Surface modification of Ti dental implants by Nd: YVO4 laser irradiation

Surface modifications have been applied in endosteal bone devices in order to improve the osseointegration through direct contact between neoformed bone and the implant without an intervening soft tissue layer. Surface characteristics of titanium implants have been modified by addictive methods, such as metallic titanium, titanium oxide and hydroxyapatite powder plasma spray, as well as by subtractive methods, such as acid etching, acid etching associated with sandblasting by either AlO2 or TiO2, and recently by laser ablation. Surface modification for dental and medical implants can be obtained by using laser irradiation technique where its parameters like repetition rate, pulse energy, scanning speed and fluency must be taken into accounting to the appropriate surface topography. Surfaces of commercially pure Ti (cpTi) were modified by laser Nd:YVO4 in nine different parameters configurations, all under normal atmosphere. The samples were characterized by SEM and XRD refined by Rietveld method. The crystalline phases alpha Ti, beta Ti, Ti6O, Ti3O and TiO were formed by the melting and fast cooling processes during irradiation. The resulting phases on the irradiated surface were correlated with the laser beam parameters: the aim of the present work was to control titanium oxides formations in order to improve implants osseointegration by using a laser irradiation technique which is of great importance to biomaterial devices due to being a clean and reproducible process. (c) 2007 Elsevier B.V. All rights reserved.

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.

Magnetic properties of acicular Fe1-xREx (RE = Nd, Sm, Eu, Tb; x=0, 0.05, 0.10) metallic nanoparticles

Acicular monodispersed Fe1-xREx (RE= Nd, Sm,Eu,Tb;x=0, 0.05, 0.10) metallic nanoparticles (60 +/- 5 nm in length and axial ratio similar to6) obtained by reduction of alumina-coated goethite nanoparticles-containing rare earth (RE) under hydrogen flow are reported. Alumina and maghemite thin layers on particle surface were used to protect the goethite particles against sintering and oxidation, respectively. Al and RE additions were obtained by successive heterocoagulation reactions. Aluminum sulfate (10 at.% based on Fe) was dissolved in water and the pH adjusted to 12.5 with NaOH solution. Goethite particles were suspended in this solution and CO2 gas was blown into the slurry to neutralize it to a pH 8.5 or less. Particles were purified and dehydrated to effect transformation to alumina-coated hematite nanoparticles, which were re-suspended in aqueous solution in which RE sulfate (0-0.15 at.% based on Fe) has been dissolved, and the pH increased by ammonia aqueous solution addition. Resulted alumina-coated RE-doped hematite nanoparticles were reduced to metal at 450 degreesC/12 h under hydrogen flow and passivated with nitrogen-containing ethanol vapor at room temperature. Acicular monodispersed metallic nanoparticle systems were obtained and the presence of Al and RE were confirmed by induced-coupled plasma spectrometry analysis. X-ray diffraction, Mossbauer spectroscopy, and magnetization data are in agreement with the nanosized alpha-Fe core in a bcc structure, having a spinel structure, gammaFe(2)O(3), with thickness similar to1.5 run on particle surface. Main magnetic parameters showed saturation magnetization decreases and significant increasing in the coercive field with the RE composition increases. Magnetic properties of these particles, similar to40% smaller than those commercially available, suggest a decrease in the bit-size for high-density magnetic or magneto-optics recording media application. (C) 2004 Published by Elsevier B.V.

Flow injection AAS determination of Cd, Cu, and Pb at trace levels in wine using solid phase extraction

A comparative study is reported between C-18 bonded silica gel and powdered polyethylene (PE) as sorbent for Cd, Cu, and Pb determination using ammonium diethyldithiophosphate (ADTP) as the complexing agent in a flow injection system. The complexes were formed in 0.14 mol L-1 HNO3 and processed in a simple flow system comprising a peristaltic pump, a manual injector-commutator, and a sorbent-packed minicolumn. Ethanol was selected as the eluent and analytes in the eluate were determined by flame atomic absorption spectrometry. The optimum concentration of the complexing agent was 0.1% (m/v) ADTP for Cu and Pb determination using either C-18 or PE, and 0.25% (m/v) ADTP for Cd determination using PE. The sample loading flow rates were 5.0, 3.6, and 3.0 mL min(-1) for Cu, Pb, and Cd, respectively. The best elution flow rate was 6.5 mL min(-1). For a 60-sec preconcentration time, the sampling rate was 40 h(-1) and the enrichment factors of 33, 36, and 11 times (C-18) or 18, 22, and 23 times (PE) were obtained for Cu, Pb, and Cd, respectively. The limits of detection (LOD) were 1.6 mug L-1 Cu, 11 mug L-1 Pb, and 2.0 mug L-1 Cd using C-18 or 2.9 mug L-1 Cu, 19 mug L-1 Pb, and 1.0 mug L-1 Cd using PE, respectively. The relative standard deviations (n = 12) were typically <2%, <2%, and <6% for Cd, Cu, and Pb, respectively. The recoveries of Cd, Cu, and Pb added to wine samples varied from 96-99%, 97-102%, and 90-99%, respectively, using C-18 or PE. Accuracy was checked for Cd, Cu, and Pb determination in six wine samples digested by block digestor and open-vessel microwave-assisted digestion systems. The results revealed that C-18 was more efficient for Cu and Pb determination, while PE was the best sorbent for Cd.

Enamel caries resistance accidentally irradiated by the Nd : YAG laser

When the carious tissue is eliminated either by conventional methods (with burs) or with lasers, the risk of accidentally damage the surface of adjacent teeth may occur, which hypothetically could lead to a more susceptible surface for canes formation. This in vitro study aims to evaluate the caries resistance of the dental enamel surface irradiated by the Nd:YAG laser applied in conditions simulating accidental exposition. Thirteen third molars were used in this study. The experimental groups were: G1: sound control and control + carious; G2: contact Nd:YAG laser at 0.75, 1, 2, or 3 W; 10 Hz; 3 sec (27, 35, 71, and 106 J/cm(2)); G3: same parameters from G2 + caries artificial induction through the demineralization and demineralization (DES/RE) dynamic model. The caries resistance analysis was evaluated by the superficial morphological aspect through SEM images and also by Ca/P proportion through energy dispersive X-ray spectroscopy (EDX). The micrograph images showed that the Nd:YAG laser changed the normalmorphology of the enamel prisms resulting in a melted and re-solidified surface intensified with the power increase. Significant statistical differences were observed applying the Kruskal-Wallis statistical test (p <= 0.01) among the Nd:YAG laser irradiated groups and the control with caries regarding the Ca/P proportion. As an exception, this was not observed when 3 W; 10 Hz; 3 sec; 106 J/cm(2) was applied and posteriously submitted to a cariogenic challenge. The results indicate that the Nd:YAG laser accidental irradiation at low power settings did not represent risks to the enamel caries resistance.

Microstructure and electrical properties of perovskite (Pb, La)TiO3 thin film deposited at low temperature by the polymeric precursor method

High-quality (Pb, La)TiO3 ferroelectric thin films were successfully prepared on a Pt(111)/Ti/SiO2/Si(100) substrate for the first time by spin coating, using the polymeric precursor method. The X-ray diffraction patterns show that the films are polycrystalline in nature. This method allows for low temperature (500 degrees C) synthesis, a high quality microstructure and superior dielectric properties. The effects on the microstructure and electrical properties were studied by changing the La content. The films annealed at 500 degreesC have a single perovskite phase with only a tetragonal or pseudocubic structure. As the La content is increased, the dielectric constant of PLT thin films increases from 570 up to 1138 at room temperature. The C-V and P-E characteristics of perovskite thin films prepared at a low temperature show normal ferroelectric behavior, representing the ferroelectric switching property. The remanent polarization and coercive field of the films deposited decreased due to the transformation from the ferroelectric to the paraelectric phase with an increased La content. (C) 2001 Kluwer Academic Publishers.

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.

Synthesis, ferroelectric and optical properties of (Pb,Ca)TiO3 thin films by soft solution processing

Calcium modified lead titanate sol was synthesized using a soft solution processing, the so-called polymeric precursor method. In soft chemistry method, soluble precursors such as lead acetate trihydrate, calcium carbonate and titanium isopropoxide, as starting materials, were mixed in aqueous solution. Pb0.7Ca0.3TiO3 thin films were deposited on platinum-coated silicon and quartz substrates by means of the spinning technique. The surface morphology and crystal structure, dielectric and optical properties of the thin films were investigated. The electrical measurements were conducted on metal-ferroelectric-metal (MFM) capacitors. The typical measured small signal dielectric constant and dissipation factor at a frequency of 100 kHz were 299 and 0.065, respectively, for a thin film with 230 nm thickness annealed at 600degreesC for 2 h. The remanent polarization (2P(r)) and coercive field (E-c) were 32 muC/cm(2) and 100 kV/cm, respectively. Transmission spectra were recorded and from them, refractive index, extinction coefficient, and band gap energy were calculated. Thin films exhibited good optical transmissivity, and had optical direct transitions. The present study confirms the validity of the DiDomenico model for the interband transition, with a single electronic oscillator at 6.858 eV. The optical dispersion behavior of PCT thin film was found to fit well the Sellmeir dispersion equation. The band gap energy of the thin film, annealed at 600degreesC, was 3.56 eV. The results confirmed that soft solution processing provides an inexpensive and environmentally friendly route for the preparation of PCT thin films.

Influence of Ca concentration on the electric, morphological, and structural properties of (Pb,Ca)TiO3 thin films

Pb1-xCaxTiO3 (0.10less than or equal toxless than or equal to0.40) thin films on Pt/Ti/SiO2/Si(100) substrates were prepared by the soft solution process and their characteristics were investigated as a function of the calcium content (x). The structural modifications in the films were studied using x-ray diffraction and micro-Raman scattering techniques. Lattice parameters calculated from x-ray data indicate a decrease in lattice tetragonality with the increasing content of calcium in these films. Raman spectra exhibited characteristic features of pure PbTiO3 thin films. Variations in the phonon mode wave numbers, especially those of lower wave numbers, of Pb1-xCaxTiO3 thin films as a function of the composition corroborate the decrease in tetragonality caused by the calcium doping. As the Ca content (x) increases from 0.10 to 0.40, the dielectric constant at room temperature abnormally increased at 1 kHz from 148 to 430. Also calcium substitution decreased the remanent polarization and coercive field from 28.0 to 5.3 muC/cm(2) and 124 to 58 kV/cm, respectively. These properties can be explained in terms of variations of phase transition (ferroelectric-paraelectric), resulting from the substitution the lead site of PbTiO(3)for the nonvolatile calcium. (C) 2002 American Institute of Physics.

SrSnO3:Nd obtained by the polymeric precursor method

In this work, the synthesis of Nd-doped SrSnO3 by the polymeric precursor method, with calcination between 250 and 700 A degrees C is reported. The powder precursors were characterized by TG/DTA and high temperature X-ray diffraction (HTXRD). After heat treatment, the material was characterized by XRD and infrared spectroscopy. Ester and carbonate amounts were strictly related to Nd-doping. According to XRD patterns, the orthorhombic perovskite was obtained at 700 A degrees C for SrSnO3 and SrSn0.99Nd0.01O3. For Sr0.99Nd0.01SnO3, the kinetics displayed an important hole in the crystallization process, as no peak was observed in HTXRD up to 700 A degrees C, while a XRD patterns showed a crystalline material after calcination at 250 A degrees C.

Structural deformation monitored by vibrational properties and orbital modeling in (Pb,Sm)TiO3 systems

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Paper-based diffusive gradients in thin films technique coupled to energy dispersive X-ray fluorescence spectrometry for the determination of labile Mn, Co, Ni, Cu, Zn and Pb in river water

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

Thermal and structural characterization of SrTi(1-x)Nd(x)O(3)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)