145 resultados para MICROSTRUCTURE
Resumo:
An exhaustive analysis of the crystallisation behaviour of palm oil was performed using low-resolution magnetic pulsed nuclear resonance, differential scanning calorimetry, polarised light microscopy and X-ray diffraction. The aim of this study was to characterise the changes induced in the crystallisation of palm oil by the addition of two different levels of tripalmitin and two different types of monoacylglycerols. The addition of monoacylglycerols led to the formation of a large number of crystallisation nuclei without changing the final solids content, accelerating the process of crystal formation, leading to the formation of smaller crystals than those found in the refined palm oil. Higher levels of tripalmitin produced crystals with larger dimensions, reducing the induction period and resulted in a higher level of solids at the end of the crystallisation period. The addition of monoacylglycerols and tripalmitin induced the formation of a polymorphic beta-form. (C) 2010 Elsevier Ltd. All rights reserved.
Resumo:
Food foams such as marshmallow, Chantilly and mousses have behavior and stability directly connected with their microstructure, bubble size distribution and interfacial properties. A high interfacial tension inherent to air/liquid foams interfaces affects its stability, and thus it has a direct impact on processing, storage and product handling. In this work, the interactions of egg albumin with various types of polysaccharides were investigated by drop tensiometry, interfacial rheology and foam stability. The progressive addition of egg albumin and polysaccharide in water induced a drop of the air-water surface tension which was dependent on the pH and polysaccharide type. At pH 4, that is below the isoeletric point of egg albumen (pI = 4.5) the surface tension was decreased from 70 mN/m to 42 mN/m by the presence of the protein, and from 70 mN/m to 43 mN/m, 40 mN/m and 38 mN/m by subsequent addition of xanthan, guar gum and kappa-carrageenan, respectively. At pH 7.5 the surface tension was decreased from 70 mN/m to 43 mN/m by the simultaneous presence of the protein and kappa-carrageenan. However, a higher surface tension of 48 and 50 mN/m was found when xanthan and guar gum were added, respectively, when compared with carrageenan addition. The main role on the stabilization of protein-polysaccharide stabilized interfaces was identified on the elasticity of the interface. Foam stability experiments confirmed that egg-albumin/kappa-carrageenan at pH below the protein isoeletric point are the most efficient systems to stabilize air/water interfaces. These results clearly indicate that protein-polysaccharide coacervation at the air/water interface is an efficient process to increase foam stability. (C) 2009 Elsevier Ltd. All rights reserved.
Resumo:
In this work, flatbed scanning, instrumental texture analysis, spectrophotometric color determination (L*, a*, b*), moisture and specific volume measurements were used to evaluate the effects of the addition of rye flour or rye flakes, yeast and boiling water in different amounts in sponge-dough rye bread production. The treatments changed significantly (P < 0.05) the crumb cell area (mm(2)), cell diameter (mm), cell perimeter (mm), texture parameters and light reflectance (L*, a*, b*). Scalding process could be used to produce new textures and color of baked products.
Resumo:
Emulsions surfer alterations in their microstructure after applied on the skin, because of the interaction with skin constituents and mainly by the evaporation of volatile components. These alterations are not even considered by cosmetic formulators, but they are extremely important because they can act on formulation stability, on delivery and on permeation of actives and also on the ability to build the occlusive film, responsible for skin`s moisturization. This research studied the phase changing during evaporation of emulsions made with three different oil phase: mineral oil, avocado oil, and isocethyl/stearoil stearate, as a function of the decrease on water ratio, using phase diagrams and evaporation test. It was observed the formation of liquid crystalline phases and their transition along the evaporation path for emulsions with the three different oil phases. It was also observed that these transitions occurred in different water ratios.
Resumo:
Preparation methods can profoundly affect the structural and electrochemical properties of electrocatalytic coatings. In this investigation, RuO(2)-Ta(2)O(5) thin films containing between 10 and 90 at.% Ru were prepared by the Pechini-Adams method. These coatings were electrochemically and physically characterized by cyclic voltammetry, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The composition and morphology of the oxide were investigated before and after accelerated life tests (ALT) by EDX and SEM. SEM results indicate typical mud-flat-cracking morphology for the majority of the films. High resolution SEMs reveal that pure oxide phases exhibit nanoporosity while binary compositions display a very compact structure. EDX analyses reveal considerable amounts of Ru in the coating even after total deactivation. XRD indicated a rutile-type structure for RuO(2) and orthorhombic structure for Ta(2)O(5). XPS data demonstrate that the binding energy of Ta is affected by Ru addition in the thin films, but the binding energy of Ru is not likewise influenced by Ta. The stability of the electrodes was evaluated by ALT performed at 750 mA cm(-2) in 80 degrees C 0.5 mol dm(-3) H(2)SO(4). The performance of electrodes prepared by the Pechini-Adams method is 100% better than that of electrodes prepared by standard thermal decomposition.
Resumo:
Chronic obstructive pulmonary disease (COPD) is associated with osteoporosis and fragility fractures. The objectives of this study were to assess static and dynamic indices of cancellous and cortical bone structure in postmenopausal women with COPD. Twenty women with COPD who had not received chronic oral glucocorticoids underwent bone biopsies after double tetracycline labeling. Biopsies were analyzed by histomorphometry and mu CT and compared with age-matched controls. Distribution of the patients according to the Global Initiative for Chronic Obstructive Lung Disease (GOLD) was: Type I (15%), Type II (40%), Type III (30%), and Type IV (15%). Mean (+/-SD) cancellous bone volume (15.20 +/- 5.91 versus 21.34 +/- 5.53%, p = .01), trabecular number (1.31 +/- 0.26 versus 1.77 +/- 0.51/mm, p = .003), and trabecular thickness (141 +/- 23 versus 174 +/- 36 mu m, p = .006) were lower in patients than in controls. Connectivity density was lower in COPD (5.56 +/- 2.78 versus 7.94 +/- 3.08 mu m, p = .04), and correlated negatively with smoking (r = -0.67; p = .0005). Trabecular separation (785 +/- 183 versus 614 +/- 136 mu m, p = .01) and cortical porosity (4.11 +/- 1.02 versus 2.32 +/- 0.94 voids/mm(2); p < .0001) were higher in COPD while cortical width (458 +/- 214 versus 762 +/- 240 mu m; p < .0001) was lower. Dynamic parameters showed significantly lower mineral apposition rate in COPD (0.56 +/- 0.16 versus 0.66 +/- 0.12 mu m/day; p = .01). Patients with more severe disease, GOLD III and IV, presented lower bone formation rate than GOLDI and II (0.028 +/- 0.009 versus 0.016 +/- 0.011 mu m(3)/mu m(2)/day;p = 04). This is the first evaluation of bone microstructure and remodeling in COPD. The skeletal abnormalities seen in cancellous and cortical bone provide an explanation for the high prevalence of vertebral fractures in this disease. (C) 2010 American Society for Bone and Mineral Research.
Resumo:
Zirconia (ZrO(2)) is a bioinert, strong, and tough ceramic, while titania (TiO(2)) is bioactive but has poor mechanical properties. It is expected that ZrO(2)-TiO(2) mixed ceramics incorporate the individual properties of both ceramics, so that this material would exhibit better biological properties. Thus, the objective of this study was to compare the biocompatibility properties of ZrO(2)-TiO(2) mixed ceramics. Sintered ceramics pellets, obtained from powders of TiO(2), ZrO(2), and three different ZrO(2)-TiO(2) mixed oxides were used. Roughnesses, X-ray diffraction, microstructure through SEM, hardness, and DRIFT characterizations were performed. For biocompatibility analysis cultured FMM1 fibroblasts were plated on the top of disks and counted in SEM micrographs 1 and 2 days later. Data were compared by ANOVA complemented by Tukey`s test. All samples presented high densities and similar microstructure. The H(2)O content in the mixed ceramics was more evident than in pure ceramics. The number of fibroblasts attached to the disks increased significantly independently of the experimental group. The cell growth on the top of the ZrO(2)-TiO(2) samples was similar and significantly higher than those of TiO(2) and ZrO(2) samples. Our in vitro experiments showed that the ZrO(2)-TiO(2) sintered ceramics are biocompatible allowing faster cell growth than pure oxides ceramics. The improvement of hardness is proportional to the ZrO(2) content. Thus, the ZrO(2)-TiO(2) sintered ceramics could be considered as potential implant material. (C) 2010 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater 94B: 305-311, 2010.
Resumo:
The resin phase of dental composites is mainly composed of combinations of dimethacrylate comonomers, with final polymeric network structure defined by monomer type/reactivity and degree of conversion. This fundamental study evaluates how increasing concentrations of the flexible triethylene glycol dimethacrylate (TEGDMA) influences void formation in bisphenol A diglycidyl dimethacrylate (BisGMA) co-polymerizations and correlates this aspect of network structure with reaction kinetic parameters and macroscopic volumetric shrinkage. Photopolymerization kinetics was followed in real-time by a near-infrared (NIR) spectroscopic technique, viscosity was assessed with a viscometer, volumetric shrinkage was followed with a linometer, free volume formation was determined by positron annihilation lifetime spectroscopy (PALS) and the sol-gel composition was determined by extraction with dichloromethane followed by (1)H NMR analysis. Results show that, as expected, volumetric shrinkage increases with TEGDMA concentration and monomer conversion. Extraction/(1)H NMR studies show increasing participation of the more flexible TEGDMA towards the limiting stages of conversion/crosslinking development. As the conversion progresses, either based on longer irradiation times or greater TEGDMA concentrations, the network becomes more dense, which is evidenced by the decrease in free volume and weight loss after extraction in these situations. For the same composition (BisGMA/TEGDMA 60-40 mol%) light-cured for increasing periods of time (from 10 to 600 s), free volume decreased and volumetric shrinkage increased, in a linear relationship with conversion. However, the correlation between free volume and macroscopic volumetric shrinkage was shown to be rather complex for variable compositions exposed for the same time (600 s). The addition of TEGDMA decreases free-volume up to 40 mol% (due to increased conversion), but above that concentration, in spite of the increase in conversion/crosslinking, free volume pore size increases due to the high concentration of the more flexible monomer. In those cases, the increase in volumetric shrinkage was due to higher functional group concentration, in spite of the greater free volume. Therefore, through the application of the PALS model, this study elucidates the network formation in dimethacrylates commonly used in dental materials. (C) 2010 Elsevier Ltd. All rights reserved.
Resumo:
Objective. To investigate the processing induced particle alignment on fracture behavior of four multiphase dental ceramics (one porcelain, two glass-ceramics and a glass-infiltrated-alumina composite). Methods. Disks (empty set12mm x 1.1 mm-thick) and bars (3 mm x 4 mm x 20 mm) of each material were processed according to manufacturer instructions, machined and polished. Fracture toughness (K(IC)) was determined by the indentation strength method using 3-point bending and biaxial flexure fixtures for the fracture of bars and disks, respectively. Microstructural and fractographic analyses were performed with scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction. Results. The isotropic microstructure of the porcelain and the leucite-based glass-ceramic resulted in similar fracture toughness values regardless of the specimen geometry. On the other hand, materials containing second-phase particles with high aspect ratio (lithium disilicate glass-ceramic and glass-infiltrated-alumina composite) showed lower fracture toughness for disk specimens compared to bars. For the lithium disilicate glass-ceramic disks, it was demonstrated that the occurrence of particle alignment during the heat-pressing procedure resulted in an unfavorable pattern that created weak microstructural paths during the biaxial test. For the glass-infiltrated-alumina composite, the microstructural analysis showed that the large alumina platelets tended to align their large surfaces perpendicularly to the direction of particle deposition during slip casting of green preforms. Significance. The fracture toughness of dental ceramics with anisotropic microstructure should be determined by means of biaxial testing, since it results in lower values. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Resumo:
The aim of this study was to test the hypothesis that the addition of continuous or milled GdAlO(3)/Al(2)O(3) fibers to a dental porcelain increases its mechanical properties. Porcelain bars without reinforcement (control) were compared to those reinforced with long fibers (30 vol%). Also, disk specimens reinforced with milled fibers were produced by adding 0 (control), 5 or 10 vol% of particles. The reinforcement with continuous fibers resulted in significant increase in the uniaxial flexural strength from 91.5 to 217.4 MPa. The addition of varied amounts of milled fibers to the porcelain did not significantly affect its biaxial flexural strength compared to the control group. SEM analysis showed that the interface between the continuous fiber and the porcelain was free of defects. On the other hand, it was possible to note the presence of cracks surrounding the milled fiber/porcelain interface. In conclusion, the reinforcement of the porcelain with continuous fibers resulted in an efficient mechanism to increase its mechanical properties; however the addition of milled fibers had no significant effect on the material because the porcelain was not able to wet the ceramic particles during the firing cycle. (C) 2008 Elsevier Ltd. All rights reserved.
Resumo:
The objective was to compare fracture toughness (K(Ic)), stress corrosion susceptibility coefficient (n), and stress intensity factor threshold for crack propagation (K(I0)) of two porcelains [VM7/Vita (V) and d.Sign/Ivoclar (D)], two glass-ceramics [Empress/Ivolcar (E1) and Empress2/Ivlocar (E2)] and a glass-infiltrated alumina composite [In-Ceram Alumina/Vita (IC)]. Disks were constructed according to each manufacturer`s processing method, and polished before induction of cracks by a Vickers indenter. Crack lengths were measured under optical microscopy at times between 0.1 and 100 h. Specimens were stored in artificial saliva at 37A degrees C during the whole experiment. K(Ic) and n were determined using indentation fracture method. K(I0) was determined by plotting log crack velocity versus log K(I). Microstructure characterization was carried out under SEM, EDS, X-ray diffraction and X-ray fluorescence. IC and E2 presented higher K(Ic) and K(I0) compared to E1, V, and D. IC presented the highest n value, followed by E2, D, E1, and V in a decreasing order. V and D presented similar K(Ic), but porcelain V showed higher K(I0) and lower n compared to D. Microstructure features (volume fraction, size, aspect ratio of crystalline phases and chemical composition of glassy matrix) determined K(Ic). The increase of K(Ic) value favored the increases of n and K(I0).
Resumo:
Objectives. To determine the stress corrosion susceptibility coefficient, n, of seven dental porcelains (A: Ceramco I; B: Ceramco-II; C: Ceramco-III; D: d.Sign; E: Cerabien; F: Vitadur-Alpha; and G: Ultropaline) after aging in air or artificial saliva, and correlate results with leucite content (LC). Methods. Bars were fired according to manufacturers` instructions and polished before induction of cracks by a Vickers indenter (19.6 N, 20 s). Four specimens were stored in air/room temperature, and three in saliva/37 degrees C. Five indentations were made per specimen and crack lengths measured at the following times: similar to 0; 1; 3; 10; 30; 100; 300; 1000 and 3000 h. The stress corrosion coefficient n was calculated by linear regression analysis after plotting crack length as a function of time, considering that the slope of the curve was (2/(3n + 2)]. Microstructural analysis was performed to determine LC. Results. LC of the porcelains were 22% (A and B); 6% (C); 15% (D); 0% (E and F); and 13% (G). Except for porcelains A and D, all materials showed a decrease in their n values when stored in artificial saliva. However, the decrease was more pronounced for porcelains B, F, and G. Ranking of materials varied according to storage media (in air, porcelain G showed higher n compared to A, while in saliva both showed similar coefficients). No correlation was found between n values and LC in air or saliva. Significance. Storage media influenced the n value obtained for most of the materials. LC did not affect resistance to slow crack growth regardless of the test environment. (c) 2008 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Resumo:
Objectives. To evaluate the effect of pH of storage medium on slow crack growth (SCG) parameters of dental porcelains. Methods. Two porcelains were selected: with (UD) and without (VM7) leucite particles, in order to assess if the microstructure would affect the response of the material to the pH variation. Disc specimens were produced following manufacturers` instructions. Specimens were stored in artificial saliva in pHs 3.5, 7.0 or 10.0 for 10 days and after that the fatigue parameters (n: SCG susceptibility coefficient and sigma(0): scaling parameter) were obtained by the dynamic fatigue test using the same pH of storage. Microstructural analysis of the materials was also performed. Results. For VM7, the values of n obtained in the different pHs were similar and varied from 29.9 to 31.2. The sigma(0) value obtained in pH 7.0 for VM7 was higher than that obtained in the other pHs, which were similar. For porcelain UD, n values obtained in pHs 7.0 and 10.0 were similar (40.8 and 39.6, respectively), and higher than that obtained in pH 3.5 (26.5). With respect to sigma(0), the value obtained for porcelain UD in pH 10.0 was lower than those obtained in pHs 3.5 and 7.0, which were similar. Significance. The effect of pH on the stress corrosion susceptibility (n) depended on the porcelain studied. While the n value of VM7 was not affected by the pH, UD presented lower n value in acid pH. For both porcelains, storage in acid or basic pH resulted in strength degradation. (C) 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Resumo:
Objectives. The purpose of this study was to investigate the effect of light-curing protocol on degree of conversion (DC), volume contraction (C), elastic modulus (E), and glass transition temperature (T(g)) as measured on a model polymer. It was a further aim to correlate the measured values with each other. Methods. Different light-curing protocols were used in order to investigate the influence of energy density (ED), power density (PD), and mode of cure on the properties. The modes of cure were continuous, pulse-delay, and stepped irradiation. DC was measured by Raman micro-spectroscopy. C was determined by pycnometry and a density column. E was measured by a dynamic mechanical analyzer (DMA), and T(g) was measured by differential scanning calorimetry (DSC). Data were submitted to two-and three-way ANOVA, and linear regression analyses. Results. ED, PD, and mode of cure influenced DC, C, E, and T(g) of the polymer. A significant positive correlation was found between ED and DC (r = 0.58), ED and E (r = 0.51), and ED and T(g) (r = 0.44). Taken together, ED and PD were significantly related to DC and E. The regression coefficient was positive for ED and negative for PD. Significant positive correlations were detected between DC and C (r = 0.54), DC and E (r = 0.61), and DC and T(g) (r = 0.53). Comparisons between continuous and pulse-delay modes of cure showed significant influence of mode of cure: pulse-delay curing resulted in decreased DC, decreased C, and decreased T(g). Influence of mode of cure, when comparing continuous and step modes of cure, was more ambiguous. A complex relationship exists between curing protocol, microstructure of the resin and the investigated properties. The overall performance of a composite is thus indirectly affected by the curing protocol adopted, and the desired reduction of C may be in fact a consequence of the decrease in DC. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Resumo:
Diabetes mellitus is the most common endocrine disturbance of domestic carnivores and can cause autonomic neurological disorders, although these are still poorly understood in veterinary medicine. There is little information available on the quantitative adaptation mechanisms of the sympathetic ganglia during diabetes mellitus in domestic mammals. By combining morphometric methods and NADPH-diaphorase staining (as a possible marker for nitric oxide producing neurons), type I diabetes mellitus-related morphoquantitative changes were investigated in the celiac ganglion neurons in dogs. Twelve left celiac ganglia from adult female German shepherd dogs were examined: six ganglia were from non-diabetic and six from diabetic subjects. Consistent hypertrophy of the ganglia was noted in diabetic animals with increase of 55% in length, 53% in width, and 61.5% in thickness. The ordinary microstructure of the ganglia was modified leading to an uneven distribution of the ganglionic units and a more evident distribution of axon fascicles. In contrast to non-diabetic dogs, there was a lack of NADPH-diaphorase perikarial labelling in the celiac ganglion neurons of diabetic animals. The morphometric study showed that both the neuronal and nuclear sizes were significantly larger in diabetic dogs (1.3 and 1.39 times, respectively). The profile density and area fraction of NADPH-diaphorase-reactive celiac ganglion neurons were significantly larger (1.35 and 1.48 times, respectively) in non-diabetic dogs compared to NADPH-diaphorase-non-reactive celiac ganglion neurons in diabetic dogs. Although this study suggests that diabetic neuropathy is associated with neuronal hypertrophy, controversy remains over the possibility of ongoing neuronal loss and the functional interrelationship between them. It is unclear whether neuronal hypertrophy could be a compensation mechanism for a putative neuronal loss during the diabetes mellitus. (C) 2007 Elsevier Ltd. All rights reserved.