Microscopic and dielectric analyses of vanadium and tungsten modified barium zirconium titanate ceramics

Dielectric spectroscopy was used in this study to examine polycrystalline vanadium and tungstendoped BaZr 0.1Ti 0.90O 3 (BZT10:2V and BZT10:2W) ceramics obtained by the mixed oxide method. According to X-ray diffraction analyses, addition of vanadium and tungsten lead to ceramics free of secondary phases. SEM analyses reveal that both dopants result in slower oxygen ion motion and consequently lower grain growth rate. Temperature dependence dielectric study showed normal ferroelectric to paraelectric transition well above the room temperature for the BZT10 and BZT10:2V ceramics. However, BZT10:2W ceramic showed a relaxor-like behavior near phase transition characterized by the empirical parameter γ. Piezoelectric force microscopy images reveals that the piezoelectric coefficient is strongly influenced by type of donor dopant suggesting promising applications for dynamic random access memories and data-storage media. Copyright © 2010 American Scientific Publishers All rights reserved.

Local electromethanical properties of the CaCu 3Ti 4O 12 ceramics

Scanning probe microscopy (SPM) was used to probe piezoelectric vibrations and local conductivity in CaCu 3Ti 4O 12 (CCTO) ceramics at room temperature. Piezoelectric contrast was observed on the polished surfaces of CCTO in both vertical (out-of-plane) and lateral (in-plane) modes and depended on the grain orientation varying in sign and amplitude. The piezoelectric contrast is shown to be controlled by the electrical bias (local poling) and displayed a ferroelectric-like reversible hysteresis accompanied with a change of the phase of piezoelectric signal. Flexoelectric effect (strain-gradient-induced polarization) due to surface relaxation was invoked to explain the observed contrast inside the grains. © 2010 Materials Research Society.

Adaptive filter feature identification for structural health monitoring in aeronautical panel

This paper presents an approach for structural health monitoring (SHM) by using adaptive filters. The experimental signals from different structural conditions provided by piezoelectric actuators/sensors bonded in the test structure are modeled by a discrete-time recursive least square (RLS) filter. The biggest advantage to use a RLS filter is the clear possibility to perform an online SHM procedure since that the identification is also valid for non-stationary linear systems. An online damage-sensitive index feature is computed based on autoregressive (AR) portion of coefficients normalized by the square root of the sum of the square of them. The proposed method is then utilized in a laboratory test involving an aeronautical panel coupled with piezoelectric sensors/actuators (PZTs) in different positions. A hypothesis test employing the t-test is used to obtain the damage decision. The proposed algorithm was able to identify and localize the damages simulated in the structure. The results have shown the applicability and drawbacks the method and the paper concludes with suggestions to improve it. ©2010 Society for Experimental Mechanics Inc.

Thickness dependence of structure and piezoelectric properties at nanoscale of polycrystalline lead zirconate titanate thin films

Lead zirconate titanate Pb(Zr0.50Ti0.50)O3 (PZT) thin films were deposited by a polymeric chemical method on Pt(111)/Ti/SiO2/Si substrates to understand the mechanisms of phase transformations and the effect of film thickness on the structure, dielectric, and piezoelectric properties in these films. PZT films pyrolyzed at temperatures higher than 350 °C present a coexistence of pyrochlore and perovskite phases, while only perovskite phase grows in films pyrolyzed at temperatures lower than 300 °C. For pyrochlore-free PZT thin films, a small (100)-orientation tendency near the film-substrate interface was observed. Finally, we demonstrate the existence of a self-polarization effect in the studied PZT thin films. The increase of self-polarization with the film thickness increasing from 200 nm to 710 nm suggests that Schottky barriers and/or mechanical coupling near the film-substrate interface are not primarily responsible for the observed self-polarization effect in our films. © 2013 AIP Publishing LLC.

Subcutaneous tissue reaction and cytotoxicity of polyvinylidene fluoride and polyvinylidene fluoride-trifluoroethylene blends associated with natural polymers

Cytotoxicity and subcutaneous tissue reaction of innovative blends composed by polyvinylidene fluoride and polyvinylidene fluoride-trifluoroethylene associated with natural polymers (natural rubber and native starch) forming membranes were evaluated, aiming its applications associated with bone regeneration. Cytotoxicity was evaluated in mouse fibroblasts culture cells (NIH3T3) using trypan blue staining. Tissue response was in vivo evaluated by subcutaneous implantation of materials in rats, taking into account the presence of necrosis and connective tissue capsule around implanted materials after 7, 14, 21, 28, 35, 60, and 100 days of surgery. The pattern of inflammation was evaluated by histomorphometry of the inflammatory cells. Chemical and morphological changes of implanted materials after 60 and 100 days were evaluated by Fourier transform infrared (FTIR) absorption spectroscopy and scanning electron microscopy (SEM) images. Cytotoxicity tests indicated a good tolerance of the cells to the biomaterial. The in vivo tissue response of all studied materials showed normal inflammatory pattern, characterized by a reduction of polymorphonuclear leukocytes and an increase in mononuclear leukocytes over the time (p < 0.05 Kruskal-Wallis). On day 60, microscopic analysis showed regression of the chronic inflammatory process around all materials. FTIR showed no changes in chemical composition of materials due to implantation, whereas SEM demonstrated the delivery of starch in the medium. Therefore, the results of the tests performed in vitro and in vivo show that the innovative blends can further be used as biomaterials. © 2013 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater 101B: 1284-1293, 2013. Copyright © 2013 Wiley Periodicals, Inc.

Obtenção e caracterização elétrica e morfológica de compósitos de borracha natural com PZT

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Fabricação, caracterização e aplicações do compósito PZT/PVDF

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Estudo de propriedades estruturais e de piezeletricidade nos cristais de ADP e KDP puros e dopados com íons Ni2+ e Mn3+ com DMRX utilizando radiação síncrotron

A difração múltipla de raios-X utilizando radiação Síncrotron foi aplicada para o estudo de cátions de metais de transição Mn³⁺ e Ni²⁺ incorporados a rede cristalina do Fosfato de Amônio Monobásico (ADP) e Fosfato de Potássio Monobásico (KDP). Em todos os diagramas Renninger obtidos para as diferentes amostras e diferentes comprimentos de onda podemos observar que as posições angulares e o número de picos não sofrem alteração. Este fato nos diz que os parâmetros da célula unitária e a simetria do cristal são praticamente os mesmos, independentemente da incorporação de cátíons Mn³⁺ e Ni²⁺. Cálculos precisos dos parâmetros da célula unitária revelam que há expansão dos parâmetros de rede a = b e contração do parâmetro de rede c do cristal de ADP dopado com Ni²⁺ e Mn³⁺. Nas medidas com ambos os comprimentos de onda no ADP:Mn o digrama Renninger apresenta picos com perfis semelhantes aos perfis dos picos nos diagrama Renninger do cristal de ADP puro. Nenhum pico extra aparece no diagrama Renninger do cristal dopado. A partir dos diagramas resultantes das medidas no cristal de ADP:Ni pode-se observar claramente: (i) alguns picos que tinham um perfil assimétrico no diagrama do cristal de ADP puro apresentam perfis quase totalmente simétricos no diagrama do cristal dopado com Ni (nas medidas com comprimento de onda abaixo da borda de absorção do Ni) e, (ii) alguns picos sofrem uma forte inversão em seus perfis (nas medidas com comprimento de onda acima da borda de absorção do Ni), por exemplo, o pico (5-12)/(-112), que representa um caso de quatro feixes. Estes resultados indicam que o diagrama Renninger com radiação Síncrotron é uma sonda de alta resolução a serem utilizados na incorporação de impurezas na rede ADP. Além disso, investigamos os coeficientes piezelétricos dos cristais de ADP:Mn, KDP:Mn e KDP:Ni por difração de raios-X à temperatura ambiente. Os resultados das medidas das reflexões 440 e 066 permitiram a obtenção dos coeficientes d₃₆ e d₂₅. Nós observamos que estes coeficientes aumentaram com a dopagem dos íons Mn³⁺ e Ni²⁺ nos cristais de ADP e KDP.

Effect of calcium on the structural properties of Ba(1-x)Ca (x) TiO3 particles synthesized by complex polymerization method

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Thickness-dependent piezoelectric behaviour and dielectric properties of lanthanum modified BiFeO3 thin films

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Preparo e caracterização de compósitos polímero/cerâmica com potencial aplicação como sensor multifuncional

Pós-graduação em Química - IQ

Interferometric measurements of nanometric displacements in a Piezoelectric Flextensional Actuator by using the new J1...J5 method

In this work, nanometric displacement amplitudes of a Piezoelectric Flextensional Actuator (PFA) designed using the topology optimization technique and operating in its linear range are measured by using a homodyne Michelson interferometer. A new improved version of the J1...J4 method for optical phase measurements, named J1...J5 method, is presented, which is of easier implementation than the original one. This is a passive phase detection scheme, unaffected by signal fading, source instabilities and changes in visibility. Experimental results using this improvement were compared with those obtained by using the J1... J4, J1...J6(pos) and J1...J 6(neg) methods, concluding that the dynamic range is increased while maintaining the sensitivity. Analysis based on the 1/f voltage noise and random fading show the new method is more stable to phase drift than all those methods. © 2012 IEEE.

Laminated Tubular-channel Ferroelectret Systems from Low-density Polyethylene Films and from Fluoroethylene-propylene Copolymer Films - A Comparison

A template-based lamination technique for the manufacture of ferroelectrets from uniform electret films was recently reported. In the present work, this technique is used to prepare similar ferroelectret structures from low-density polyethylene (LDPE) films and from fluoro-ethylene-propylene (FEP) copolymer films. A comparative analysis of the pressure-, temperature-, and frequency-dependent piezoelectric properties has been performed on the two ferroelectret systems. It is observed that the FEP ferroelectrets exhibit better piezoelectric responses and are thermally more stable. The difference between the piezoelectric d(33) coefficients of the two ferroelectret systems is partially explained here by their different elastic moduli. The anti-resonance peaks of both structures have been investigated by means of dielectric resonance spectroscopy and electroacoustic sound-pressure measurements. A difference of more than 10 kHz is observed between the anti-resonance frequencies of the two ferroelectret systems.

Fluoropolymer piezoelectrets with tubular channels: resonance behavior controlled by channel geometry

Ferro- or piezoelectrets are dielectric materials with two elastically very different macroscopic phases and electrically charged interfaces between them. One of the newer piezoelectret variants is a system of two fluoroethylenepropylene (FEP) films that are first laminated around a polytetrafluoroethylene (PTFE) template. Then, by removing the PTFE template, a two-layer FEP structure with open tubular channels is obtained. After electrical charging, the channels form easily deformable macroscopic electric dipoles whose changes under mechanical or electrical stress lead to significant direct or inverse piezoelectricity, respectively. Here, different PTFE templates are employed to generate channel geometries that vary in height or width. It is shown that the control of the channel geometry allows a direct adjustment of the resonance frequencies in the tubular-channel piezoelectrets. By combining several different channel widths in a single ferroelectret, it is possible to obtain multiple resonance peaks that may lead to a rather flat frequency-response region of the transducer material. A phenomenological relation between the resonance frequency and the geometrical parameters of a tubular channel is also presented. This relation may help to design piezoelectrets with a specific frequency response.

Mixed Mode Fracture Behaviour of Piezoelectric Materials

Piezoelectrics present an interactive electromechanical behaviour that, especially in recent years, has generated much interest since it renders these materials adapt for use in a variety of electronic and industrial applications like sensors, actuators, transducers, smart structures. Both mechanical and electric loads are generally applied on these devices and can cause high concentrations of stress, particularly in proximity of defects or inhomogeneities, such as flaws, cavities or included particles. A thorough understanding of their fracture behaviour is crucial in order to improve their performances and avoid unexpected failures. Therefore, a considerable number of research works have addressed this topic in the last decades. Most of the theoretical studies on this subject find their analytical background in the complex variable formulation of plane anisotropic elasticity. This theoretical approach bases its main origins in the pioneering works of Muskelishvili and Lekhnitskii who obtained the solution of the elastic problem in terms of independent analytic functions of complex variables. In the present work, the expressions of stresses and elastic and electric displacements are obtained as functions of complex potentials through an analytical formulation which is the application to the piezoelectric static case of an approach introduced for orthotropic materials to solve elastodynamics problems. This method can be considered an alternative to other formalisms currently used, like the Stroh’s formalism. The equilibrium equations are reduced to a first order system involving a six-dimensional vector field. After that, a similarity transformation is induced to reach three independent Cauchy-Riemann systems, so justifying the introduction of the complex variable notation. Closed form expressions of near tip stress and displacement fields are therefore obtained. In the theoretical study of cracked piezoelectric bodies, the issue of assigning consistent electric boundary conditions on the crack faces is of central importance and has been addressed by many researchers. Three different boundary conditions are commonly accepted in literature: the permeable, the impermeable and the semipermeable (“exact”) crack model. This thesis takes into considerations all the three models, comparing the results obtained and analysing the effects of the boundary condition choice on the solution. The influence of load biaxiality and of the application of a remote electric field has been studied, pointing out that both can affect to a various extent the stress fields and the angle of initial crack extension, especially when non-singular terms are retained in the expressions of the electro-elastic solution. Furthermore, two different fracture criteria are applied to the piezoelectric case, and their outcomes are compared and discussed. The work is organized as follows: Chapter 1 briefly introduces the fundamental concepts of Fracture Mechanics. Chapter 2 describes plane elasticity formalisms for an anisotropic continuum (Eshelby-Read-Shockley and Stroh) and introduces for the simplified orthotropic case the alternative formalism we want to propose. Chapter 3 outlines the Linear Theory of Piezoelectricity, its basic relations and electro-elastic equations. Chapter 4 introduces the proposed method for obtaining the expressions of stresses and elastic and electric displacements, given as functions of complex potentials. The solution is obtained in close form and non-singular terms are retained as well. Chapter 5 presents several numerical applications aimed at estimating the effect of load biaxiality, electric field, considered permittivity of the crack. Through the application of fracture criteria the influence of the above listed conditions on the response of the system and in particular on the direction of crack branching is thoroughly discussed.