance of the amorphous phase contribution to the formation of the piezoelectric properties in polymeric materials. Full article

Bone regeneration demands biomaterials capable of supporting tissue integration and mimicking the native piezodynamic properties of bone. In this study, hydroxyapatite–barium titanate (HA-BT) composite coatings with varying BT content (10, 30, and 50 wt%) were developed to enhance the piezoelectric response and corrosion resistance of Ti6Al4V implants. The coatings were synthesized via high-energy ball milling and atmospheric plasma spraying (APS). XRD analysis with Rietveld refinement confirmed the presence of HA along with secondary phases (TTCP, β-TCP, CaO). Electrochemical tests revealed lower corrosion current densities for the coatings containing ≤30% BT, indicating improved stability in physiological environments. Cytotoxicity assays (MTT) demonstrated biocompatibility across all formulations. Piezoresponse force microscopy (DART-SS-PFM) confirmed enhanced d₃₃-eff values for the 50% BT coating (>15 pm/V); however, biological assays under low-intensity pulsed ultrasound (LIPUS) stimulation showed increased osteocalcin expression for ≤30% BT, while 50% BT induced cellular stress. Overall, HA-BT coatings with up to 30% BT exhibited optimal electrochemical stability, favorable piezoelectric performance, and enhanced biological response, underscoring their potential for orthopedic implant applications and regenerative tissue engineering. Full article

Porous PZT films offer significant potential due to tunable electromechanical properties, yet the polarization behavior remains insufficiently understood because of discontinuous morphology and domain structures. In this work, we study the impact of porosity on the spontaneous polarization and electromechanical response of PZT thin films fabricated using a multilayer spin-coating technique with various concentrations (0–14%) of polyvinylpyrrolidone (PVP) as a porogen. Atomic force microscopy (AFM) and piezoresponse force microscopy (PFM) were employed to analyze the local topography, domain distribution, and polarization behavior of the films. The results indicate that increasing porosity leads to substantial changes in grain morphology, dielectric permittivity, and polarization response. Films with higher porosity exhibit a more fragmented polarization distribution and reduced piezoresponse, while certain orientations demonstrate enhanced domain mobility. Despite the decrease in overall polarization, the local coercive field remains relatively stable, suggesting structural stability during the local polarization switching. The findings highlight the crucial role of grain boundaries and local charge redistribution in determining local polarization behavior. Full article

This paper investigates the synthesis and characterization of eco-friendly piezoelectric composite thin films composed of chitosan and Ln₂O₃-doped Na_0.5Bi_0.5TiO₃-BaTiO₃ (NBT-BT) nanoparticles. The films were fabricated using a solution-casting technique, successfully embedding the particles into the chitosan matrix, which resulted in enhanced piezoelectric properties compared to pure chitosan. Characterization methods, such as photoluminescence spectroscopy and piezo-response force microscopy (PFM) which revealed strong electromechanical responses, with notable improvements in piezoelectric performance due to the inclusion of NBT-BT nanoparticles. X-ray diffraction (XRD) analysis revealed a pure perovskite phase with the space group R3c for NBT-BT and NBT-BT-Ln particles. Scanning electron microscopy (SEM) images showed a non-uniform distribution of NBT-BT particles within the chitosan matrix. The results also suggest that the incorporation of rare earth elements further enhances the electrical and piezoelectric properties of the composites, highlighting their potential in flexible and smart device applications. Overall, these findings underscore the potential of chitosan-based composites in addressing environmental concerns while offering effective solutions for energy harvesting and biomedical applications. Full article

The study of the properties of ferroelectric materials against irradiation has a long history. However, anti−irradiation research on the ferroelectric domain has not been carried out. In this paper, the irradiation of switched domain structure is innovatively proposed. The switched domain of 700 nm lithium niobate (LiNbO₃, LN) thin film remains stable after gamma irradiation from 1 krad to 10 Mrad, which was prepared by piezoresponse force microscopy (PFM). In addition, the changing law of domain wall resistivity is explored through different sample voltages, and it is verified that the irradiated domain wall conductivity is still larger than the domain. This domain wall current (DWC) property can be applied to storage, logic, sensing, and other devices. Based on these, a ferroelectric domain irradiation resistance model is established, which explains the reason at an atomic level. The results open a possibility for exploiting ferroelectric materials as the foundation in the application of space and nuclear fields. Full article

Quantitative converse piezoelectric coefficient (d₃₃) mapping of polymer ultrafine fibers of poly(acrylonitrile) (PAN), as well as of poly(vinylidene fluoride) (PVDF) as a reference material, obtained by rotating electrospinning, was carried out by piezoresponse force microscopy in the constant-excitation frequency-modulation mode (CE-FM-PFM). PFM mapping of single fibers reveals their piezoelectric activity and provides information on its distribution along the fiber length. Uniform behavior is typically observed on a length scale of a few micrometers. In some cases, variations with sinusoidal dependence along the fiber are reported, compatibly with a possible twisting around the fiber axis. The observed features of the piezoelectric yield have motivated numerical simulations of the surface displacement in a piezoelectric ultrafine fiber concerned by the electric field generated by biasing of the PFM probe. Uniform alignment of the piezoelectric axis along the fiber would comply with the uniform but strongly variable values observed, and sinusoidal variations were occasionally found on the fibers laying on the conductive substrate. Furthermore, in the latter case, numerical simulations show that the piezoelectric tensor’s shear terms should be carefully considered in estimations since they may provide a remarkably different contribution to the overall deformation profile. Full article

This paper presents data on the macroscopic polarization of copolymer films of vinylidene fluoride with tetrafluoroethylene obtained with a modified apparatus assembled according to the Sawyer–Tower Circuit. The kinetics of the polarization process were analyzed taking into consideration the contributions of both bound and quasi-free (impurity) charges. It was shown that an “abnormal” decrease in conductivity was observed in fields near the coercive fields. This could be associated with the appearance of deep traps of the impurity charge carriers formed by the polar planes of β-phase crystals. The conductivity data obtained from the charge and current responses differed. It was concluded that chain segments contributing to polarization with sufficiently low fields were present in the amorphous phase. A comparison showed that the average size of β-phase crystals (crystals of X-ray diffraction reflection width) was almost one order of magnitude lower than the domain size obtained using piezoresponse force microscopy (PFM). The analysis of the fast-stage dielectric response before and after polarization indicated that as the external polarizing field increased in the ferroelectric polymer chains, conformational transitions occurred according to the T₃GT₃G⁻ → (-TT-)_n и TGTG → (-TT-)_n types. This was accompanied by an increase in the effective dipole moment in the amorphous phase chains. The analysis of the IR spectroscopy data obtained in transmission and ATR modes revealed a difference in the conformational states of the chains in the core and surface parts of the film. Full article

Bi₂Se₃, one of the most extensively studied topological insulators, has received significant attention, and abundant research has been dedicated to exploring its surface electronic properties. However, little attention has been given to its piezoelectric properties. Herein, we investigate the piezoelectric response in a five-layer Bi₂Se₃ nanosheet using scanning probe microscopy (SPM) techniques. The piezoelectricity of Bi₂Se₃ is characterized using both conventional piezoresponse force microscopy (PFM) and a sequential excitation scanning probe microscopy (SE-SPM) technique. To confirm the linear piezoelectricity of Bi₂Se₃ two-dimensional materials, measurements of point-wise linear and quadratic electromechanical responses are carried out. Furthermore, the presence of polarization and relaxation is confirmed through hysteresis loops. As expected, the Bi₂Se₃ nanosheet exhibits an electromechanical solid response. Due to the inevitable loss of translational symmetry at the crystal edge, the lattice of the odd-layer Bi₂Se₃ nanosheet is noncentrosymmetric, indicating its potential for linear piezoelectricity. This research holds promise for nanoelectromechanical systems (NEMS) applications and future nanogenerators. Full article

The functional role of collagen piezoelectricity has been under debate since the discovery of piezoelectricity in bone in 1957. The possibility that piezoelectricity plays a role in bone remodeling has generated interest in the investigation of this effect in relevant physiological conditions; however, there are conflicting reports as to whether collagen is piezoelectric in a humid environment. In macroscale measurements, the piezoelectricity in hydrated tendon has been shown to be insignificant compared to dehydrated tendon, whereas, at the nanoscale, the piezoelectric effect has been observed in both dry and wet bone using piezoresponse force microscopy (PFM). In this work, the electromechanical properties of type I collagen from a rat tail tendon have been investigated at the nanoscale as a function of humidity using lateral PFM (LPFM) for the first time. The relative humidity (RH) was varied from 10% to 70%, allowing the piezoelectric behavior to be studied dry, humid, as well as in the hydrated range for collagen in physiological bone (12% moisture content, corresponding to 40–50% RH). The results show that collagen piezoresponse can be measured across the humidity range studied, suggesting that piezoelectricity remains a property of collagen at a biologically relevant humidity. Full article

We successfully synthesized millimeter-sized single crystals of the molecular erbium(III) complex Er(acac)₃(cphen), where acac = acetylacetonate and cphen = 5-chloro-1,10-phenanthroline. The novelty of this work stems from the exhaustive examination of the polar and electronic properties of the obtained samples at the macro-, micro-, and nanoscale levels. The single crystal X-ray diffraction method demonstrates the monoclinic (noncentrosymmetric space group P2₁) crystallographic structure of the synthesized samples and scanning electron microscopy exhibits the terrace–ledge morphology of the surface in erbium(III) crystals. By using the piezoelectric force microscopy mode, the origin of the polar properties and the hyperpolarizability in the synthesized samples were assigned to the internal domain structure framed by the characteristic terrace–ledge topography. The direct piezoelectric coefficient (~d33) was found to be intensely dependent on the local area and was measured in the range of 4–8 pm/V. A nanoscale study using the kelvin probe force and capacitance force (dC/dz) microscopy modes exposed the effect of the Er ions clustering in the erbium(III) complex. The PFM method applied solely to the Er ion revealed the corresponding direct piezoelectric coefficient (~d33) of about 4 pm/V. Given the maximum piezoelectric coefficient in the erbium(III) complex at 8 pm/V, we highlight the significant importance of the spatial coordination between the lanthanide ion and the ligands. The polar coordination between the lanthanide ion and the nitrogen and oxygen atoms was also corroborated by Raman spectroscopy supported by the density functional theory calculations. The obtained results can be of paramount importance for the application of molecular erbium(III) complex crystals in low-magnitude magnetic or electric field devices, which would reduce the energy consumption and speed up the processing switching in nonvolatile memory devices. Full article

This work addresses the global sustainable development concerns by investigating the enhancement of piezo-photocatalytic efficiency in bismuth ferrite-based thin films synthesized using reactive high-power impulse magnetron sputtering. The influence of substrate type and Cr addition on structural, optical and ferroelectric properties of bismuth ferrite (BFO) based thin films was investigated. X-ray diffraction measurements showed the formation of different phases depending on the substrate used for sample growth. Compared to the BFO film deposited on FTO (F-SnO₂), the Cr-doped BFO (BFCO) sample on SrTiO₃ (STO) exhibits higher photodegradation efficiency (52.3% vs. 27.8%). The enhanced photocatalytic activity of BFCO is associated with a lower energy band gap (1.62 eV vs. 1.77 eV). The application of ultrasonic-wave vibrations simultaneously with visible light improved 2.85 times and 1.86 times the photocatalytic degradation efficiencies of BFO/FTO and BFCO/STO catalysts, respectively. The piezoresponse force microscopy (PFM) measurements showed that both catalysts exhibit ferroelectric behavior, but a higher piezoelectric potential was evidenced in the case of the BFO/FTO thin film. The enhancement of piezo-photodegradation efficiency was mainly attributed to the piezoelectric-driven separation and transport of photo-generated carriers toward the surface of the photocatalyst. Full article

Over recent decades, the scientific community has managed to make great progress in the theoretical investigation and practical characterization of bismuth ferrite thin films. However, there is still much work to be completed in the field of magnetic property analysis. Under a normal operational temperature, the ferroelectric properties of bismuth ferrite could overcome the magnetic properties due to the robustness of ferroelectric alignment. Therefore, investigation of the ferroelectric domain structure is crucial for functionality of any potential devices. This paper reports deposition and analyzation of bismuth ferrite thin films by Piezoresponse Force Microscopy (PFM) and XPS methods, aiming to provide a characterization of deposited thin films. In this paper, thin films of 100 nm thick bismuth ferrite material were prepared by pulsed laser deposition on multilayer substrates Pt/Ti(TiO₂)/Si. Our main purpose for the PFM investigation in this paper is to determine which magnetic pattern will be observed on Pt/Ti/Si and Pt/TiO₂/Si multilayer substrates under certain deposition parameters by utilizing the PLD method and using samples of a deposited thickness of 100 nm. It was also important to determine how strong the measured piezoelectric response will be, considering parameters mentioned previously. By establishing a clear understanding of how prepared thin films react on various biases, we have provided a foundation for future research involving the formation of piezoelectric grains, thickness-dependent domain wall formations, and the effect of the substrate topology on the magnetic properties of bismuth ferrite films. Full article

The (001) plate-like BaTiO₃ piezoelectric micromaterials are synthesized by topochemical microcrystal conversion technique. BaTiO₃ plates with a length of 2~10 μm and thickness of 0.5~1.3 μm are obtained. The dependence of morphology on synthesis conditions is discussed in detail. The crystal symmetry and multiscale domain structures of BaTiO₃ plates are systematically investigated by various characterizations. X-ray diffraction (XRD) and Raman spectra analyses demonstrate the tetragonal symmetry of the (001) oriented BaTiO₃ plates at room temperature. The domain configurations of the micron BaTiO₃ are investigated with a polarized light microscope (PLM) and piezoresponse force microscopy (PFM). The single-crystal-like quality and uniformity are supported by PLM observations. More importantly, the classical 90° banded ferroelectric domains of ~125 nm width are observed for the first time in such BaTiO₃ plates. The domain features in the mesoscale BaTiO₃ plate are discussed and compared with its bulk counterparts. The results may provide insights into understanding and designing the mesoscale BaTiO₃ functional materials. Full article