A model for the structural hysteresis in poling and thermal depoling of PZT ceramics

A structural hysteresis associated with domain orientation during poling and thermal depoling of lead titanate zirconate (PZT) ceramics has been observed. The poled materials appear to lose their piezoelectric properties at a temperature somewhat below the Curie temperature and yet the domain configurations remain unchanged. The above phenomenon is successfully explained by a model which predicts that upon thermal depolarization, poled ceramics undergo transformation from the poled state into the antiferroelectric state before returning back to their original unpoled state.     

Influence of Electric Poling on Pb0.9Bi0.1Fe0.55Nb0.45O3 Multiferroic

This paper analyzes the influence of electric poling on structure, magnetism, and ferroelectricity by temperature-dependent Raman scattering (180 K–500 K), magnetic susceptibility, and ferroelectric measurements on Pb_0.9Bi_0.1Fe_0.55Nb_0.45O₃ (PBFNO) multiferroic. X-ray diffraction (XRD) has confirmed the monoclinic structure for PBFNO sample before and after poling. Rietveld refined XRD for poled and unpoled sample shows the influence of electric poling on Fe-O1, Fe-O2, Nb–O, and Bi-O modes with small variation in the lattice parameters. The unpoled PBFNO exhibits broad and overlapping 10 active modes at room temperature (100 to 1300 cm^?1) at 147, 212, 255, 431, 479, 561, 700, 795, 835, and 1112 cm^?1. In case of a poled sample, Pb–O and Nb–O-Nb modes become more active compared to the unpoled sample. Changes observed in the temperature-dependent magnetic measurements, i.e., ZFC/FC and M-H loop, evidence the poling effects on Fe–O and Nb–O active modes. By poling the improvement in ferroelectric domain, ordering occurs, and it is confirmed by P-E loops. The consequences of numerous investigations on electric poling of PBFNO will provide the foundation for future device development and design.

     

MSP方法评价PLZT压电陶瓷的强度

采用MSP方法简便有效地评价了氧化物混合法和机械合金化法制备的PLZT压电陶瓷的破坏强度. MA法制备PLZT陶瓷在较低温度下就能烧结致密,具有较好的化学和结构均匀性.相同温度烧结的PLZT陶瓷不仅比MO方法制备的PLZT陶瓷电学性能好,而且破坏强度也更高.PLZT陶瓷经极化后,破坏强度会下降.     

Anisotropic microhardness in single-crystal and polycrystalline BaTiO3

The room-temperature hardness of single-crystal and dense polycrystalline BaTiO₃ was investigated by microindentation. The longer diagonal of the Knoop indenter was oriented either parallel or perpendicular to the poled axis of the material. The hardness of the unpoled sample was isotropic. However, hardnesses in the poled samples were anisotropic, with the highest hardnesses resulting when the longer diagonal was parallel to the poled axis. The hardness anisotropy may be due primarily to residual stresses caused by the piezoelectric coupling effect.     

Scandia—A potential biomaterial?

Biocompatibility is a pre-requisite for all biomaterials used for medical application. During the last two decades significant advances have been made in the development of novel materials and selection and use of these materials has been directly dependent upon their biocompatibility. Several materials containing calcium or titanium cations demonstrate biocompatibility and are routinely used in various forms within the human body. Due to its position in the periodic table, scandium in the form of its oxide scandia (Sc₂O₃) was studied as the first stage of a wider exploration of the biocompatibility of ceramics. A commercial human osteoblast-like cell line (HOS TE 85) was used to study the biocompatibility of both sintered and abraded scandia surfaces. Scanning electron microscopy was used to examine cell adhesion, the MTT assay was used to measure cell metabolic function and the alamarBlue^™ for the assessment of proliferation. Although the results are only preliminary findings, qualitative observations showed that both sintered and abraded surfaces favoured cell adhesion to the same extent. Quantitatively, a significant increase in cell proliferation was observed on Sc₂O₃ compared to Thermanox^™, tissue culture control. Furthermore, Sc₂O₃ has been shown to be non-toxic, able to be maintain cell viability and support cell growth and proliferation.     

Microstructural effects on the phase transitions and the thermal evolution of elastic and piezoelectric properties in highly dense,submicron-structured NaNbO<Subscript>3</Subscript> ceramics

The dielectric, piezoelectric and elastic coefficients, as well as the electromechanical coupling factors, of NaNbO₃ submicron-structured ceramics have been obtained by an automatic iterative method from impedance measurements at resonance. Poled thin discs were measured from room temperature up to the depoling one, close to 300 °C. Dielectric thermal behaviour was determined also for unpoled ceramics up to the highest phase transition temperature. Ceramics were processed by hot-pressing from mechanically activated precursors. Microstructural effects on the properties are discussed. The suppression of the classical maximum in dielectric permittivity in unpoled ceramics at the phase transition at 370 °C was found when a bimodal distribution of grain sizes, with a population of average grain size of 110 nm in between much coarser grains, is observed. The appearance of a phase transition at 150 °C took place when Na vacancies are minimised. The occurrence of a non-centrosymmetric, ferroelectric phase, in the unpoled ceramic from room temperature to ~300 °C, highly polarisable resulting in high ferro–piezoelectric properties was also observed in the ceramic which presents grain size below 160 nm. Maximum values of k _p = 14%, d ₃₁ = −8.7 × 10⁻¹² C N⁻¹ and N _p = 3772 Hz m at room temperature, and k _p = 18%, d ₃₁ = −25.4 × 10⁻¹² C N⁻¹ and N _p = 3722 Hz m at 295 °C were achieved in the best processing conditions of the ceramics.     

Effects of surface-treated cpTi and Ti6Al4V alloy on the initial attachment of human osteoblast cells

This study concerns the effect of simple surface treatments on the nature of the oxide layer, of commercially pure titanium (cpTi) and Ti6Al4V alloy substrates and their effect on human osteoblast cells (HOBS). After treatment the surfaces were analyzed by X-ray photoelectron spectroscopy (XPS) in order to identify the surface groups responsible for the cell attachment process. The assessment of cell attachment was monitored by the Alamar blue assay (AB), measuring cell activity, in three types of media: phosphate-buffered saline (PBS), serum containing and serum-free Dulbecco's modified Eagle's cell culture medium (SER+ and SERF respectively). XPS analysis of the treated surfaces revealed consistent peaks representative of TiO₂ on all surfaces and Ti⁰ and Ti₂O₃ on the non-heat-treated surfaces. The cell activity assays indicated that there were no significant differences in cellular activity caused by surface treatments, but the cellular activity compared between the three types of medium was greatest in the PBS over the initial stages of attachment.     

A Note on Tensile Testing of Poled and Unpoled Piezoelectric Ceramics

Abstract:  Tensile tests were carried out on unpoled and poled soft lead zirconate titanate (PZT) ceramic materials: APC #855 (APC International) and PZT-5H (Morgan Electro Ceramics). The tests were performed on a dog-bone specimen with holes at its edges. A methodology is presented for carrying out these tests. A tensile stress was applied by means of Kevlar strings through the specimen holes. The poling direction was perpendicular to the longitudinal specimen axis. For the poled specimens, two electrical boundary conditions were applied, namely, E  =   0 and D  =   0. Strains were measured at four points on the sample. For each specimen, the bending percentage was calculated. For all specimens, stress–strain curves were found to be initially linear; at a strain of approximately 0.0001, the curves became nonlinear. Young's modulus was measured in the linear region of the stress–strain curve. Young's modulus values were highest for the poled material with an open circuit boundary condition ( D  =   0) and lowest for the unpoled material.     

Field-induced effect in the <111>-oriented 0.70Pb(Mg1/3Nb2/3)O3–0.30PbTiO3 single crystals

Temperature-dependent dielectric constant, X-ray diffraction(XRD), thermally stimulated discharging current (TSDC) and polarization hysteresis loops for <111>-oriented 0.70Pb(Mg_1/3Nb_2/3)O₃–0.30PbTiO₃ crystals after poling under different fields were measured. Comparing with unpoled sample during heating, except that there is a transition from the state of normal ferroelectric rhombohedral (macro-domain) to the state of relaxor ferroelectric rhombohedral (micro-domain) for the poled samples, it was found that no other phase transition was induced by poling fields. XRD showed that after poling the piezoelectric elongation of the unit cell occurred along the polar direction. It was suggested that an extra peak in the T–ε curve of poled sample around 105 °C is not only caused by a macro–micro domain transition but also caused by the depolarization process of 180° and 71° domain switching simultaneously.     

In vitro cellular response to titanium electrochemically coated with hydroxyapatite compared to titanium with three different levels of surface roughness

The in vitro response of primary human osteoblast-like (HOB) cells to a novel hydroxyapatite (HA) coated titanium substrate, produced by a low temperature electrochemical method, was compared to three different titanium surfaces: as-machined, Al₂O₃-blasted, plasma-sprayed with titanium particles. HOB cells were cultured on different surfaces for 3, 7 and 14 days at 37 °C. The cell morphology was assessed using scanning electron microscopy (SEM). Cell growth and proliferation were assessed by the measurement of total cellular DNA and tritiated thymidine incorporation. Measurement of alkaline phosphatase (ALP) production was used as an indicator of the phenotype of the cultured HOB cells. After three days incubation, the electrochemically coated HA surface produced the highest level of cell proliferation, and the Al₂O₃-blasted surface the lowest. Interestingly, as the incubation time was increased to 7 days all surfaces produced a large drop in tritiated thymidine incorporation apart from the Al₂O₃-blasted surface, which showed a small increase. Cells cultured on all four surfaces showed an increased expression of ALP with increased incubation time, although there was not a statistically significant difference between surfaces at each time point. Typical osteoblast morphology was observed for cells cultured on all samples. The HA coated sample showed evidence of a deposited phase after three days of incubation, which was not observed on any other surface. Cells incubated on the HA coated substrate appeared to exhibit the highest number of cell processes attaching to the surface, which was indicative of optimal cell attachment. The crystalline HA coating, produced by a low temperature route, appeared to result in a more bioactive surface on the c.p. Ti substrate than was observed for the other three different Ti surfaces.     

Phase assemblage study and cytocompatibility property of heat treated potassium magnesium phosphate–silicate ceramics

This article reports the study on a new generation bioactive ceramic, based on MgKPO₄ (Magnesium Potassium Phosphate, abbreviated as MKP) for biomedical applications. A series of heat treatment experiments on the slip cast silica (SiO₂) containing MKP ceramics were carried out at 900, 1,000 and 1,100°C for 4 h in air. The density of the slip cast ceramic increases to 2.5 gm/cm³ upon heat treatment at 900°C. However, no significant change in density is measured upon heat treatment to higher temperature of 1,000 and 1,100°C. On the basis of XRD results, the presence of K₂MgSi₅O₁₂ and dehydrated MgKPO₄ were confirmed and complementary information has also been obtained using FT-IR and Raman spectroscopy. In order to confirm the in vitro cytocompatibility property, the cell culture tests were carried out on selected samples and the results reveal good cell adhesion and spreading of L929 mouse fibroblast cells. MTT assay analysis with L929 cells confirmed non-cytotoxic behavior of MKP containing ceramics and the results are comparable with sintered HAp ceramics. It is expected that the newly developed MKP based materials could be a good substitute for hydroxyapatite (HAp or HA) based bioceramics.     

Studies on electrical conduction in Bi4SrTi4O15

The ferroelectric Bi₄SrTi₄O₁₅ has been synthesized and a study of the electrical (AC) conductivity was made on both poled and unpoled samples in the frequency range from 100 Hz to 1 MHz and from room temperature to 550°C. In the case of unpoled samples the activation energy was found to be 0·54 eV and subsequent to poling it was lowered to 0·39 eV indicating an increased conductivity after poling. Further the conductivity increased with increasing frequency and temperature. DC conductivity measurements were also carried out. Dielectric measurements indicate a peak in the dielectric constant at 530°C.     

Piezoelectric properties of sol-gel-derived samarium-dysprosium-modified lead titanate ceramics

Samarium- and dysprosium-modified lead titanate ceramics have been prepared by a sol-gel route to utilize the finer control of the process on homogeneity and microstructure. By varying the sintering schedule (temperature and time) for samarium-modified PbTiO₃, ceramics with grain sizes ranging from submicrometre to 4 m have been prepared. The dielectric and piezoelectric properties of ceramics poled sequentially from 0 to 60 kV cm^–1 are reported. The dependence of the electromechanical properties on grain size and poling conditions is discussed. It is shown that dysprosium behaves very differently to samarium, and the successful insertion of dysprosium into the Pb²⁺ sites to produce true dysprosium-modified PbTiO₃ ceramics was not possible.     

On fracture testing of piezoelectric ceramics

Fracture tests carried out on unpoled and poled PZT-5H four-point bend specimens are presented in this paper. The crack faces were parallel to the poling direction. Both mechanical loads and electric fields were applied to the poled specimens. The experimental results were analyzed by means of the finite element method and a conservative M-integral including the crack face boundary conditions. Fracture tests on four-point bend PIC-151 specimens with the crack faces perpendicular to the poling directions were also analyzed here; the experimental results were taken from the literature. A mixed mode fracture criterion is proposed for piezoelectric ceramics. This criterion is based upon the energy release rate and two phase angles. This criterion was implemented with experimental results from the literature and from this investigation. Excellent agrement was found between the fracture curve and the experimental results of the specimens with the crack faces perpendicular to the poling direction. With some scatter, reasonable agreement was observed between the fracture curve and the experimental results of the specimens with crack faces parallel to the poling direction.     

Hydroxyapatite/SiO2 Composites via Freeze Casting for Bone Tissue Engineering

Freeze casting is a fabrication method that allows producing near‐net‐shaped ceramics with variable porosity. Hydroxyapatite (HA) was modified by the addition of different amounts of SiO₂ nanoparticles during freeze cast preparation. The addition of SiO₂ introduced a partial phase transformation of HA to β‐tricalcium phosphate and improved the form stability due to less shrinkage after sintering. The impact of surface roughness of pure HA ceramics and the influence of SiO₂ introduction during freeze casting on adhesion, proliferation, and differentiation of human osteoblast‐like cells (MG‐63) was investigated. While both cell attachment and proliferation of smooth pressed HA was significantly enhanced compared to rough freeze cast HA, the addition of SiO₂ improved the cell numbers of the latter. The expression of cell differentiation markers osteocalcin and collagen I was found to be supported by rough surfaces (R_a = 5–6 µm) in particular on ceramics containing SiO₂     

Effective diffraction gratings via acidic etching of thermally poled glass

Relief diffraction gratings are formed via acidic chemical etching of a periodically poled soda-lime glass. The thermal poling under 1000 V DC is performed at 325 °C using a thermally stable glassy-carbon anodic electrode with periodic grooves, the depth of the grooves being of ∼650 nm. Poling-induced modification of the glass results in deepening the glass anodic surface in the regions under the ribs of the anodic electrode due to volume relaxation and in increasing chemical durability of these regions in acidic media comparatively to the virgin glass. Chemical etching of the poled glass in NH₄F:8H₂O solution allows additional to the thermal poling shaping of the glass surface via faster dissolution of unpoled/less poled glass regions. The morphology of the glass surface before and after the etching is characterized with atomic force and scanning electron microscopy. About 30 min etching provides the formation of ∼0.9 μm in height relief diffraction gratings with the diffraction efficiency close to the theoretically achievable ∼30% for multi-order diffraction. In vivo measuring of the diffraction efficiency in the course of the etching allows precise fabrication of the gratings.     

Poling and properties of nano-composite thin film PT/PEK-C

The composite thin films of PT nanometer particles and high transparent polymer PEK-C were prepared. The poling conditions that PT particles in composites are aligned under external electric field was optimized through the dielectric properties of PT and PEK-C polymer and effective field intensity theory. Through the X-ray diffraction of poled composite thin film, it was obtained that the c axis orientation ratio of nano-crystal PbTiO₃ was calculated to be 68%. The transparency spectra in the range 380–900 nm was measured. The optical band-gaps of poled and unpoled composite thin films were estimated to be 3.14 and 3.06 eV, respectively.     

基于压电效应的人工耳蜗的实验研究

为了提高聋耳的听力, 将压电材料植入到耳蜗内, 利用压电效应直接将声波转化为电信号刺激听神经, 以提高听力. 本研究通过未极化与极化的高灵敏性压电陶瓷的对比, 从体外模拟实验中的声电响应曲线和动物体内植入实验的结果中得到: 未极化的压电陶瓷没有压电响应, 而极化后的压电陶瓷能够将声音信号转化为电信号, 证实了压电陶瓷的压电特性的确可以刺激动物的听神经, 从而降低听阈阈值. 比较了压电陶瓷与压电高分子之间的差异, 结果表明压电高分子也可以刺激听神经来提高听力.     

Polycrystalline secondary ferroics

Domain walls in secondary ferroics can be displaced by electric fields, magnetic fields, mechanical stresses, or by some combination of the three. The expected physical properties of fully “poled” secondary ferroics are calculated and compared with those of the unpoled polycrystalline material, and with available experimental evidence. The effects of poling are most obvious for null properties such as piezoelectricity and magnetoelectricity, which depend entirely on domain alignment. Experiments on NH₄Cl provide the first demonstration of ferroelastoelectric “poling” in a polycrystalline material; piezoelectricity appears after annealing at ?30°C in parallel electric fields and mechanical stress. Other examples of “poled” polycrystalline secondary ferroics include ferromagnetoelectric Cr₂O₃, ferrobielastic SiO₂, and ferrobimagnetic MnO.     

Biofunctionalization strategies on tantalum-based materials for osseointegrative applications

The use of tantalum as biomaterial for orthopedic applications is gaining considerable attention in the clinical practice because it presents an excellent chemical stability, body fluid resistance, biocompatibility, and it is more osteoconductive than titanium or cobalt-chromium alloys. Nonetheless, metallic biomaterials are commonly bioinert and may not provide fast and long-lasting interactions with surrounding tissues. The use of short cell adhesive peptides derived from the extracellular matrix has shown to improve cell adhesion and accelerate the implant’s biointegration in vivo. However, this strategy has been rarely applied to tantalum materials. In this work, we have studied two immobilization strategies (physical adsorption and covalent binding via silanization) to functionalize tantalum surfaces with a cell adhesive RGD peptide. Surfaces were used untreated or activated with either HNO₃ or UV/ozone treatments. The process of biofunctionalization was characterized by means of physicochemical and biological methods. Physisorption of the RGD peptide on control and HNO₃-treated tantalum surfaces significantly enhanced the attachment and spreading of osteoblast-like cells; however, no effect on cell adhesion was observed in ozone-treated samples. This effect was attributed to the inefficient binding of the peptide on these highly hydrophilic surfaces, as evidenced by contact angle measurements and X-ray photoelectron spectroscopy. In contrast, activation of tantalum with UV/ozone proved to be the most efficient method to support silanization and subsequent peptide attachment, displaying the highest values of cell adhesion. This study demonstrates that both physical adsorption and silanization are feasible methods to immobilize peptides onto tantalum-based materials, providing them with superior bioactivity.