Surface characterization of Ti-7.5Mo alloy modified by biomimetic method

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

Surface characterization of feldspathic ceramic using ATR FT-IR and ellipsometry after various silanization protocols

Objectives. This study characterized the feldspathic ceramic surfaces after various silanization protocols.Methods. Ceramic bars (2 mm x 4 mm x 10 mm) (N = 18) of feldpathic ceramic (VM7, VITA Zahnfabrik) were manufactured and finished. Before silane application, the specimens were ultrasonically cleaned in distilled water for 10 min. The ceramic specimens were randomly divided into nine groups (N = 2 per group) and were treated with different silane protocols. MPS silane (ESPE-Sil, 3M ESPE) was applied to all specimens and left to react at 20 degrees C for 2 min (G20). After drying, the specimens were subjected to heat treatment in an oven at 38 degrees C (G38), 79 degrees C (G79) or 100 degrees C (G100) for 1 min. Half of the specimens of each group were rinsed with water at 80 degrees C for 15 s (G20B, G38B, G79B, G100B). The control group (GC) received no silane. Attenuated total reflection infrared Fourier transform analysis (ATR FT-IR) was performed using a spectrometer. Thickness of silane layer was measured using a spectroscopic ellip-someter working in the lambda = 632.8 nm (He-Ne laser) at 70 degrees incidence angle. Surface roughness was evaluated using an optical profilometer. Specimens were further analyzed under the Scanning Electron Microscopy (SEM) to observe the topographic patterns.Results. ATR FT-IR analysis showed changes in Si-O peaks with enlarged bands around 940 cm(-1). Ellipsometry measurements showed that all post-heat treatment actions reduced the silane film thickness (30.8-33.5 nm) compared to G20 (40 nm). The groups submitted to rinsing in hot water (B groups) showed thinner silane films (9.8-14.4 nm) than those of their corresponding groups (without washing) (30.8-40 nm). Profilometer analysis showed that heat treatments (Ra approximate to 0.10-0.19 mu m; Rq approximate to 0.15-0.26 mu m) provided a smoother surface than the control group (Ra approximate to 0.48 mu m; Rq approximate to 0.65 mu m). Similar patterns were also observed in SEM images.Significance. Heat treatment after MPS silane application improved the silane layer network. Rinsing with boiling water eliminated the outmost unreacted regions of the silane yielding to thinner film thicknesses. (C) 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Surface characterization of absorbing polymer films deposited on transparent glasses

PANI films were deposited on glass substrates by in-situ polymerization and characterized by UV-VIS spectroscopy and atomic force microscopy. A method is developed to accurately analyze ellipsometric data obtained for transparent glass substrates before and after modification with absorbing polymer films. Surface modification was made with an overlayer such as polyaniline ( PANI), which exhibits different optical properties by varying its oxidation state. First, the issue of using transparent substrates for ellipsometry studies was examined and then, spectroscopic ellipsometry was used to characterize absorbing overlayers on transparent glasses. The same methodologies of data analysis can be also applied to other absorbing films on transparent substrates, and deposited by different techniques.

Comparison of Physicochemical Surface Conditioning Methods for Adhesion of bis-GMA Resin Cement to Particulate Filler Composite and Surface Characterization

This study compared the effect of physicochemical surface conditioning methods on the adhesion of bis-GMA-based resin cement to particulate filler composite (PFC) used for indirect dental restorations. PFC blocks (N (block)=54, n (block)=9 per group) were polymerized and randomly subjected to one of the following surface conditioning methods: a) No conditioning (Control-C), b) Hydrofluoric acid (HF)etching for 60s (AE60), c) HF for 90s (AE90), d) HF for 120s (AE120), e) HF for 180s (AE180), and f) air-abrasion with 30 mu m silica-coated alumina particles (AB). The conditioned surfaces were silanized with an MPS silane, and an adhesive resin was applied. Resin composite blocks were bonded to PFC using resin cement and photo-polymerized. PFC-cement-resin composite blocks were cut under coolant water to obtain bar specimens (1mmx0.8mm). Microtensile bond strength test (mu TBS)was performed in a universal testing machine (1mm/min). After debonding, failure modes were classified using stereomicroscopy. Surface characterization was performed on a set of separate specimen surfaces using Scanning Electron Microscopy (SEM), X-Ray Dispersive Spectroscopy (XDS), X-Ray Photoelectron Spectroscopy (XPS), and Fourier Transform-Raman Spectroscopy (FT-RS). Mean mu TBS (MPa) of C (35.6 +/- 4.9) was significantly lower than those of other groups (40.2 +/- 5.6-47.4 +/- 6.1) (p<0.05). The highest mu TBS was obtained in Group AB (47.4 +/- 6.1). Prolonged duration of HF etching increased the results (AE180: 41.9 +/- 7), but was not significantly different than that of AB (p>0.05). Failure types were predominantly cohesive in PFC (34 out of 54) followed by cohesive failure in the cement (16 out of 54). Degree of conversion (DC) of the PFC was 63 +/- 10%. SEM analysis showed increased irregularities on PFC surfaces with the increased etching time. Chemical surface analyses with XPS and FT-RS indicated 11-70% silane on the PFC surfaces that contributed to improved bond strength compared to Group C that presented 5% silane, which seemed to be a threshold. Group AB displayed 83% SiO2 and 17% silane on the surfaces.

Air abrasion before and/or after zirconia sintering: surface characterization, flexural strength, and resin cement bond strength

The purpose of this in vitro study was to evaluate the effect of air-abrasion/zirconia sintering order on the yttria partially stabilized tetragonal zirconia polycrystal (Y-TZP) surface characterization (roughness, morphology, and phase transformation), flexural strength (FS), and shear bond strength (SBS) to a resin cement. Y-TZP specimens were air abraded with 50-μm Al2O3 particles after (AS), before (BS), or before and after zirconia sintering (BAS). For roughness (Ra), 30 block specimens (12×12×3.0 mm; n=10) had their surfaces analyzed by a profilometer. Next, on the air-abraded surfaces of these specimens, composite resin discs (n=30) were bonded with RelyX ARC. The bonded specimens were stored for 24 hours in distilled water at 37°C before shear testing. Failure mode was determined with a stereomicroscope (20×). The surface morphology (n=2) was evaluated by SEM (500×). For the four-point flexural strength test (EMIC DL2000), 39 bar-shaped specimens (20×4.0×1.2 mm; n=13) were air abraded according to the three conditions proposed, and an additional group (nonabraded) was evaluated (n=13). The quantitative analysis of phase transformation (n=1) was completed with Rietveld refinement with X-ray diffraction data. Ra (μm) and SBS (MPa) data were analyzed by one-way analysis of variance (ANOVA) and the Tukey test (α=0.05). Pearson correlation analysis was used to determine if there was a correlation between roughness and SBS. For FS (MPa) data, one-way ANOVA and the Dunnett C-test (α=0.05) were used. The air-abrasion/zirconia sintering order influenced significantly (p<0.001) Ra, SBS, and FS. The BS and AS groups presented the highest (1.3 μm) and the lowest (0.7 μm) Ra. The highest SBS (7.0 MPa) was exhibited by the BAS group, followed by the AS group (5.4 MPa) and finally by the BS group (2.6 MPa). All groups presented 100% adhesive failure. A weak correlation (r=−0.45, p<0.05) was found between roughness and SBS. The air-abrasion/zirconia sintering order provided differences in the surface morphology. The nonabraded (926.8 MPa) and BS (816.3 MPa) groups exhibited statistically similar FS values but lower values than the AS (1249.1 MPa) and BAS (1181.4 MPa) groups, with no significant difference between them. The nonabraded, AS, BS, and BAS groups exhibited, respectively, percentages of monoclinic phase of 0.0 wt%, 12.2 wt%, 0.0 wt%, and 8.6 wt%. The rougher surface provided by the air-abrasion before zirconia sintering may have impaired the bonding with the resin cement. The morphological patterns were consistent with the surface roughness. Considering the short-term SBS and FS, the BAS group exhibited the best performance. Air abrasion, regardless of its performance order, provides tetragonal to monoclinic transformation, while sintering tends to zero the monoclinic phase content.

Surface characterization of lithium disilicate ceramic after nonthermal plasma treatment

Statement of problem. Surface transformation with nonthermal plasma may be a suitable treatment for dental ceramics, because it does not affect the physical properties of the ceramic material.Purpose. The purpose of this study was to characterize the chemical composition of lithium disilicate ceramic and evaluate the surface of this material after nonthermal plasma treatment.Material and methods. A total of 21 specimens of lithium disilicate (10 mm in diameter and 3 mm thick) were fabricated and randomly divided into 3 groups (n=7) according to surface treatment. The control group was not subjected to any treatment except surface polishing with abrasive paper. In the hydrofluoric acid group, the specimens were subjected to hydrofluoric acid gel before silane application. Specimens in the nonthermal plasma group were subjected to the nonthermal plasma treatment. The contact angle was measured to calculate surface energy. In addition, superficial roughness was measured and was examined with scanning electron microscopy, and the chemical composition was characterized with energy-dispersive spectroscopy analysis. The results were analyzed with ANOVA and the Tukey honestly significant difference test (alpha=.05).Results. The water contact angle was decreased to 0 degrees after nonthermal plasma treatment. No significant difference in surface roughness was observed between the control and nonthermal plasma groups. Scanning electron microscopy and energy-dispersive spectroscopy images indicated higher amounts of oxygen (O) and silicon (Si) and a considerable reduction in carbon (C) in the specimens after nonthermal plasma treatment.Conclusions. Nonthermal plasma treatment can transform the characteristics of a ceramic surface without affecting its surface roughness. A reduction in C levels and an increase in 0 and Si levels were observed with the energy-dispersive spectroscopy analysis, indicating that the deposition of the thin silica film was efficient.

Surface characterization and osteoblast-like cells culture on collagen modified PLDLA scaffolds

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

Biological Performance of Chemical Hydroxyapatite Coating Associated With Implant Surface Modification by Laser Beam: Biomechanical Study in Rabbit Tibias

Purpose: Considering the potential of the association between laser ablation and smaller scale hydroxyapatite (HA) coatings to create a stable and bioactive surface on titanium dental implants, the aim of the present study was to determine, by the removal torque test, the effects of a surface treatment created by laser-ablation (Nd:YAG) and, later, thin deposition of HA particles by a chemical process, compared to implants with only laser-ablation and implants with machined surfaces.Materials and Methods: Forty-eight rabbits received I implant by tibia of the following surfaces: machined surface (MS), laser-modified surface (LMS), and biomimetic hydroxiapatite coated surface (HA). After 4, 8, and 12 weeks of healing, the removal torque was measured by a torque gauge. The surfaces studied were analyzed according to their topography, chemical composition, and roughness.Results: Average removal torque in each period was 23.28, 24.0, and 33.85 Ncm to MS, 33.0, 39.87, and 54.57 Ncm to LMS, and 55.42, 63.71 and 64.0 Ncm to HA. The difference was statistically significant (P < .05) between the LMS-MS and HA-MS surfaces in all periods of evaluation, and between LMS-HA to 4 and 8 weeks of healing. The surface characterization showed a deep, rough, and regular topography provided by the laser conditioning, that was followed by the HA coating.Conclusions: Based on these results, it was possible to conclude that the implants with laser surface modification associated with HA biomimetic coating can shorten the implant healing period by the increase of bone implant interaction during the first 2 months after implant placement. (C) 2009 American Association of Oral and Maxillofacial Surgeons J Oral Maxillofac Surg 67:1706-1715, 2009

Evaluation of titanium implants with surface modification by laser beam. Biomechanical study in rabbit tibias

The purpose of the present study was to evaluate, using a biomechanical test, the force needed to remove implants with surface modification by laser (Nd:YAG) in comparison with implants with machined surfaces. Twenty-four rabbits received one implant with each surface treatment in the tibia, machined surface (MS) and laser-modified surface (LMS). After 4, 8 and 12 weeks of healing, the removal torque was measured by a torque gauge. The surfaces studied were analyzed according to their topography, chemical composition and roughness. The average removal torque in each period was 23.28, 24.0 and 33.85 Ncm for MS, and 33.0, 39.87 and 54.57 Ncm for LMS, respectively. The difference between the surfaces in all periods of evaluation was statistically significant (p < 0.05). Surface characterization showed that a deep and regular topography was provided by the laser conditioning, with a great quantity of oxygen ions when compared to the MS. The surface micro-topography analysis showed a statistical difference (p < 0.01) between the roughness of the LMS (R a = 1.38 ± 0.23 μm) when compared to that of the MS (R a = 0.33 ± 0.06 μm). Based on these results, it was possible to conclude that the LMS implants' physical-chemical properties increased bone-implant interaction when compared to the MS implants. © 2009 Sociedade Brasileira de Pesquisa Odontológica.

Soft-chemical synthesis, characterization and humidity sensing behavior of WO3/TiO2 nanopowders

Tungsten oxide/titania (WO3/TiO2) nanopowders were synthesized by the polymeric precursor method which varied the WO3 content between 0 and 10 mol%. The powders were thermally treated in a conventional furnace and their structural, microstructural and electric properties were evaluated by X-ray diffraction (XRD), Raman spectrometry, N 2 physisorption, NH3 chemisorption, temperature-programmed reduction (TPR), X-ray absorption near-edge spectroscopy (XANES) in situ XANES and extended X-ray absorption fine structure spectroscopy (EXAFS) and transmission electron microscopy (TEM). XRD and Raman spectrometry confirmed the homogeneous distribution of an amorphous WO3 phase in the TiO 2 matrix which stabilized the anatase phase through the generation of [TiO5·V0] or [TiO5·V 0] complex sites. Conventional TPR-H2 (temperature programmed reduction) along with XANES TPR-H2 and XANES TPR-EtOH showed that WO3/TiO2 sample reduction occurs through the formation of these complex clusters. Moreover, the addition of WO3 promoted an increase in the surface acidity of doped samples as revealed by NH3 chemisorption. The WO3/TiO2 bulk-ceramic samples were further used to estimate their potential application in a humidity sensor in the range of 15-85% relative humidity. Probable reasons that lead to the different humidity sensor responses of samples were given based on the structural and surface characterizations. Correlation between the sensing performance of the sensor and its structural features are also discussed. Although all samples responded as a humidity sensor, the W2T sample (2 mol% added WO3) excelled for sensitivity due to the increase in acid sites, optimum mean pore size and pore size distribution. © 2013 Elsevier B.V.

Relationship between the surface chemical composition of implants and contact with the substrate

The purpose of the study was to use scanning electron microscopy and energy dispersive x-ray spectrometry to assess possible morphologic and chemical changes after performing double-insertion and pullout tests of implants of different shapes and surface treatments. Four different types of implants were used—cylindrical machined-surface implants, cylindrical double-surface–treated porous implants, cylindrical surface-treated porous implants, and tapered surface-treated porous implants—representing a total of 32 screws. The implants were inserted into synthetic bone femurs, totaling 8 samples, before performing each insertion with standardized torque. After each pullout the implants were analyzed by scanning electron microscopy and energy dispersive x-ray spectrometry using a universal testing machine and magnified 35 times. No structural changes were detected on morphological surface characterization, only substrate accumulation. As for composition, there were concentration differences in the titanium, oxygen, and carbon elements. Implants with surface acid treatment undergo greater superficial changes in chemical composition than machined implants, that is, the greater the contact area of the implant with the substrate, the greater the oxide layer change. In addition, prior manipulation can alter the chemical composition of implants, typically to a greater degree in surface-treated implants.

Stability of cp-Ti and Ti-6Al-4V alloy for dental implants as a function of saliva pH - an electrochemical study

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Response of human alveolar bone-derived cells to a novel poly(vinylidene fluoride-trifluoroethylene)/barium titanate membrane

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

Morphology and topography analysis of mesoporous titania templated by micrometric latex sphere arrays

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

Synthesis and electrochemical behavior of single-crystal magnetite nanoparticles

Water-dispersed magnetite nanoparticle synthesis from iron(II) chloride in dimethyl sulfoxide (DMSO)-water solution at different DMSO-water ratios in alkaline medium was reported. TEM and XRD results suggest a single-crystal formation with mean particle size in the range 4-27 nm. Magnetic nanoparticles are formed by the oxidative hydrolysis reaction from green rust species that leads to FeOOH formation, followed by autocatalysis of the adsorbed available Fe(II) on the FeOOH surfaces. The available hydroxyl groups seem to be dependent on the DMSO-water ratio due to strong molecular interactions presented by the solvent mixture. Goethite phase on the magnetite surface was observed by XRD data only for sample synthesized in the absence of DMSO. In addition, cyclic voltammetry with carbon paste electroactive electrode (CV-CPEE) results reveal two reduction peaks near 0 and +400 mV associated with the presence of iron(III) in different chemical environments related to the surface composition of magnetite nanoparticles. The peak near +400 mV is related to a passivate thin layer surface such as goethite on the magnetite nanoparticle, assigned to the intensive hydrolysis reaction due to strong interactions between DMSO-water molecules in the initial solvent mixture that result in a hydroxyl group excess in the medium. Pure magnetite phase was only observed in the samples prepared at 30% (30W) and 80% (80W) water in DMSO in agreement with the structured molecular solvent cluster formation. The goethite phase present on the, magnetite nanoparticle surface like a thin passivate layer only was detectable using CV-CPEE, which is a very efficient, cheap, and powerful tool for surface characterization, and it is able to determine the passivate oxyhydroxide or oxide thin layer presence on the nanoparticle surface.