905 resultados para Nano-Indentation


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

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Nano- (30-60 nm) and submicron (100-350 nm) ZnO particles were synthesized using solvothermal method at 200 degrees C from an ethanolic solution of zinc acetate dihydrate, applying different reaction conditions, i.e., pH value of precursor and time of the reaction. The X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), UV-vis diffuse reflectance (DR), Raman spectroscopy, and photoluminescence (PL) spectroscopy have been employed for characterization of synthesized ZnO powders. It was shown that the structural, morphological, and optical properties are largely determined by reaction conditions during solvothermal synthesis. The particle crystallinity improves with the decrease of pH value and/or the increase of time of the reaction. The Raman and PL spectra analyses indicate that the oxygen interstitials are dominant intrinsic defects in solvothermally synthesized ZnO powders. It was observed that concentration of defects in wurtzite ZnO crystal lattices slightly changes with the variation of pH value of the precursor and time of the solvothermal reaction. The correlation between structural ordering and defect structure of particles and corresponding growth processes was discussed.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Curcumin possesses wide-ranging anti-inflammatory and anti-cancer properties and its biological activity can be correlated to its potent antioxidant capacity. Novel maghemite (gamma-Fe3O4) nanoparticles, characterized by a diameter of about 10 nm and possessing peculiar colloidal properties and surface interactions, called Surface Active Maghemite Nanoparticles (SAMN), were superficially modified with curcumin by simple incubation, due to the presence of under-coordinated Fe(III) atoms on nanoparticle surface. The resulting curcumin-modified SAMNs (SAMN@curcumin) were characterized by transmission electron microscopy (TEM), FTIR, Mossbauer, EPR and UV-Vis spectroscopy. The redox properties of bound curcumin were tested by electrochemistry. Finally, SAMN@curcumin was studied in the presence of different electroactive substances, namely hydroquinone, NADH and ferrocyanide, in order to assess its electrochemical behavior. Moreover, SAMN@curcumin was electrochemically tested in the presence of one of the most diffuse reactive oxygen specie, such as hydrogen peroxide, demonstrating its stability. SAMN@curcumin in which curcumin is firmly bound, but still retaining its redox features represents a feasible adduct: a magnetically drivable nano-bio-conjugate mimicking free Curcumin redox behavior. The proposed nanostructured material could be exploited as magnetic drivable curcumin vehicle for biomedical applications.

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This in vitro study compared the effect of bleaching agents modified by the addition of calcium and/or fluoride and the application of a nano-hydroxyapatite paste after bleaching, on the susceptibility of enamel to erosion. Bovine enamel cylindrical samples (3 mm diameter) were assigned to six groups (n = 20 specimens/group) according to the bleaching agent: no bleaching (C-control), 7.5% hydrogen peroxide gel (HP), HP with 0.5% calcium gluconate (HP+Ca), HP with 0.2% sodium fluoride (HP+F), HP with calcium and fluoride (HP+Ca+F) and HP followed by the application of a nano-hydroxyapatite agent (HP+NanoP). The gels were applied on the enamel surface (1 h) followed by cyclic erosive challenges (Sprite Zero®-2 min), for 14 days. The paste was applied after bleaching for 5 min (HP+NanoP). The enamel surface alteration was measured by contact profilometry (µm) (after 7 and 14 days). C-control (mean ± SD: 2.29 ± 0.37 at 7 days/4.86 ± 0.72 at 14 days) showed significantly lower loss compared to the experimental groups. HP+Ca (3.34 ± 0.37/6.75 ± 1.09) and HP+F (4.49 ± 0.92/7.61 ± 0.90) presented significantly lower enamel loss than HP (4.18 ± 0.50/10.30 ± 1.58) only for 14 days and HP+Ca+F (4.92 ± 1.03/8.12 ± 1.52) showed values similar to the HP+F group. The HP+NanoP (5.51 ± 1.04/9.61 ± 1.21) resulted in enamel loss similar to the HP after 14 days. It was found that 7.5% hydrogen peroxide increased the susceptibility of enamel to erosion. The addition of calcium or fluoride to the bleaching gel reduced the erosion effect, while the nano-hydroxyapatite agent did not provide any protective effect.

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

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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In the analysis of instrumented indentation data, it is common practice to incorporate the combined moduli of the indenter (E-i) and the specimen (E) in the so-called reduced modulus (E-r) to account for indenter deformation. Although indenter systems with rigid or elastic tips are considered as equivalent if E-r is the same, the validity of this practice has been questioned over the years. The present work uses systematic finite element simulations to examine the role of the elastic deformation of the indenter tip in instrumented indentation measurements and the validity of the concept of the reduced modulus in conical and pyramidal (Berkovich) indentations. It is found that the apical angle increases as a result of the indenter deformation, which influences in the analysis of the results. Based upon the inaccuracies introduced by the reduced modulus approximation in the analysis of the unloading segment of instrumented indentation applied load (P)-penetration depth (delta) curves, a detailed examination is then conducted on the role of indenter deformation upon the dimensionless functions describing the loading stages of such curves. Consequences of the present results in the extraction of the uniaxial stress-strain characteristics of the indented material through such dimensional analyses are finally illustrated. It is found that large overestimations in the assessment of the strain hardening behavior result by neglecting tip compliance. Guidelines are given in the paper to reduce such overestimations.

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In this work, different methods to estimate the value of thin film residual stresses using instrumented indentation data were analyzed. This study considered procedures proposed in the literature, as well as a modification on one of these methods and a new approach based on the effect of residual stress on the value of hardness calculated via the Oliver and Pharr method. The analysis of these methods was centered on an axisymmetric two-dimensional finite element model, which was developed to simulate instrumented indentation testing of thin ceramic films deposited onto hard steel substrates. Simulations were conducted varying the level of film residual stress, film strain hardening exponent, film yield strength, and film Poisson's ratio. Different ratios of maximum penetration depth h(max) over film thickness t were also considered, including h/t = 0.04, for which the contribution of the substrate in the mechanical response of the system is not significant. Residual stresses were then calculated following the procedures mentioned above and compared with the values used as input in the numerical simulations. In general, results indicate the difference that each method provides with respect to the input values depends on the conditions studied. The method by Suresh and Giannakopoulos consistently overestimated the values when stresses were compressive. The method provided by Wang et al. has shown less dependence on h/t than the others.

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Nano-biocomposites based on a biodegradable bacterial copolyester, poly(hydroxybutyrate-co-hydroxyvalerate), have been elaborated with an organo-modified montmorillonite (OMMT) clay as nanofiller, and acetyl tributyl citrate as plasticizer. The corresponding (nano)structures, thermal and mechanical properties, permeability, and biodegradability have been determined. Polyhydroxyalkanoates are very thermal sensitive then to follow the degradation the corresponding matrices have been analyzed by size exclusion chromatography. The results indicate that the addition of the plasticizer decreases the thermo-mechanical degradation, during the extrusion. These nano-biocomposites show an intercalated/exfoliated structure with good mechanical and barrier properties, and an appropriated biodegradation kinetic. Intending to understand the changes in the thermal properties, the nano-biocomposites were characterized by thermal gravimetric analysis and differential scanning calorimetry. The presence of the OMMT clay did not influence significantly the transition temperatures. However, the filler not only acted as a nucleating agent which enhanced the crystallization, but also as a thermal barrier, improving the thermal stability of the biopolymer. The results indicated that the addition of the plasticizer reduces the glass transition temperature and the crystalline melting temperature. The plasticizer acts as a processing aid and increases the processing temperature range (lower melting temperature).

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This in vitro study evaluated the preventive potential of experimental pastes containing 10% and 20% hydroxyapatite nanoparticles (Nano-HAP), with or without fluoride, on dental demineralization. Bovine enamel (n=15) and root dentin (n=15) specimens were divided into 9 groups according to their surface hardness: control (without treatment), 20 Nanop paste (20% HAP), 20 Nanop paste plus (20% HAP + 0.2% NaF), 10 Nanop paste (10% HAP), 10 Nanop paste plus (10% HAP + 0.2% NaF), placebo paste (without fluoride and HAP), fluoride paste (0.2% NaF), MI paste (CPP-ACP, casein phosphopeptide-amorphous calcium phosphate), and MI paste plus (CPP-ACP + 0.2% NaF). Both MI pastes were included as commercial control products containing calcium phosphate. The specimens were treated with the pastes twice a day (1 min), before and after demineralization. The specimens were subjected to a pH-cycling model (demineralization–6-8 h/ remineralization-16-18 h a day) for 7 days. The dental subsurface demineralization was analyzed using cross-sectional hardness (kgf/mm 2 , depth 10-220 µm). Data were tested using repeated-measures two-way ANOVA and Bonferroni's test (p<0.05). The only treatment able to reduce the loss of enamel and dentin subsurface hardness was fluoride paste (0.2% NaF), which differed significantly from the control at 30- and 50-µm depth (p<0.0001). The other treatments were not different from each other or compared with the control. The experimental Nanop pastes, regardless of the addition of fluoride, were unable to reduce dental demineralization in vitro.

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Abstract Im Rahmen dieser Arbeit wurden verschiedene neue Synthesewege zur Darstellung poröser Kieselgele untersucht. Als porenbildende Template wurden hierzu eine Reihe niedermolekularer und polymerer Verbindungen eingesetzt. Dabei sollten die Teilchenmorphologie und die Parameter der Porenstruktur durch die Bedingungen bei der Reaktion und nicht durch eine Nachbehandlung eingestellt werden. Hauptziel der Arbeit war es, eine Synthese zu entwickeln, bei der durch den Einsatz eines geeigneten Templats sphärische Kieselgelpartikel mit Porengrößen über 10 nm hergestellt werden können. Zusätzlich zur Materialsynthese gelang es Informationen über den Bildungsmechanismus poröser Kieselgele zu erhalten.Weiterhin wurden die Materialien als Säulenmaterial in der Chromatographie, als Adsorbens zur Probensammlung (sample tracking), als Katalysatorträgermaterial und als Marker für Biomoleküle eingesetzt.