Methanol oxidation on PtRu/C electrocatalysts prepared by a microemulsion method

PtRu/C nanocatalysts were prepared by a microemulsion method using different values of water/surfactant molar ratio in order to get different particle sizes. Crystallite sizes and structural properties were determined by X-ray diffraction. Particle size and distribution were characterized by transmission electron microscopy and average composition was determined by energy dispersive X-ray analysis. Differential scanning calorimetry measurements indicated the presence of oxides in the as-prepared catalysts. The general electrochemical behavior was evaluated by cyclic voltammetry in 0.5 M sulfuric acid and the electrocatalytic activity towards the oxidation of methanol was studied in 0.5 M methanol acid solutions by potential sweeps and chronoamperometry. copyright The Electrochemical Society.

Investigation of the metal/porcelain interface in LASER-welded Ni-Cr-Mo alloy

The interface formed between the metal and the porcelain of laser-welded Ni-Cr-Mo alloy was studied on a metallurgical basis. The characterization was carried out by using optical microscope, electron scan microscopy and X-ray dispersive spectroscopy techniques and mechanical three-point flexion tests, in the laser-welded region, with and without porcelain. The union of the porcelain with the alloy is possible only after the oxidation of the metallic surface and the subsequent application of a bonding agent known as opaque. The porcelain applied to the base metal and weld bead showed different behaviours - after the flexion test, the base metal showed cracks, while that in the weld bead broke away completely. It was noted that the region subjected to laser welding had lower adherence to the porcelain than the base metal region, due to microstructural refinement of the weld bead. These results can be shown by the X-ray dispersive spectroscopy carried out on the regions studied. The flexion tests demonstrated that the Ni-Cr-Mo alloy subject to laser welding had significant alterations in its mechanical properties after application of the porcelain.

Precipitates segmentation from scanning electron microscope images through machine learning techniques

The presence of precipitates in metallic materials affects its durability, resistance and mechanical properties. Hence, its automatic identification by image processing and machine learning techniques may lead to reliable and efficient assessments on the materials. In this paper, we introduce four widely used supervised pattern recognition techniques to accomplish metallic precipitates segmentation in scanning electron microscope images from dissimilar welding on a Hastelloy C-276 alloy: Support Vector Machines, Optimum-Path Forest, Self Organizing Maps and a Bayesian classifier. Experimental results demonstrated that all classifiers achieved similar recognition rates with good results validated by an expert in metallographic image analysis. © 2011 Springer-Verlag Berlin Heidelberg.

Conductive nanocomposites based on cellulose nanofibrils coated with polyaniline-DBSA via in situ polymerization

Cellulose nanofibrils (CNF) were extracted by acid hydrolysis from cotton microfibrils and nanocomposites with polyaniline doped with dodecyl benzenesulphonic acid (PANI-DBSA) were obtained by in situ polymerization of aniline onto CNF. The ratios between DBSA to aniline and aniline to oxidant were varied in situ and the nanocomposites characterized by four probe DC electrical conductivity, ultraviolet-visible-near infrared (UV-Vis - NIR) and Fourier-transform infrared (FTIR) spectroscopies and X-ray diffraction (XRD). FTIR and UV-Vis/NIR characterization confirmed the polymerization of PANI onto CNF surfaces. Electrical conductivity of about 10 -1 S/cm was achieved for the composites; conductivity was mostly independent of DBSA/aniline (between 2 and 4) and aniline/oxidant (between 1 and 5) molar ratios. X-ray patterns of the samples showed crystalline peaks characteristic of cellulose I for CNF samples, and a mixture of both characteristic peaks of PANI and CNF for the nanocomposites. Field emission scanning electron microscopy (FESEM) characterization corroborated the abovementioned results showing that PANI coated the surface of the nanofibrils. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Caracterização morfométrica de sementes e plântulas e germinação de anadenanthera macrocarpa (benth.) brenan

Anadenanthera macrocarpa (Benth.) Brenan is a tree species belonging to the family Leguminosae-Mimosoideae which is popularly known as mimosa-black. It features characteristics of early successional, natural occurrence in Brazil and can form clusters almost homogeneous, with great potential in the recovery of degraded areas. This study was conducted at the Center for Agricultural Sciences, University Federal of Alagoas state, aiming at the physical and morphological characterization of seeds, describing the various stages of post-seminal development, and to evaluate various conditions of temperature and substrate to perform the test germination. The seeds were manually extracted, then homogenized, where two samples of 50 seeds were used to determine the initial moisture. Another sample, consisting of eight repetitions of 100 seeds was used to measure the biometry and the number of seeds per fruit. The morphological characterization and the seeds were immersed in distilled water to allow the cuts to the observed structure in microscopes. In the post-seminal study, it was observed the daily processes of seedling growth in rolled paper filter and constant temperature of 30 °C. To assess the germination behavior, the constant temperatures of 15 °C, 25 °C, 30 °C, 40 °C and 20-30 °C as well as the paper and the sand substrates were tested and it was evaluated the percentage, the rate of germination, the relative frequency distribution, and the tests conducted in a randomized design in factorial 5 x 2 (x substrate temperature) with four replicates of 25 seeds, and the averages compared by Duncan 5 % probability. The fruits of black angico show great variation in the seed number per fruit. The embryonic axis occupies part of the central region of the seed with axial and linear positions. The germination is epigeal and the seedlings are fanerocotylar. The temperature determines the 30 °C and the filter paper substrate provided higher average percentage and germination rate.

High-pressure assisted sintering of Ti-20Si-10B and Ti-10Si-5B powders

This work presents the structural characterization of Ti-10Si-5B and Ti-20Si-10B (at-%) alloys produced by high-pressure assisted sintering. Sintering was performed in air at 1100 and 1200°C for 60 s using pressure levels of 5 GPa. Structural evaluation of sintered samples was conducted by means of scanning electron microscopy and energy dispersive spectrometry. Samples were successfully consolidated after sintering, which presented theoretical density values higher than 99%. The microstructures of the sintered Ti-10Si-5B and Ti-20Si-10B alloys revealed the presence of the TiSS, TiB, TiB2, Ti5Si3, Ti5Si4, TiSi, and TiSi2.phases. A small amount of Ti6Si2B was formed after high-pressure assisted sintering of the Ti-20Si-10B alloy (5GPa, 1100°C for 60 s) indicating that equilibrium structures were not achieved during short sintering times. No oxygen and carbon contamination was detected in structures of Ti-Si-B alloys after high-pressure sintering at 1100 and 1200°C without controlled atmosphere. © (2012) Trans Tech Publications, Switzerland.

Growth mechanism and photocatalytic properties of SrWO4 microcrystals synthesized by injection of ions into a hot aqueous solution

This paper reports our initial research to obtain SrWO4 microcrystals by the injection of ions into a hot aqueous solution and their photocatalytic (PC) properties. These microcrystals were structurally characterized by X-ray diffraction (XRD), Rietveld refinements and Fourier transform (FT)-Raman spectroscopy. The shape and average size of these SrWO 4 microcrystals were observed by field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). In addition, we have investigated the PC activity of microcrystals for the degradation of rhodamine B (RhB) and rhodamine 6G (Rh6G) dyes. XRD patterns, Rietveld refinement data and FT-Raman spectroscopy confirmed that SrWO4 microcrystals have a scheelite-type tetragonal structure without deleterious phases. FT-Raman spectra exhibited 12 Raman-active modes in a range from 50 to 1000 cm-1. FE-SEM and TEM images suggested that the SrWO4 microcrystals (rice-like - 95%; star-, flower-, and urchin-like - 5%) were formed by means of primary/secondary nucleation events and self-assembly processes. Based on these FE-SEM/TEM images, a crystal growth mechanism was proposed and discussed in details in this work. Finally, a good PC activity was first discovered of the SrWO4 microcrystals for the degradation of RhB after 80 min and Rh6G after 50 min dyes under ultraviolet-light, respectively. © 2012 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder.

Low-temperature synthesis of nanosized bismuth ferrite by the soft chemical method

This paper describes research on a simple low-temperature synthesis route to prepare bismuth ferrite nanopowders by the polymeric precursor method using bismuth and iron nitrates. BiFeO 3 (BFO) nanopowders were characterized by means of X-ray diffraction analyses, (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy (Raman), thermogravimnetric analyses (TG-DTA), ultra-violet/vis (UV/Vis) and field emission scanning electron microscopy (FE-SEM). XRD patterns confirmed that a pure perovskite BiFeO 3 structure with a rhombohedral distorted perovskite structure was obtained by heating at 850 °C for 4 hours. Typical FT-IR spectra for BFO powders revealed the formation of a perovskite structure at high temperatures due to a metal-oxygen bond while Raman modes indicated oxygen octahedral tilts induced by structural distortion. A homogeneous size distribution of BFO powders obtained at 850 °C for 4 hours was verified by FE-SEM analyses. © 2012 Elsevier Ltd and Techna Group S.r.l.

Effect of microthread presence and restoration design (screw versus cemented) in dental implant reliability and failure modes

Objectives: This study evaluated the reliability and failure modes of implants with a microthreaded or smooth design at the crestal region, restored with screwed or cemented crowns. The postulated null hypothesis was that the presence of microthreads in the implant cervical region would not result in different reliability and strength to failure than smooth design, regardless of fixation method, when subjected to step-stress accelerated life-testing (SSALT) in water. Materials and methods: Eighty four dental implants (3.3 × 10 mm) were divided into four groups (n = 21) according to implant macrogeometric design at the crestal region and crown fixation method: Microthreads Screwed (MS); Smooth Screwed (SS); Microthreads Cemented (MC), and Smooth Cemented (SC). The abutments were torqued to the implants and standardized maxillary central incisor metallic crowns were cemented (MC, SC) or screwed (MS, SS) and subjected to SSALT in water. The probability of failure versus cycles (90% two-sided confidence intervals) was calculated and plotted using a power law relationship for damage accumulation. Reliability for a mission of 50,000 cycles at 150 N (90% 2-sided confidence intervals) was calculated. Differences between final failure loads during fatigue for each group were assessed by Kruskal-Wallis along with Benferroni's post hoc tests. Polarized-light and scanning electron microscopes were used for failure analyses. Results: The Beta (β) value (confidence interval range) derived from use level probability Weibull calculation of 1.30 (0.76-2.22), 1.17 (0.70-1.96), 1.12 (0.71-1.76), and 0.52 (0.30-0.89) for groups MC, SC, MS, and SS respectively, indicated that fatigue was an accelerating factor for all groups, except for SS. The calculated reliability was higher for SC (99%) compared to MC (87%). No difference was observed between screwed restorations (MS - 29%, SS - 43%). Failure involved abutment screw fracture for all groups. The cemented groups (MC, SC) presented more abutment and implant fractures. Significantly higher load to fracture values were observed for SC and MC relative to MS and SS (P < 0.001). Conclusion: Since reliability and strength to failure was higher for SC than for MC, our postulated null hypothesis was rejected. © 2012 John Wiley & Sons A/S.

Reliability and failure modes of internal conical dental implant connections

Objective: Biological and mechanical implant-abutment connection complications and failures are still present in clinical practice, frequently compromising oral function. The purpose of this study was to evaluate the reliability and failure modes of anterior single-unit restorations in internal conical interface (ICI) implants using step-stress accelerated life testing (SSALT). Materials and methods: Forty-two ICI implants were distributed in two groups (n = 21 each): group AT-OsseoSpeed™ TX (Astra Tech, Waltham, MA, USA); group SV-Duocon System Line, Morse Taper (Signo Vinces Ltda., Campo Largo, PR, Brazil). The corresponding abutments were screwed to the implants and standardized maxillary central incisor metal crowns were cemented and subjected to SSALT in water. Use-level probability Weibull curves and reliability for a mission of 50,000 cycles at 200 N were calculated. Differences between groups were assessed by Kruskal-Wallis along with Bonferroni's post-hoc tests. Polarized-light and scanning electron microscopes were used for failure analyses. Results: The Beta (β) value derived from use level probability Weibull calculation was 1.62 (1.01-2.58) for group AT and 2.56 (1.76-3.74) for group SV, indicating that fatigue was an accelerating factor for failure of both groups. The reliability for group AT was 0.95 and for group SV was 0.88. Kruskal-Wallis along with Bonferroni's post-hoc tests showed no significant difference between the groups tested (P > 0.27). In all specimens of both groups, the chief failure mode was abutment fracture at the conical joint region and screw fracture at neck's region. Conclusions: Reliability was not different between investigated ICI connections supporting maxillary incisor crowns. Failure modes were similar. © 2012 John Wiley & Sons A/S.

Influence of the network modifier on the characteristics of MSnO 3 (M=Sr and Ca) thin films synthesized by chemical solution deposition

CaSnO3 and SrSnO3 alkaline earth stannate thin films were prepared by chemical solution deposition using the polymeric precursor method on various single crystal substrates (R- and C-sapphire and 100-SrTiO3) at different temperatures. The films were characterized by X-ray diffraction (θ-2θ, ω- and φ-scans), field emission scanning electron microscopy, atomic force microscopy, micro-Raman spectroscopy and photoluminescence. Epitaxial SrSnO3 and CaSnO 3 thin films were obtained on SrTiO3 with a high crystalline quality. The long-range symmetry promoted a short-range disorder which led to photoluminescence in the epitaxial films. In contrast, the films deposited on sapphire exhibited a random polycrystalline growth with no meaningful emission regardless of the substrate orientation. The network modifier (Ca or Sr) and the substrate (sapphire or SrTiO3) influenced the crystallization process and/or the microstructure. Higher is the tilts of the SnO6 octahedra, as in CaSnO3, higher is the crystallization temperature, which changed also the nucleation/grain growth process. © 2012 Elsevier Inc. All rights reserved.

Growth of TiO2 nanotubes by anodization of Ti-7.5Mo in NH 4F solutions

Titanium and its alloys are widely used as biomaterials due to their mechanical, chemical and biological properties. To enhance the biocompatibility of titanium alloys, various surface treatments have been proposed. In particular, the formation of titanium oxide nanotubes layers has been extensively examined. According to the literature, it is possible to induce the growth of TiO2 on the surface of titanium, employing the aqueous anodizing electrolyte. This Ti-7.5Mo alloy was anodized in glycerol electrolytes containg 0.25 wt% of NH4F, with variations in time, voltage and calcinations temperature. After anodization, the sample surfaces were analyzed with a field emission scanning electron microscopy, DRX and contact angle measurements. It was possible to observe the formation of TiO2 on the surface and these findings represent a simple surface treatment for Ti alloys that has high potential for biomedical applications. Copyright © 2013 American Scientific Publishers. All rights reserved.

Synthesis of wurtzite ZnS nanoparticles using the microwave assisted solvothermal method

In this article, we report the development of an efficient and rapid microwave assisted solvothermal (MAS) method to prepare wurtzite ZnS nanoparticles at 413 K using different precursors. The materials obtained were analyzed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (MET) ultraviolet-visible (UV-vis) and photoluminescence (PL) measurements. The structure, surface chemical composition and optical properties were investigated as a function of the precursor. In addition, effects as well as merits of microwave heating on the processing and characteristics of ZnS nanoparticles obtained are reported. The possible formation mechanism and optical properties of these nanoparticles were also reported. © 2012 Elsevier B.V. All rights reserved.

A brief discussion about image quality and SEM methods for quantitative fractography of polymer composites

The methodology for fracture analysis of polymeric composites with scanning electron microscopes (SEM) is still under discussion. Many authors prefer to use sputter coating with a conductive material instead of applying low-voltage (LV) or variable-pressure (VP) methods, which preserves the original surfaces. The present work examines the effects of sputter coating with 25 nm of gold on the topography of carbon-epoxy composites fracture surfaces, using an atomic force microscope. Also, the influence of SEM imaging parameters on fractal measurements is evaluated for the VP-SEM and LV-SEM methods. It was observed that topographic measurements were not significantly affected by the gold coating at tested scale. Moreover, changes on SEM setup leads to nonlinear outcome on texture parameters, such as fractal dimension and entropy values. For VP-SEM or LV-SEM, fractal dimension and entropy values did not present any evident relation with image quality parameters, but the resolution must be optimized with imaging setup, accompanied by charge neutralization. © Wiley Periodicals, Inc.

Spin-resolved local density of states for an Anderson adatom in a ferromagnetic island

In this work, we investigate theoretically the spin-resolved local density of states (SR-LDOS) of a ferromagnetic (FM) island hybridized with an adatom, which is described by the Single Impurity Anderson Model (SIAM). Our results are comparable with Scanning Tunneling Microscope (STM) experimental data. © 2012 Springer Science+Business Media, LLC.