Poling Conditions of Pre-Stressed Piezoelectric Actuators and Their Displacement

The poling procedure has always been the key issue in producing piezoelectric actuators with optimised performance. This is also true with the relatively new category of pre-stressed bender actuators, where mechanical bias achieved with a passive layer is introduced in the actuators during manufacturing. Due to these factors, the behaviour of the actuator under poling is different compared to its bulk counterparts. In this paper, two different thicknesses of commercial PZT 5A and PZT 5H materials were used in bulk actuators and pre-stressed benders realised by new method. Pre-stress was introduced by using a post-fired biasing layer utilising sintering shrinkage and difference in thermal expansion. The hysteresis loop of the actuators was measured under 0.5–7.0 MV/m electric fields at 25–125^∘C temperatures, providing information about their remnant polarisation and coercive field before poling. The results showed that high electric field and 25^∘C temperatures in poling provided higher remnant polarisation and coercive electric field than using 125^∘C temperature at poling. Difference was especially significant in coercive electric field values where up to 114.8% difference was obtained for PZT 5H bulk actuator and 65.9% for pre-stressed actuators. Higher coercive fields can be utilized as increased operating voltage range of piezoelectric devices. The differences in results obtained here and by others can be explained by the different pre-stress level, stronger clamping of the thicker passive layers of the RAINBOW and THUNDER actuators and passive ring area introducing high tensile stresses. The same conditions were used to pole the actuators, after which the displacement and dielectric constant of the actuators were measured. The displacement measurements showed that remnant polarisation has good correlation with displacement. This fact can be used in estimating pre-stressed actuator performance before actual poling. The dielectric constant measurements with a small signal after poling gave even better correlation than the remnant polarisation.     

Preparation and Characterization of PZT films Fabricated on Si Substrate

Lead zirconium titanate (PZT) films (Zr/Ti=45:55) with a high dielectric constant are prepared successfully on the low-resistance Si substrate in sol–gel dip-coating process with PT film used as the buffer layer. The dielectric and ferroelectric properties of the films as well as the relationship between crystallization and preparing condition are studied. It is shown that the PZT ferroelectric thin films with a (110) preferred orientation and a well-crystallized perovskite structure could be obtained after annealing at 800°C for 15 min. The particle size of the sample is about 14–25 nm. The P–E hysteresis loops are measured by means of the Sawyer-Tower test system with a compensation resistor at room temperature. The remanent polarization (P _r) and coercive electric field (E _c) of the measured PZT thin films are 47.7 μC/cm² and 18 kV/cm, respectively. The relative dielectric constant ε _r and the dissipation factor tgδ of the PZT thin films were measured with an LCR meter and were found to be 158 and 0.04–0.005, respectively. Translated from “Preparation and Characterization of PZT Films Fabricated on Si Substrates” published in Chinese Journal of Semiconductors, 2004, 25(4): 404–409 (in Chinese)     

Characteristics of ferroelectric gate mos and mosfets

Abstract

Electrical characteristics of metal-insulator-semiconductor (MIS) capacitors of a variety of ferroelectric materials like lead zirconate titanate (PZT), lead titanate (PT) and barium magnesium fluoride (BMF) on p-silicon have been studied. PZT was deposited by r.f. magnetron sputtering from a composite target and PT from co-evaporation. The films were annealed in oxygen atmosphere in the temperature range 550–700°C for various times. PZT and PT films which are directly deposited on silicon showed low effective dielectric constant.¹⁰ For normal applied bias voltages (±5 V), the C-V curves did not show significant hysteresis. The effective dielectric constant was improved significantly by the incorporation of a buffer layer. BMF film was deposited in ultra high vacuum on a heated substrate and the film was encapsulated by a zirconium oxide layer. The C-V curves for these MIS capacitors shows hysteresis and the direction of hysteresis corresponds to ferroelectric polarization.     

Water-Immersible Micromachined Pb(Zr, Ti)O3 Thin Film Actuators

We demonstrate a water-immersible thin film lead zirconate titanate, Pb(Zr, Ti)O₃, [PZT] actuator, without special passivation layer, towards in-vivo or in-vitro scanning probe microscope (SPM) measurements of living cells in water or biological fluids. In order to be water-immersible, the electrodes need to be electrically insulated and the piezoelectric layer needs to be protected against direct water contact. This paper describes our design solution with a simple fabrication process for a water-immersible piezoelectric device, which separates the bottom electrode from the top electrode by having a narrow ditch covered with PZT film. The PZT film is then encapsulated with the top metal electrode without insulation layer. In this structure, the PZT is sandwiched between the top and bottom metal electrodes to prevent water permeation. The device is fabricated using lift-off processing for the bottom and top electrodes, sol-gel spinning for the PZT thin film and wet etching for the PZT patterning. The piezoelectric constant, d₃₁, is about –100 pC/N. The dielectric polarization and fatigue properties of the devices were measured in air and water. The spontaneous polarization, remnant polarization, coercive field and dielectric constant are 54 C/cm², 15 C/cm², 60 kV/cm and 1200, respectively. The polarization property of the device was unchanged in either air or water up to 1 × 10⁹ continuous cycles.     

EFFECTS OF PZT BUFFER LAYERS ON PZFNT FERROELECTRIC THIN FILMS

ABSTRACT

PZFNT thin films were fabricated on 5-inch Pt/Ti/SiO₂/Si and PZT/Pt/Ti/SiO₂/Si substrates by RF magnetron sputtering method and rapid thermal annealing process. By investigating the two thin films at various annealing temperatures, the results show that the annealing temperature of PZFNT thin films without PZT buffer layers is about 730°C, which is higher than that of PZFNT films with PZT buffer layers. By use of PZT buffer layers, the annealing temperature of PZFNT films is decreased greatly, and the dielectric and ferroelectric properties are improved. In the optimum process, the thin films with PZT buffer layers have a dielectric constant of 1199 and dielectric loss of 3.0% at 1 KHz. The remanent polarization and coercive field of the thin films are 21.1 μC/cm² and 53.5 KV/cm respectively. The films have the significant potential for FRAM and pyroelectric infrared detectors.     

Effect of Nb doping on structural and electric properties of PZT (65/35) ceramic

The aim of this study is to determine the effect of Nb⁵⁺ doping on PZT (65/35) based bulk materials in their structure, micro structure and electrical properties. The Nb content was chosen 0-9 mole%. These materials were prepared by conventional mixed oxide method. X ray diffraction studies suggest the compound to be of rhombohedral perovskite phase. Excess addition of Nb result in pyrochlore and fluorite phase develops in PZT (65/35) sample. Detailed studies of dielectric constant as a function of temperature (40degC to 500degC) and frequency (100 Hz to 1 MHz) suggest that the compounds undergo diffuse type of phase transition. Maximum dielectric constant and resistivity were found to be strongly dependent on doping and measuring frequencies. Using complex impedance analysis micro structural parameters such as bulk and grain boundary resistance, bulk charge carrier concentration and relaxation time were determined     

Preparation and characteristics of fine-grained ferroelectric glass-ceramic composites via a modified hybrid route at low temperature sintering

Dense, homogeneous and fully developed fine-grained ferroelectric Pb(Zr_0.53Ti_0.47)O₃?Cbased glass-ceramics have been successfully prepared at a low-sintering temperature of 850?C900°C by a modified hybrid process in air. The influence of the PbO-B₂O₃-SiO₂ (abbreviated as PBS) glass-gel content on the microstructure, dielectric, and ferroelectric properties of such glass-ceramics has been investigated. The temperature dependence of the dielectric constant indicated that the fine-grained Pb(Zr_0.53Ti_0.47)O₃ (abbreviated as PZT(53/47)) based glass-ceramic shows the characteristic dispersion at the Curie point. Ferroelectric hysteresis loop analyses have been performed to manifest the ferroelectric nature of the highly crystallized PZT(53/47) phase prepared by this modified novel hybrid process despite containing higher wt% glass-gel contents. The best dielectric and ferroelectric properties in a typical sample with 5% by weight of glass-gel content were found to have dielectric constant and loss tangent of 920 and 0.02 at 1 kHz, respectively. The saturation polarization (P _s ), and remanent polarization (P _r ) as well as the coercive field (E _c ) are 21.9 ??C/cm², 10.8 ??C/cm² and 2.19 kV/mm, respectively.     

Effect of Nb Doping on (Sr,Ba)TiO3 (BST) Ceramic Samples

The effect of doping the Sr_0.3Ba_0.7Ti_(1–5y/4)Nb _y O₃ ceramic with different concentration of Nb is studied by scanning electron microscopy (SEM), X-ray diffraction and thermoelectric analysis. It is observed that the grain size decreases as the Nb concentration increases. The critical temperature T _c has a linear decrease at a rate of 19°C/mol% of Nb. The temperature dependence of the dielectric permittivity presents strongly broadened curves, which suggest a non Curie-Weiss behavior near the transition temperature. The diffuse phase transition coefficient () was also determined and its value leads to the conclusion that the degree of disorder in the system increases with the presence of the Nb cation.     

Scaling Effect on the Dielectric Constant in Ba(Ti x Zr1−x )O3 Thin Films

Recent work on PZT and BST thin films reveal a thickness dependence of the dielectric constant for a film thickness below 100 nm. This effect is commonly attributed to an interfacial layer between the electrode and the dielectric film (dead layer). In this contribution we report on the influence of the film thickness on the dielectric constant of Ba(Ti_xZr_{1 – x})O₃ thin films with different Zr-contents (x = 0–30 at.%). The films were prepared by chemical solution deposition (CSD) with thickness between 30 and 350 nm.The electrical characterization was performed in a temperature range between 25 and 200C. Results were interpreted with respect to the formation of a serial dead layer capacitance.     

Tunability and Calculation of the Dielectric Constant of Capacitor Structures with Interdigital Electrodes

The voltage dependence of the dielectric constant of ferroelectricmaterials makes them attractive for use as tuning elements in microwavecircuits. In this study, capacitance tuning and loss measurements wereperformed on ferroelectric materials prepared by the sol-gel process and RFmagnetron sputtering. We find that Pb(Zr,Ti)O₃ (PZT) thinfilms with interdigital electrodes can be fabricated with reasonably lowloss to make them useful for room temperature tuning applications. Inaddition, it is found that high temperature post-deposition annealing ofboth sputtered SrTiO₃ (ST) and sol-gel derivedBaTiO₃ (BT) films markedly improves their tuning and lossfactor characteristics. By annealing the samples in the range of1000–1100°C, the tunability was increased by as much as a factorof seven, while the dissipation factors were decreased to values of0.3–0.5%. In addition, it is shown that the permittivity of thefilms in these interdigitated capacitor structures can be calculated usingan analytical model previously described by Farnell et al. [1].     

Device effects of various Zr/Ti ratios of PZT thin-films prepared by sol-gel method

Abstract

PZT, PbZr_xTI_1?xO₃, thin-films with various Zr/Ti ratios, 100/0 (lead zirconate) to 0/100 (lead titanate), were prepared by the sol-gel method. Basic electric properties, dielectric constant, tan σ, P-E hysteresis curve, switching properties were measured respectively as a function of composition. Dielectric constant indicated a specific peak value (～1100) around the morphotropic phase boundary between tetragonal and rhombohedral phase. Satisfactory low-voltage saturated hysteresis curves were observed for the compositions of PZT(90/10) through PZT(20/80). The remanent polarization and the coercive field increased as the titanium content decreased. The result of X-ray measurement showed that the lattice constants of thin-Film PZT are different from bulk ceramics for compatible compositionsS. The boundary, on which the c/a ratio must be 1 (rhombohedral phase), was slightly shifted to PbTiO₃ side. This distortion in crystal structure is considered to be due to the thin-film effect, which the lattice mismatch between the platinum substrate and the PZT layer, restricted the ions to position into proper cites.     

Sol-gel derived la modified PZT thin films: structure and properties

Lanthanum modified PZT thin films with compositions, namely 8/60/40, 8/70/30, 10/70/30 and 12/70/30 were deposited on platinized silicon substrates by sol-gel spin coating technique. Characterization of these films by XRD and SEM show that the films possess perovskite phase with submicron crystallite size. The saturation polarization (Ps), remnant polarization (PR) and coercive field (Ec) of polarization-electric field hysteresis loop are presented for all compositions. The 8/60/40 composition shows hysteresis loop with P/sub R/ = 11 /spl mu/C/cm/sup 2/. The temperature dependence of dielectric constant and dielectric loss of these films are also studied. Leakage current densities for these thin films are found to be in the range of 10/sup -/-10/sup -/ A/cm/sup 2/. To show the possible application of these thin films for micro electromechanical system (MEMS), a device incorporating an 8/60/40 PLZT thin film has been fabricated using silicon micromachining technology. This device functions satisfactorily as a vibration sensor with a resonance frequency of approximately 8.45 MHz.     

Effect of Buffer Layer on the Properties of Laser Ablated PZT Thin Films

Lead zirconate titanate (PbZr _x Ti_1?x O₃) or PZT ceramics are a class of piezoelectric materials that are currently experiencing widespread use in industry as electromechanical devices. PtSi/ZnO/PZT thin films were deposited by pulsed laser deposition at relatively low substrate temperature. The PZT thin films on PtSi substrates and on ZnO buffer layer were deposited at substrate temperature 300°C. The composition analysis shows that the film deposited at low temperature is stoichiometric. The films exhibit ferroelectric nature with coercive field of 19.6 kV/cm for 800 nm thick film. The leakage current density of the films shows a good insulating behavior.     

Influence of electric field on the ultrasound velocity in PZT ceramics

The paper deals with the influence of the electric bias field on the ultrasound velocity of various samples of Pb(Zr _x Ti_1−x )O₃ (PZT) ceramics. The ultrasonic velocities were measured on commercial types of PZT ceramics as APC 841, APC 850, and APC 856, at room temperature. The comparison of the ultrasound velocities dependence on electric bias field was made for poled/unpoled soft ceramics. The ultrasonic pulse-echo technique was used in our experiment. The ultrasonic system is based on Matec Instruments, Inc. modules. The time domain response was recorded and time of flight between echoes was directly measured by digital oscilloscope, type Agilent 54622D. The high bias field was applied on disk samples by the high voltage amplifier type Trek 610D, using a special setup and sample holder. The sound velocity was found to change drastically near the coercive field for a PZT ceramics, where the velocity of longitudinal waves decreases with an increasing field while the velocity of shear waves increases, which is caused by the change of the elastic anisotropy under influence of the depolarization field. The consequent change of the piezoelectric contribution to effective elastic constant decreases the velocity of longitudinal waves and at the same time increases the velocity of shear waves around the coercive field.     

Effect of AC&DC Field on the Dielectric Response of (Pb,La)TiO3 Thin Films

Lanthanum doped lead titanate thin films are the potential candidates for the capacitors, actuators and pyroelectric sensor applications due to their excellent dielectric, and ferroelectric properties. Lanthanum doped lead titanate thin films are grown on platinum coated Si substrates by excimer laser ablation technique. A broad diffused phase transition with the maximum dielectric permittivity (?_max) shifting to higher temperatures with the increase of frequency, along with frequency dispersion below T_c, which are the signatures of the relaxor like characteristics were observed. The dielectric properties are investigated from ?60°C to 200°C with an application of different dc fields. With increasing dc field, the dielectric constant is observed to reduce and phase transition temperature shifted to higher temperature. With the increased ac signal amplitude of the applied frequency, the magnitude of the dielectric constant is increasing and the frequency dispersion is observed in ferroelectric phase, whereas in paraelectric phase, there is no dispersion has been observed. The results are correlated with the existing theories.     

Enhancement of dielectric properties by optimization of sintering condition in tungsten–bronze structured Ba5SmTi3Nb7O30 ferroelectric ceramics

In this work, polycrystalline Ba₅SmTi₃Nb₇O₃₀ tungsten–bronze structured ferroelectric ceramics were synthesized by solid-state reaction technique at different sintering temperatures and durations. The X-ray diffractograms reveal the formation of the compounds in orthorhombic crystal system. The density of the compound is observed to increase with increase in sintering temperature and duration. Scanning electron microscopy (SEM) has been used for the microstructural investigation. Detailed dielectric properties of the compounds have been studied as a function of frequency and temperature. The variations of dielectric constant $\left( {\varepsilon \prime _r } \right)$ with temperature show that the compounds undergo a diffuse type ferro-paraelectric phase transition. The dielectric constant is found to increase with the increasing sintering temperature and duration. In all the samples, the variation of dielectric loss (tan δ) with temperature is observed to be almost constant initially but it increases as temperature is increased and a peak is observed only when the material is sintered at higher temperature for longer duration. The frequency dependence of dielectric constant and loss shows a decreasing trend up to nearly 10 kHz and beyond this frequency there is almost no variation. Also, the diffusivities of the samples have been calculated and it is found to increase with increasing sintering temperature and duration.     

Piezoelectric and dielectric aging in pb(zr,ti)o3 thin films and bulk ceramics

Abstract

Piezoelectric and dielectric aging was studied in Pb(Zr,Ti)O₃ (PZT) thin films and bulk ceramics. It was found that piezoelectric aging in thin films obeys the logarithmic time dependence with the relative aging rate much higher than that of the dielectric constant, while comparable aging rates of piezoelectric and dielectric constants were found in PZT ceramics. The origin of piezoelectric aging in PZT films was related to depolarization of the films rather than to suppression of the domain wall motion as was generally accepted for PZT ceramics.     

Low temperature sintering of screen-printed Pb(ZrTi)O3 thick films

Abstract

There has been increasing interest in ferroelectric lead zirconate titanate (PZT) films for the applications in piezoelectric and pyroelectric devices. Many potential applications require a film thickness of above 10 μm for higher force, better sensitivity and stability. But it is very difficult to fabricate the PZT thick film on the silicon substrate because of the volatility of PbO and the interdiffusion of the Pb and Si through the bottom electrode during the sintering at normal temperatures (such as above 1200°C). We speculated densification and reaction mechanism of the PZT thick films fabricated at relatively low temperature (under 1000°C) without sintering aids. The PZT thick films were screen-printed on Pt / Al₂O₃ substrate using a paste of PbO, ZrO₂ and TiO₂ powder mixture. Highly densified PZT thick films could be fabricated on Pt / Al₂O₃ substrate at 1000°C, and we achieved the density, remanent polarization, coercive field, dielectric permittivity, dissipation factor and breakdown field of 98%, 10 μC/cm² and 20 kV/cm, 540, 0.009 and 15 MV/m, respectively. The results show the possibility of densification of the PZT thick film at relatively low temperature without sintering aids, and the results are promising for the use of PZT thick films in various applications.     

Influence of Space Charge Layers on the Dielectric Properties of Ba0.6 Sr0.4TiO3 Nanostructured Thin Films

Barium strontium titanate (Ba_0.6Sr_0.4TiO₃) nanostructured thin films have been deposited on platinized silicon substrates by the sol-gel method. The as-fired films were found to be amorphous, which crystallize to cubic phase after annealing at 550°C in air for one hour. The low-frequency dielectric responses of the BST films were measured as functions of frequency range from 1 kHz to 1MHz. The thickness dependence dielectric constant of the BST thin films were measured in the temperature range from ?150°C to 150°C at 100 kHz and discussed in the light of an interfacial dead layer. All the samples showed a diffuse type phase transitions. Both the dielectric constant and loss tangent showed anomaly peaks at about 10°C, which corresponds to a tetragonal ferroelectric-to-cubic paraelectric phase transition.     

Electrical Properties of Nb-Doped PZT 65/35 Ceramics: Influence of Nb and Excess PbO

The effect of Nb and excess PbO on the structural and electrical properties of conventionally prepared Nb-doped PZT 65/35 ceramics has been studied in this work. It is found that, from excess PbO contents as high as 4 mol%, the solubility limit of Nb in PZT occurs below 4 mol%, while a secondary prevoskite-like phase develops in the dielectric system for a further increase of Nb content. The ferroelectric and piezoelectric properties (permittivity, ferro-paraelectric phase transition, polarization, electromechanical coefficients) of such materials are thus found to be strongly dependent on the degree of densification and structural phase development during sintering at high temperatures. In particular, the nature of the ferro- to para-electric phase transition is in these materials noted to better fit a generalized rather than Smolenskii-Isupov equation, the former being appropriate for the characterization of non-purely diffuse transitions. In nice agreement with the Bokov model, substitution of Nb^{5 +} for (Zr,Ti)^{4 +} is found to induce only poorly diffuse phase transition in these materials. The electrical properties reported in this work are in magnitude comparable to those exhibited by PZT-based materials.