Lignin from sugar cane bagasse: Extraction, fabrication of nanostructured films, and application

Four lignin samples were extracted from sugar cane bagasse using four different alcohols (methanol, ethanol, n-propanol, and 1-butanol) via the organosolv-CO2 supercritical pulping process. Langmuir films were characterized by surface pressure vs mean molecular area (Pi-A) isotherms to exploit information at the molecular level carrying out stability tests, cycles of compression/expansion (hysteresis), subphase temperature variations, and metallic ions dissolved into the water subphase at different concentrations. Briefly, it was observed that these lignins are relatively stable on the water surface when compared to those obtained via different extraction processes. Besides, the Pi-A isotherms are shifted to smaller molecular areas at higher subphase temperatures and to larger molecular areas when the metallic ions are dissolved into the subphase. The results are related to the formation of stable aggregates (domains) onto the water subphase by these lignins, as shown in the Pi-A isotherms. It was found as well that the most stable lignin monolayer onto the water subphase is that extracted with 1-butanol. Homogeneous Langmuir-Blodgett (LB) films of this lignin could be produced as confirmed by UV-vis absorption spectroscopy and the cumulative transfer parameter. In addition, FTIR analysis showed that this lignin LB film is structured in a way that the phenyl groups are organized preferentially parallel to the substrate surface. Further, these LB films were deposited onto gold interdigitated electrodes and ITO and applied in studies involving the detection of Cd+2 ions in aqueous solutions at low concentration levels throughimpedance spectroscopy and electrochemical measurements. FTIR spectroscopy was carried out before and after soaking the thin films into Cd+2 aqueous solutions, revealing a possible physical interaction between the lignin phenyl groups and the heavy metal ions. The importance of using nanostructured systems is demonstrated as well by comparing both LB and cast films.

Microstructural and ferroelectric properties of PbZr1-xTi(x)O(3) thin films prepared by the polymeric precursor method

The polymeric precursor method was employed in the preparation of PZT thin films on Pt(111)Ti/SiO2/Si(100) substrates. X-ray diffraction patterns revealed the polycrystalline nature of the PZT (53:47) thin films, which had a granular structure and a grain size of approximately 70 nm. A 350-nm thick film was obtained by running three cycles of the dip-coating/heating process. Atomic force microscopy (AFM) analyses showed the surface of these thin films to be smooth, dense and crack-free with low surface roughness (= 2.0 nm). The PZT (53:47) thin films annealed at 700 degreesC showed a well-saturated hysteresis loop. The C-V curves of perovskite thin film displayed normal ferroelectric behavior, while the remanent polarization (2P(r)) and coercive field (E-e) of the film deposited and measured at room temperature were 40 muC/cm(2) and 110 kV/cm, respectively. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Effect of the excess of bismuth on the morphology and properties of the BaBi2Ta2O9 ceramics

In this study, the effect of bismuth content on the crystal structure, morphology and electric properties of barium-bismuth-tantalate (BBT) ceramics was explored with the aid of X-ray diffraction (XRD), scanning electron microcopy (SEM), dielectric properties and ferroelectric hysteresis loops. BaBi2Ta2O9 (BBT) ceramics have been successfully prepared by the solid-state reaction. The BBT phase was crystallized at 900 degreesC for 2 h. The excess of bismuth controls the grain size, affecting the density of the material. Measurements of dieletric constant and dieletric losses confirm that the material is a ferroeletric with a Curie temperature around 77 degreesC. The dieletric constant measured at room temperature was 400, with a dielectric loss of 0.03. Both the phase-transition behaviour and ferroelectric properties, such as spontaneous polarization (P-s), showed a dependence on Bi content. (C) 2004 Elsevier B.V. All rights reserved.

Synthesis and electrical characterization of tungsten doped Pb(Zr0.53Ti0.47)O-3 ceramics obtained from a hybrid process

Pure and W-doped PZT ceramics (PZT and PZTW) were prepared by a hybrid process consisting in the association of polymeric precursor and partial oxalate methods. The phase formation was investigated by simultaneous thermal analysis (TG/DSC) and X-ray diffraction (XRD). The effect of W doping PZT and their electrical properties was evaluated. Substitution of W by Ti leads to an increase of Curie temperature and broadening of dielectric constant. A typical hysteresis loop was observed at room temperature and the remnant polarization was increased with the content of W. (c) 2007 Elsevier B.V. All rights reserved.

Crystallographic and magnetic structure of polycrystalline Zn7-xNixSb2O12 spinels

The crystallographic and magnetic structure of sintered, polycrystalline samples of zinc-antimony spinel, Zn7-xNixSb2O12, have been investigated. The samples were prepared by the modified polymeric precursors method. The magnetic contributions of the Ni2+ ions distributed in three non-equivalent crystallographic sites were investigated, revealing the occurrence of different magnetic regimes. A hysteresis response in the magnetic susceptibility indicates a spin-glasslike behavior at low temperatures. (C) 2000 Elsevier B.V. S.A. All rights reserved.

Ferroelectric properties of mechanically synthesized nanosized barium titanate

Barium titanate ceramics were prepared through mechanochemical synthesis starting from fresh prepared barium oxide and titanium oxide in rutile form. Mixture of oxides was milled in zirconia oxide jar in the planetary ball-mill during 30, 60, 120 and 240 min. Extended time of milling directed to formation of higher amount of barium titanate perovskite phase. Barium titanate with good crystallinity was formed after 240 min. Sintering without pre-calcinations step was performed at 1330 degrees C for 2 hours with heating rate of 10 degrees C/min. The XRD, DSC, IR and TEM analyses were performed. Electric and ferroelectric properties were studied. Very well defined hysteresis loop was obtained.

Preparation of Pb(Zr,Ti)O-3 thin films by soft chemical route

Lead zirconate titanate, Pb(Zr0.3Ti0.7)O-3 (PZT) thin films were prepared with success by the polymeric precursor method. Differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), Micro-Raman spectroscopy and X-ray diffraction (XRD) were used to investigate the formation of the PZT perovskite phase. X-ray diffraction revealed that the film showed good crystallinity and no presence of secondary phases was identified. This indicates that the PZT thin films were crystallized in a single phase. PZT thin films showed a well-developed dense grain structure with uniform distribution, without the presence of rosette structure. The Raman spectra undoubtedly revealed these thin films in the tetragonal phase. For the thin films annealed at the 500-700 degreesC range, the vibration modes of the oxygen sublattice of the PZT perovskite phase were confirmed by FT-IR. The room temperature dielectric constant and dielectric loss of the PZT films, measured at 1 kHz were 646 and 0.090, respectively, for thin film with 365 nm thickness annealed at 700 degreesC for 2 h. A typical P-E hysteresis loop was observed and the measured values of P-s, P-r and E-c were 68 muC/cm(2), 44 muC/cm(2) and 123 kV/cm, respectively. The leakage current density was about 4.8 x 10(-7) A/cm(2) at 1.5 V. (C) 2003 Elsevier Ltd. All rights reserved.

Influence of temperature on the microstructure and electrical properties of BBT thin films

The BBT films were prepared by a spin-coating process from the polymeric precursor method (Pechini process). In order to study the influence of the temperature on the BBT microstructure and electrical properties, the films were deposited on platinum coated silicon substrates and annealed from 700degreesC to 800degreesC for 2 hours in oxygen atmosphere. The crystallinity of the films was examined by X-ray diffraction while the surface morphology was analysed by atomic force microscope. The dielectric properties and dissipation factor of BaBi2Ta2O9 films at 1 MHz were observed. The polarization-electric field hysteresis loops revealed the ferroelectric characteristics of BaBi2Ta2O9 thin films.

Very large dielectric constant of highly oriented Pb1-xBaxTiO3 thin films prepared by chemical deposition

Highly (100) oriented Pb0.8Ba0.2TiO3/LaNiO3 structures were grown on LaAlO3(100) substrates by using a wet, soft chemical method and crystallized by the microwave oven technique. The Au/PBT/LaNiO3/LaAlO3 capacitor shows a hysteresis loop with remnant polarization, P-r, of 15 muC/cm(2), and coercive field, E-c, of 47 kV/cm at an applied voltage of 3 V, along with a dielectric constant over 1800. Atomic force microscopy showed that Pb0.8Ba0.2TiO3 is composed of large grains about 300 nm. The experimental results demonstrated that the microwave preparation is rapid, clean, and energy efficient. Therefore, we demonstrated that the combination of the soft chemical method with the microwave process is a promising technique to grow highly oriented thin films with excellent dielectric and ferroelectric properties, which can be used in various integrated device applications. (C) 2004 American Institute of Physics.

The effect of Nb doping on ferroelectric properties of PZT thin films prepared from polymeric precursors

Pure and Nb doped PbZr0.4Ti0.603 thin films was prepared by the polymeric precursor method and deposited by spin coating on Pt/Ti/SiO2/Si (100) substrates and annealed at 700 degreesC. The films are oriented in (1 1 0) and (1 0 0) direction. The electric properties of PZT thin films show strong dependence of the crystallographic orientation. The P-E hysteresis loops for the thin film with composition PbZr0.39Ti0.6Nb0.103 showed good saturation, with values for coercive field (E-c) equal to 60 KV cm(-1) and for remanent polarization (P-r) equal to 20 muC cm(-2). The measured dielectric constant (epsilon) is 1084 for this film. These results show good potential for application in FERAM. (C) 2004 Elsevier B.V. All rights reserved.

Dielectric and fatigue properties of Pb(Zr0.53Ti0.47)O-3 thin films prepared from oxide precursors method

Fatigue is an important problem to be considered if a ferroelectric film is used for non-volatile memory devices. In this phenomena, the remanent polarization and coercive field properties degrades in cycles which increase in hysteresis loops. The reasons have been attributed to different mechanisms such as a large voltage applied on ferroelectric film in every reading process in Ferroelectric Random Access Memory (FeRAM) or memories for digital storage in computer, grain size effects and others. The aim of this work is to investigate the influence of the crystallization kinetics on dielectric and ferroelectric properties of the Pb(Zr0.53Ti0.47)O-3 thin films prepared by an alternative chemical method. Films were crystallized in air on Pt/Ti/SiO2/Si substrates at 700 degrees C for 1 hour, in conventional thermal annealing (CTA), and at 700 degrees C for 1 min and 700 degrees C 5 min, using a rapid thermal annealing (RTA) process. Final films were crack free and presented an average of 750 nm in thickness. Dielectric properties were studied in the frequency range of 100 Hz - 1 MHz. All films showed a dielectric dispersion at low frequency. Ferroelectric properties were measured from hysteresis loops at 10 kHz. The obtained remanent polarization (P-r) and coercive field (E-c) were 3.7 mu C/cm(2) and 71.9 kV/cm respectively for film crystallized by CTA while in films crystallized by RTA these parameters were essentially the same. In the fatigue process, the P, value decreased to 14% from the initial value after 1.3 x 10(9) switching cycles, for film by CTA, while for film crystallized by RTA for 5 min, P, decreased to 47% from initial value after 1.7 x 10(9) switching cycles.

AMS and grain shape fabric of the Late Palaeozoic diamictites of the Southeastern Paran Basin, Brazil

Diamictites interbedded with marine shales and turbidites onlap the eastern border of the Parana Basin (Southern Brazil). These poorly sorted sediments were deposited during the Permo-Carboniferous glaciation, and their matrix-supported clasts show no preferred orientation. These massive rocks have been studied using anisotropy of magnetic susceptibility (AMS) and grain shape fabric. Hysteresis loops and thermomagnetic measurements show that AMS depends mostly on the paramagnetic clays, but fine ferromagnetic particles also contribute to the anisotropy. The coarse silt to sand grain preferred orientation study supports the use of AMS in describing the diamictite fabric, at least regarding the orientation of the foliation. AMS and grain shape data reveal subhorizontal to weakly inclined magnetic and grain shape foliation parallel to the regional bedding. The magnetic lineations are normally scattered within the foliation plane in agreement with the oblate AMS ellipsoids found in these rocks. Both fabric patterns are consistent with deposition by subaqueous mudflows that were resedimented downslope, with elastic supply from continental sources. The off-vertical grain shape foliation poles suggest that the deposition of diamictites was controlled by the depocentre topography of the Rio do Sul sub-basin.

Inferior alveolar nerve transposition with involvement of the mental foramen for implant placement

Inferior Alveolar Nerve (IAN) transposition is an option for prosthetic rehabilitation in cases of moderate or even severe bone reabsorption for patients that do not tolerate removable dentures. The aim of the present report is to describe an inferior alveolar nerve transposition with involvement of the mental foramen for implant placement. The surgical procedure was performed under local anesthesia, by the inferior alveolar, lingual and buccal nerve blocking technique. Centripetal osteotomy was performed, and bone tissue was removed, leaving the nerve tissue free in the foramen area. After that, transsection of the incisor nerve was performed, and lateral osteotomy was started from the buccal direction, toward the trajectory of the IAN. The procedure was concluded, by making use of a delicate resin spatula to manipulate the vascular-nervous bundle. The drilling sequence for placing the dental implants was performed, and autogenous bone was harvested using a bone collector attached to the surgical suction appliance. After the implants were placed, the bone tissue previously collected during the osteotomies and drilling processes was placed in order to protect the IAN from contact with the implants. The surgical protocol for inferior alveolar nerve transposition, followed by implant placement presented excellent results, with complete recovery of the sensitivity, seven months after the surgical procedure.

Structure, microstructure, ferroelectric/electromechanical properties and retention characteristics of [Bi1-x Nb (x) ]FeO3 thin films

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