Effects of thermal treatment on phase transitions and on the mechanical relaxation in poly(vinylidene fluoride)

This work reports on the effects from thermal treatment in poly(vinylidene fluoride), PVDF, obtained with differential scanning calorimetry (DSC) and dynamic thermal analysis (DMA) measurements. It is shown that in successive DMA measurements performed with one sample the α relaxation peak almost disappears while the γ′ peak appears. The α relaxation peak, at ∼100°C in DMA measurements, is attributed to the preferential orientation of chains in the amorphous phase while the γ′ relaxation peak, at ∼50°C, is related to the thermal treatment to which the sample was submitted.

Effect of Nb on barium titanate prepared from citrate solutions

The influence of the addition of dopants on the microstructure development and electrical properties of BaTiO3 doped with 0.2, 0.4, 0.6, 0.8 mol% of Nb and 0.01 mol% of Mn based compounds was studied. Doped barium titanate was prepared using the polymeric precursor method from citrate solutions. The powders calcined at 700°C for 4 hours were analysed by infrared (IR) spectroscopy to verify the presence of carbonates, and by X-ray diffraction (XRD) for phase formation. The phase composition, microstructure and dielectric properties show a strong dependence on the amount of added niobium.

Microstructure of doped barium titanate prepared from polymeric precursors

Barium titanate is used extensively as a dielectric in ceramic capacitors, particularly due to its high dielectric constant and low dielectric loss characteristics. It can be made semiconducting by addition of certain dopants and by proper modification of grains and grain boundary properties obtaining very interesting characteristics for various applications. The synthesis method and sintering regime have a strong influence on properties of obtained barium titanate ceramics. Doped barium titanate was prepared with Nb+5 and Y+3 ions as donor dopants, and with Mn+2 ions as acceptor dopant by polymeric precursors method. By this procedure nanosized powders were obtained after calcination. Sintering was performed in the temperature range of 1290°C to 1380°C The microstructure of doped BaTiO3 was performed using scanning electron microscopy. The influence of dopants and sintering temperature on grain size was analysed.

Estudio de PMN cerámico dopado con KNbO3 y LiNbO 3 sintetizado por Pechini

PMN belongs to a special class of materials named relaxor ferroelectrics. It has high volumetric efficiency due to its high dielectric constant, which makes it in a perfect material for application in multilayer capacitors. When prepared the columbite route its preparation has many advantages. In this work, the preparations of columbite and PMN were done by Pechini and Partial Oxalate methods, respectively. The effects of the KNbO3 and LiNbO3 dopants added in various concentrations. The idea is founded on the correlations that they have with BaTiO3 y PbTiO3, respectively. The whole process was supervised by TG/DTA, XRD, SEM and determination of the specific surface area of the powders. LiNbO3 carries out the pre-sinterization of the particles, observed by a reduction in the surface area. There are not particle grow, but occur its lengthening. However, for KNbO3 these particle growth, but the agglomerates are softer. The effect produced by the doping during the synthesis of the PMN powder is different from the one produced in the columbite precursor. Pure precursor shows an average particle size of 0,2μm, but the addition of 5,0mol% of dopants carries out the formation of agglomerates close to 4μm. LiNbO 3 addition carries out spherical particles and pre-sinterization, while KNbO3 addition does not change the particles shape.

The influence of the sintering system on PMN properties

PMN powder samples with PbO excess of 0, 1,2 and 3% were submitted to the pressing and sintering at 1200°C for 4h with a heating rate of 3°C/min. A new sintering system, developed at our laboratories, was used. It allows obtaining more information on the sintering process. The sintered samples in the new system were compared to sintered samples in the C system. The microstructure, dielectric properties and the effect of the PbO excess in different sintering systems were compared. The N system permitted to obtain a ceramic with better properties, such density, dielectric constant and very homogeneous microstructure.

Influence of oxygen atmosphere on LiNbO3 thin films prepared by Pechini process

Thin films of lithium niobate were deposited on the Pt/Ti/SiO2 (111) substrates by the polymeric precursor method (Pechini process). Annealing in static air and oxygen atmosphere was performed at 500°C for 3 hours. The films obtained were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The dielectric constant, dissipation factor and resistance were measured in frequency region from 10 Hz to 10 MHz. Electrical characterizations of the films pointed to ferroelectricity via hysteresis loop. The influence of oxygen atmosphere on crystallization and properties of LiNbO3 thin films is discussed.

Estudio de la adición de K+ y LiNbO3 en las propiedades finales del relaxor PMN procesado por mezcla de polvos

PMN ceramic relaxor has been investigated by several researchers and many aspects of this material, like powder morphology, phase decomposition, weight loss during sintering process, densification, between others, still are investigated. PMN powder preparation has been shown more efficient when synthesized by columbite route, however lead addition stage for the PMN powder synthesis remains problematical. Therefore, this work proposes a new association of methodologies, using columbite route and the hydroxide precipitation method. Through use of the powder mixture technique, which permitted to obtain good green and sintered densities, was possible to observe K+ y Li + dopants reduce weight loss in sintering process and change significantly the dielectric properties. Addition of LiNbO3 seeds in conformation stage, which react in a distinct way as a function of the particle size, promotes the formation of differenced grains in the ceramic bulk. Consequently, very different dielectrics properties from conventional PMN ceramic were obtained.

Structure study of donor doped barium titanate prepared from citrate solutions

Barium titanates doped with Nb5+, and Y3+, were prepared. The starting powders were synthesized from citrate solutions by the Pechini process and partial Pechini process in two steps. Sintering was performed in the range from 1310° up to 1380°C for 2 hours in air atmosphere. The structural study concerning the incorporation of Nb and Y ions in the barium titanate crystal lattice was performed by XRD, XANES and EXAFS techniques. The dielectric properties were analyzed and the relationship between properties and structure of doped barium titanate was established.

The synergistic effects of Nb/Mn and Sb/Mn on the microstructure and electrical characteristics of BaTiO3 based ceramics

The microstructure and dielectric properties of Nb-Mn or Sb-Mn codoped BaTiO3 compositions were investigated. Starting ceramics powders were prepared by Pechini method. The composites were sintered at 1310°C and 1330°C in an air atmosphere for two hours. The microstructure and compositional investigations were done with SEM equipped with EDS. Two distinguish microstructure regions are observed in Nb/0.05Mn doped BaTiO 3 ceramics sintered at low temperature. The first, large one, with grain sizes from 5-40 μm and the second region with small grain sizes from 1 to 5 μm. Sintering at higher temperature, independent of Mn content, enables to achieve a uniform microstructure with grains less than 6 μm. In Sb/Mn doped ceramics, for both sintering temperatures, bimodal microstructures with fine grained matrix and grains up to 10 μm is formed. The highest value of permittivity at room temperature and the greatest change of permittivity in function of temperature are observed in Nb/0.01Mn doped ceramics compared to the same ones in Sb/Mn doped ceramics. The greatest shift of Curie temperature towards lower temperature has been noticed in Sb/Mn BaTiO3 ceramics compared to others samples. In all investigated samples the dielectric loss after initially large values at low frequency maintains a constant value for f>3 kHz.

Physical characterization of K-doped 0.9PMN-0.1PT synthesized by an association of the columbite route and the polymeric precursor method

The solid solution 0.9PbMg 1/3Nb 2/3O 3-0.1PbTiO 3 is one of the most widely investigated relaxor ceramic, because of its high dielectric constant and low sintering temperatures. PMN-PT powders containing single perovskite phase were prepared by using a Timodified columbite precursor obtained by the polymeric precursor method. Such precursor reacts directly with stoichiometric amount of PbO to obtain pyrochlore-free PMN-PT powders. The structural effects of K additive included in the columbite precursor and 0.9PMN-0.1PT powders were also studied. The phase formation at each processing step was verified by XRD analysis, being these results used for the structural refinement by the Rietveld method. It was verified the addition of K in the columbite precursor promotes a slight increasing in the powder crystallinity. There was not a decrease in the amount of perovskite phase PMN-PT for 1mol% of K, and the particle and grain size were reduced, making this additive a powerful tool for grain size control.

PTCa/PEEK composite acoustic emission sensors

Composites made of Calcium-modified lead titanate (PTCa) and poly (ether-etherketone) (PEEK) high performance polymer matrix were prepared in the film form using a hot press. The ceramic volume fraction reaches up to 60 percent providing a composite with 0-3 and 1-3 mixed connectivities due to the high ceramic content and the resulting materials could be considered PEEK-bonded PTCa particulate composite. The composites were characterized using piezoelectric spectroscopy and ultrasonic immersion techniques. Values up to 38.5 pC/N were obtained for the longitudinal d33 piezoelectric coefficient. The composite was surface-mounted on a carbon fiber plate-like specimen and the ability of the PTCa/PEEK composite to detect acoustic emission (AE) is reported. © 2006 IEEE.

Development of a new TDR probe for determining soil water content and dry density

A few traditional methods for determining water content in the field are either inaccurate or time consuming. As an alternative, the time domain reflectometry (TDR) technology has been used in the determination of the soil water content for geotechnical applications. This paper presents the preliminary results on the development of a new TDR probe for determining soil water content and dry density at different depths. This new probe is intended to be pushed into the ground using piezocone equipment. Different from the standard TDR probes with straight rods, the new probe consists of two parallel copper stripes coiled around a PVC-steel core. The probe diameter is the same as the standard 10 cm2 piezocone diameter. Through laboratory calibrations, it is possible to establish expressions relating the soil apparent dielectric constant and the bulk electrical conductivity with the gravimetric water content and the dry density. Copyright ASCE 2007.

Magnetoelectric coefficient in strontium ruthenate buffered lanthanum modified bismuth ferrite thin films grown by chemical method

This paper focuses on the magnetoelectric coupling (ME) at room temperature in lanthanum modified bismuth ferrite thin film (BLFO) deposited on SrRuO 3-buffered Pt/TiO 2/SiO 2/Si(100) substrates by the soft chemical method. BLFO film was coherently grown at a temperature of 500 °C. The magnetoelectric coefficient measurement was performed to evidence magnetoelectric coupling behavior. Room temperature magnetic coercive field indicates that the film is magnetically soft. The maximum magnetoelectric coefficient in the longitudinal direction was close to 12 V/cmOe. Dielectric permittivity and dielectric loss demonstrated only slight dispersion with frequency due the less two-dimensional stress in the plane of the film. Polarization reversal was investigated by applying dc voltage through a conductive tip during the area scanning. We observed that various types of domain behavior such as 71 ° and 180° domain switching, and pinned domain formation occurred. Copyright © 2009 American Scientific Publishers All rights reserved.

Diffuse Effect of the Tungsten Doped Ba(Zr0.10Ti0.90)O3 Ferroelectric Ceramics

Barium zirconate titanate Ba(Ti0.90Zr0.10)O3 ceramics doped with WO3 (BZT:2W) have been prepared by a traditional solid phase reaction. The effect of temperature on the structural and electrical properties was investigated. X ray diffraction data evidenced formation of secondary phases for the samples sintered at 1300oC end 1350oC while the pure phase was attained at 1200oC. A modified Curie-Weiss law was used to describe the diffuseness of a phase transition. As temperature increases, the maximum dielectric permittivity decreased. The fine-grained sample showed a 'diffuse-like' ferroelectric behavior. The dielectric permittivity reaches a maximum value (εm ~6420 at 10 kHz) for the ceramics sintered at 1200oC for 4 hours.

Observation of piezoelectric response on tungsten doped barium zirconium titanate ceramics

This study describes observation of piezoelectric response of Ba(Zr 0.10Ti 0.90.O3 ceramics modified with tungsten (BZT:2W) by the mixed oxide method. According to X ray diffraction analysis, the ceramics are free of secondary phases. Transmission electron microscopy (TEM) analyses reveals the absence of segregates in the grain boundaries indicates the high solubility of WO3 in the BZT matrix. The dielectric permittivity measured at a frequency of 10 KHz was equal to 6500 with dieletric loss of 0.15. A typical hysteresis loop was observed at room temperature. Electron Paramagnetic Resonance (EPR) analyses reveals that substitution of W6+ by Ti4+ causes distortion in the crystal structure changing lattice parameter. Polarization reversal was investigated by applying dc voltage through a conductive tip during the area scanning. Piezoelectric force microscopy images reveals that in-plane response may not change its sign upon polarization switching, while the out-of-plane response does. Copyright © 2010 American Scientific Publishers.