Density improvement of the sol-gel dip-coated SnO2 films by chemical surface modification

We compare the effect of organic (Tiron (R)) and inorganic (Mn(11)) additives on the low temperature (< 600 degrees C) densification of the sol-gel dip-coated SnO2 films. The structural and compositional properties of the samples were investigated by X-ray reflectometry (XRR), X-ray absorption spectroscopy (XAS) and X-ray photoelectron spectroscopy (XPS). The results suggest that the replacement of hydroxyl groups at the particle surface by Tiron (R) reduces the level of agglomeration of the sol, increasing the particles packing and the apparent density of the coatings. Undoped and Mn-doped films drawn from a Tiron (R) containing suspension show after firing at 500 degrees C a porosity reduction of 12 and 8.6%, respectively. The porosity decrease is less pronounced (4.3%) for the film without additives. Both XAS and XPS data show the presence of trivalent manganese. The formation of a non-homogeneous solid solution characterised by the presence of Mn(111) replacing tin atom near to the crystallite surface was evidenced by XAS. Additionally, XPS results reveal the presence of metallic Sn at the surface of films containing Tirono. (c) 2005 Elsevier Ltd. All rights reserved.

Corrosion protection of fluorzirconate glasses coated by a layer of surface modified tin oxide nanoparticles

The protection efficiency against water corrosion of fluorozirconate glass, ZBLAN, dip-coated by nanocrystalline tin oxide film containing the organic molecule Tiron® was investigated by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). The chemical bonding structure of the surface region and morphology were studied before and after two water exposure periods of 5 and 30 min. The results of the analysis for the as-grown sample revealed a SnO1.6 phase containing carbon and sulfur, related to Tiron®, and traces of elements related to ZBLAN (Zr, F, Ba). This fact and the clear evidence of the presence of tin oxifluoride specie (SnOxF y) indicates a diffusion of the glass components into the porous coating. After water exposure, the increase of the oxygen concentration accompanied by a strong increase of Zr, F, Ba and Na content is interpreted as filling of the nanopores of the film by glass compounds. The formation of a compact protective layer is supported by the morphological changes observed by AFM. © 2005 Elsevier B.V. All rights reserved.

Concentration of Cu(II) and Cd(II) from natural river water by Adsorption on a Modified Silica Surface

A high surface area silica gel (737 ± m2 g-1) was synthesized modified through a two-step reaction with a 4-amino-2-mercaptopyrimidine ligand and applied to Cu(II) and Cd(II) adsorption from an aqueous medium. The modified material was characterized by FTIR, which showed that attachment of the molecule occurred via thiol groups at 2547 and 2600 cm-1, and by elemental analysis that indicated the presence of 0.0102 mmol of ligand. The data from adsorption experiments were adjusted to a modified Langmuir equation and the maximum adsorption capacity was 6.6 and 3.8 μmol g-1 for Cu(II) and Cd(II), respectively. After adjusting several parameters, the material was applied in the preconcentration of natural river water using a continuous flow system before and after sample mineralization, and the results showed a 10-fold enrichment factor. The proposed method was validated through preconcentration and analysis of certified standard reference material (1643e), whose results were in agreement with the values provided by the manufacturer.

Study of polypropylene surface modification by air dielectric barrier discharge operated at two different frequencies

In this work, air dielectric barrier discharge (DBD) operating at the line frequency (60 Hz) or at frequency of 17 kHz was used to improve the wetting properties of polypropylene (PP). The changes in the surface hydrophilicity were investigated by contact angle measurements. The plasma-induced chemical modifications of PP surface were studied by X-ray photoelectron spectroscopy (XPS) and Fourier-transformed infrared spectroscopy (FTIR). The polymer surface morphology and roughness before and after the DBD treatment were analyzed by atomic force microscopy (AFM). To compare the plasma treatment effect at different frequencies the variation of the contact angle is presented as a function of the deposited energy density. The results show that both DBD treatments leaded to formation of water-soluble low molecular weight oxidized material (LMWOM), which agglomerated into small mounts on the surface producing a complex globular structure. However, the 60 Hz DBD process produced higher amount of LMWOM on the PP surface comparing to the 17 kHz plasma treatment with the same energy dose. The hydrophilic LMWOM is weakly bounded to the surface and can be easily removed by polar solvents. After washing the DBD-treated samples in de-ionized water their surface roughness and oxygen content were reduced and the PP partially recovered its original wetting characteristics. This suggested that oxidation also occurred at deeper and more permanent levels of the PP samples. Comparing both DBD processes the 17 kHz treatment was found to be more efficient in introducing oxygen moieties on the surface and also in improving the PP wetting properties. © 2012 Elsevier B.V. All rights reserved.

Plasma treatment maintains surface energy of the implant surface and enhances osseointegration

The surface energy of the implant surface has an impact on osseointegration. In this study, 2 surfaces: nonwashed resorbable blasting media (NWRBM; control) and Ar-based nonthermal plasma 30 days (Plasma 30 days; experimental), were investigated with a focus on the surface energy. The surface energy was characterized by the Owens-Wendt-Rabel-Kaelble method and the chemistry by X-ray photoelectron spectroscopy (XPS). Five adult beagle dogs received 8 implants (n = 2 per surface, per tibia). After 2 weeks, the animals were euthanized, and half of the implants (n = 20) were removal torqued and the other half were histologically processed (n = 20). The bone-to-implant contact (BIC) and bone area fraction occupancy (BAFO) were evaluated on the histologic sections. The XPS analysis showed peaks of C, Ca, O, and P for the control and experimental surfaces. While no significant difference was observed for BIC parameter (P > 0.75), a higher level for torque (P < 0.02) and BAFO parameter (P < 0.01) was observed for the experimental group. The surface elemental chemistry was modified by the plasma and lasted for 30 days after treatment resulting in improved biomechanical fixation and bone formation at 2 weeks compared to the control group. © 2013 Fernando P. S. Guastaldi et al.

Geochemical and ecotoxicological assessment for estuarine surface sediments from Southern Brazil

Sediments from Guaratuba Bay (PR, Brazil), a marine protected area, were collected and evaluated for geochemistry and toxicity. High levels of P and acute toxicity were observed in some samples. Concentrations of Cu, Cd, Pb and Zn were relatively low; however, Cd levels eventually exceeded Threshold Effect Level. Toxicities were associated to nutrients and metals enrichment. Results suggest that impacts are incipient and occur only at specific sites, associated to multiple contamination sources. Despite sediments quality seems to range between good and fair, attention is required to land-use planning around Guaratuba Bay and controlling local pollution sources. © 2013 Elsevier Ltd. All rights reserved.

The reactive surface of Castor leaf [Ricinus communis L.] powder as a green adsorbent for the removal of heavy metals from natural river water

In this study, a green adsorbent was successfully applied to remove toxic metals from aqueous solutions. Dried minced castor leaves were fractionated into 63-μm particles to perform characterization and extraction experiments. Absorption bands in FTIR (Fourier Transform Infrared Spectroscopy) spectra at 1544, 1232 and 1350 cm-1 were assigned to nitrogen-containing groups. Elemental analysis showed high nitrogen and sulfur content: 5.76 and 1.93%, respectively. The adsorption kinetics for Cd(II) and Pb(II) followed a pseudo-second-order model, and no difference between the experimental and calculated Nf values (0.094 and 0.05 mmol g-1 for Cd(II) and Pb(II), respectively) was observed. The Ns values calculated using the modified Langmuir equation, 0.340 and 0.327 mmol g-1 for Cd(II) and Pb(II), respectively, were superior to the results obtained for several materials in the literature. The method proposed in this study was applied to pre-concentrate (45-fold enrichment factor) and used to measure Cd(II) and Pb(II) in freshwater samples from the Paraná River. The method was validated through a comparative analysis with a standard reference material (1643e). © 2013 Elsevier B.V. © 2013 Elsevier B.V. All rights reserved.

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.

Effect of Abutment Screw Surface Treatment on Reliability of Implant-Supported Crowns

Purpose: To evaluate and compare the reliability of implant-supported single crowns cemented onto abutments retained with coated (C) or noncoated (NC) screws and onto platform-switched abutments with coated screws. Materials and Methods: Fifty-four implants (DT Implant 4-mm Standard Platform, Intra-Lock International) were divided into three groups (n = 18 each) as follows: matching-platform abutments secured with noncoated abutment screws (MNC); matching-platform abutments tightened with coated abutment screws (MC); and switched-platform abutments secured with coated abutment screws (SC). Screws were characterized by scanning electron microscopy and x-ray photoelectron spectroscopy (XPS). The specimens were subjected to step-stress accelerated life testing. Use-level probability Weibull curves and reliability for 100,000 cycles at 200 N and 300 N (90% two-sided confidence intervals) were calculated. Polarized light and scanning electron microscopes were used for fractographic analysis. Results: Scanning electron microscopy revealed differences in surface texture; noncoated screws presented the typical machining grooves texture, whereas coated screws presented a plastically deformed surface layer. XPS revealed the same base components for both screws, with the exception of higher degrees of silicon in the SiO2 form for the coated samples. For 100,000 cycles at 300 N, reliability values were 0.06 (0.01 to 0.16), 0.25 (0.09 to 0.45), and 0.25 (0.08 to 0.45), for MNC, MC, and SC, respectively. The most common failure mechanism for MNC was fracture of the abutment screw, followed by bending, or its fracture, along with fracture of the abutment or implant. Coated abutment screws most commonly fractured along with the abutment, irrespective of abutment type. Conclusion: Reliability was higher for both groups with the coated screw than with the uncoated screw. Failure modes differed between coated and uncoated groups.

Characterization of metal-biomass interactions in the lanthanum(III) biosorption on Sargassum sp using SEM/EDX, FTIR, and XPS: Preliminary studies

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Sugarcane bagasse cellulose fibres and their hydrous niobium phosphate composites: synthesis and characterization by XPS, XRD and SEM

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

Surface modification of polymeric materials by cold atmospheric plasma jet

In this work we report the surface modification of different engineering polymers, such as, polyethylene terephthalate (PET), polyethylene (PE) and polypropylene (PP) by an atmospheric pressure plasma jet (APPJ). It was operated with Ar gas using 10 kV, 37 kHz, sine wave as an excitation source. The aim of this study is to determine the optimal treatment conditions and also to compare the polymer surface modification induced by plasma jet with the one obtained by another atmospheric pressure plasma source the dielectric barrier discharge (DBD). The samples were exposed to the plasma jet effluent using a scanning procedure, which allowed achieving a uniform surface modification. The wettability assessments of all polymers reveal that the treatment leads to reduction of more than 40 degrees in the water contact angle (WCA). Changes in surface composition and chemical bonding were analyzed by x-ray photoelectron spectroscopy (XPS) and Fourier-Transformed Infrared spectroscopy (FTIR) that both detected incorporation of oxygen-related functional groups. Surface morphology of polymer samples was investigated by Atomic Force Microscopy (AFM) and an increase of polymer roughness after the APPJ treatment was found. The plasma-treated polymers exhibited hydrophobic recovery expressed in reduction of the O-content of the surface upon rinsing with water. This process was caused by the dissolution of low molecular weight oxidized materials (LMWOMs) formed on the surface as a result of the plasma exposure. (C) 2014 Elsevier B.V. All rights reserved.

Oxide surface modification: Synthesis and characterization of zirconia-coated alumina

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