Piezoresponse force microscopy characterization of rare-earth doped BiFeO3 thin films grown by the soft chemical method

The multiferroic behavior with ion modification using rare-earth cations on crystal structures, along with the insulating properties of BiFeO3 (BFO) thin films was investigated using piezoresponse force microscopy. Rare-earth-substituted BFO films with chemical compositions of (Bi 1.00-xRExFe1.00O3 (x=0; 0.15), RE=La and Nd were fabricated on Pt (111)/Ti/SiO2/Si substrates using a chemical solution deposition technique. A crystalline phase of tetragonal BFO was obtained by heat treatment in ambient atmosphere at 500 °C for 2 h. Ion modification using La3+ and Nd3+ cations lowered the leakage current density of the BFO films at room temperature from approximately 10-6 down to 10-8 A/cm2. The observed improved magnetism of the Nd3+ substituted BFO thin films can be related to the plate-like morphology in a nanometer scale. We observed that various types of domain behavior such as 71° and 180° domain switching, and pinned domain formation occurred. The maximum magnetoelectric coefficient in the longitudinal direction was close to 12 V/cm Oe. © 2012 Elsevier Ltd and Techna Group S.r.l.

Piezoresponse force microscopy behaviour of Bi4Ti3O12 ceramics with various excess bismuth

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

Effect of oxidizing and reducing atmospheres on Ba(Ti0.90 Zr0.10)O3:2V ceramics as characterized by piezoresponse force microscopy

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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.

Mapping of adhesion forces on soil minerals in air and water by atomic force spectroscopy (AFS)

The adhesion force between an atomic force microscope (AFM) tip and sample surfaces, mica and quartz substrates, was measured in air and water. The force curves show that the adhesion has a strong dependence on both the surface roughness and the environmental conditions surrounding the sample. The variability of the adhesion force was examined in a series of measurements taken at the same point, as well as at different places on the sample surface. The adhesion maps obtained from the distribution of the measured forces indicated regions contaminated by either organic compounds or adsorbed water. Using simple mathematical expressions we could quantitatively predict the adhesion force behavior in both air and water. The experimental results are in good agreement with theoretical calculations, where the adhesion forces in air and water were mostly associated with capillary and van der Waals forces, respectively. A small long-range repulsive force is also observed in water due to the overlapping electrical double-layers formed on both the tip and sample surfaces.

Pressure-induced electrical and structural anomalies in Pb1-xCaxTiO3 thin films grown at various oxygen pressures by chemical solution route

Lead calcium titanate (Pb1-xCaxTiO3 or PCT) thin films have been thermally treated under different oxygen pressures, 10, 40 and 80 bar, by using the so-called chemical solution deposition method. The structural, morphological, dielectric and ferroelectric properties were characterized by x-ray diffraction, FT-infrared and Raman spectroscopy, atomic force microscopy and polarization-electric-field hysteresis loop measurements. By annealing at a controlled pressure of around 10 and 40 bar, well-crystallized PCT thin films were successfully prepared. For the sample submitted to 80 bar, the x-ray diffraction, Fourier transformed-infrared and Raman data indicated deviation from the tetragonal symmetry. The most interesting feature in the Raman spectra is the occurrence of intense vibrational modes at frequencies of around 747 and 820 cm(-1), whose presence depends strongly on the amount of the pyrochlore phase. In addition, the Raman spectrum indicates the presence of symmetry-breaking disorder, which would be expected for an amorphous (disorder) and mixed pyrochlore-perovskite phase. During the high-pressure annealing process, the crystallinity and the grain size of the annealed film decreased. This process effectively suppressed both the dielectric and ferroelectric behaviour. Ferroelectric hysteresis loop measurements performed on these PCT films exhibited a clear decrease in the remanent polarization with increasing oxygen pressure.

Effect of oxidizing atmosphere on the electrical properties of SrBi4Ti4O15 thin films obtained by the polymeric precursor method

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

Phase-Locked loops lock-in range in Frequency Modulated-Atomic Force Microscope nonlinear control system

Since the mid 1980s the Atomic Force Microscope is one the most powerful tools to perform surface investigation, and since 1995 Non-Contact AFM achieved true atomic resolution. The Frequency-Modulated Atomic Force Microscope (FM-AFM) operates in the dynamic mode, which means that the control system of the FM-AFM must force the micro-cantilever to oscillate with constant amplitude and frequency. However, tip-sample interaction forces cause modulations in the microcantilever motion. A Phase-Locked loop (PLL) is used to demodulate the tip-sample interaction forces from the microcantilever motion. The demodulated signal is used as the feedback signal to the control system, and to generate both topographic and dissipation images. As a consequence, a proper design of the PLL is vital to the FM-AFM performance. In this work, using bifurcation analysis, the lock-in range of the PLL is determined as a function of the frequency shift (Q) of the microcantilever and of the other design parameters, providing a technique to properly design the PLL in the FM-AFM system. (C) 2011 Elsevier B.V. All rights reserved.

Phase-Locked Loop design applied to frequency-modulated atomic force microscope

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

Effect of the excess of bismuth on the morphology and properties of the BaBi2Nb2O9 thin films

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

Dielectric properties of Ca(Zr0.05Ti0.95)O-3 thin films prepared by chemical solution deposition

Ca(Zr0.05Ti0.95)O-3 (CZT) thin films were grown on Pt(1 1 1)/Ti/SiO2/Si(1 0 0) substrates by the soft chemical method. The films were deposited from spin-coating technique and annealed at 928 K for 4 h under oxygen atmosphere. CZT films present orthorhombic structure with a crack free and granular microstructure. Atomic force microscopy and field-emission scanning electron microscopy showed that CZT present grains with about 47 nm and thickness about 450 nm. Dielectric constant and dielectric loss of the films was approximately 210 at 100 kHz and 0.032 at 1 MHz. The Au/CZT/Pt capacitor shows a hysteresis loop with remnant polarization of 2.5 mu C/cm(2), and coercive field of 18 kV/cm, at an applied voltage of 6 V. The leakage current density was about 4.6 x 10(-8) A/cm(2) at 3 V. Dielectric constant-voltage curve is located at zero bias field suggesting the absence of internal electric fields. (c) 2006 Elsevier B.V. All rights reserved.

Filmes finos de SrBi2Ta2O9 processados em forno microondas

Filmes finos de SrBi2Ta2O9 foram depositados em substratos de Pt/Ti/SiO2/Si e, pela primeira vez, sinterizados em forno microondas doméstico. Os padrões de difração de raios X mostraram que os filmes são policristalinos. O processamento por microondas permite utilizar baixa temperatura na síntese e obter filmes com boas propriedades elétricas. Ensaios de microscopia eletrônica de varredura (MEV) e de Força Atômica (MFA) revelam boa aderência entre filme e substrato, com microestrutura de superfície apresentando grãos finos e esféricos e rugosidade de 4,7 nm. A constante dielétrica e o fator de dissipação, para freqüência de 100 KHz, à temperatura ambiente, foram de 77 e 0,04, respectivamente. A polarização remanescente (2Pr) e o campo coercitivo (Ec) foram 1,04 miC/cm² e 33 kV/cm. O comportamento da densidade de corrente de fuga revela três mecanismos de condução: linear, ôhmico e outro mecanismo que pode ser atribuído à corrente de Schottky. Dos padrões de DRX, análises das imagens por MEV e topografia de superfície por MFA observa-se que 10 min de tratamento térmico a 550 ºC, em forno microondas, é tempo suficiente para se obter a cristalização do filme.

Preparation and properties of ferroelectric Pb1-xCaxTiO3 thin films produced by the polymeric precursor method

Pb1- xCaxTiO3 thin films with x = 0.24 composition were prepared by the polymeric precursor method on Pt/Ti/SiO2/Si substrates. The surface morphology and crystal structure, and the ferroelectric and dielectric properties of the films were investigated. X-ray diffraction patterns of the films revealed their polycrystalline nature. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) analyses showed the surface of these thin films to be smooth, dense and crack-free with low surface roughness. The multilayer Pb1-xCaxTO3 thin films were granular in structure with a grain size of approximately 60-70 nm. The dielectric constant and dissipation factor were, respectively, 174 and 0.04 at a 1 kHz frequency. The 600-nm thick film showed a current density leakage in the order of 10(-7) A/cm(2) in an electric field of about 51 kV/cm. The C-V characteristics of perovskite thin films showed normal ferroelectric behavior. The remanent polarization and coercive field for the deposited films were 15 muC/cm(2) and 150 kV/cm, respectively. (C) 2001 Kluwer Academic Publishers.

Oriented growth of Bi3.25La0.75Ti3O12 thin films on RuO2/SiO2/Si substrates by using the polymeric precursor method: Structural, microstructural and electrical properties

c-axis oriented Bi3.25La0.75Ti3O12 (BLT) thin films were grown on a RuO2 top electrode deposited on a (100) SiO2/Si substrate by the polymeric precursor method. X-ray diffraction and atomic force microscope investigations indicate that the films exhibit a dense, well crystallized microstructure having random orientations with a rather smooth surface morphology. The electrical properties of preferred oriented Bi3.25La0.75Ti3O12 (BLT) thin films deposited on RuO2 bottom electrode leaded to a large remnant polarization (P-r ) of 17.2 mu C/cm(2) and (V-c ) of 1.8 V, fatigue free characteristics up to 10(10) switching cycles and a current density of 2.2 mu A/cm(2) at 5 V. We found that the polarization loss is insignificant with nine write/read voltages at a waiting time of 10,000 s. Independently of the applied electric field the retained switchable polarization approached a nearly steady-state value after a retention time of 10 s.

Effects of post-annealing on the dielectric properties of Au/BaTiO3/Pt thin film capacitors

Barium titanate thin films were prepared by the polymeric precursor method and deposited onto Pt/Ti/SiO2/Si substrates. X-ray diffraction (XRD), scanning electron microscopy (SEM) and atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FT-IR) and micro-Raman spectroscopy were used to investigate the formation of the BaTiO3 perovskite phase. Afterwards, the films were submitted to post-annealing treatments in oxygen and nitrogen atmospheres at 300 degreesC for 2 h, and had their dielectric properties measured. It was observed that the electric properties of the thin films are very sensitive to the nature of the post-annealing atmosphere. This study demonstrates that post-annealing in an oxygen atmosphere increases the dielectric relaxation phenomenon and that post-annealing in a nitrogen atmosphere produces a slight dielectric relaxation. (C) 2004 Elsevier B.V All rights reserved.