Application of impedance spectroscopy to evaluate the effect of different setting accelerators on the developed microstructures of calcium phosphate cements

The main goal of the present study was to evaluate the effect of different setting accelerator agents on the developed microstructures of calcium phosphate cements (CPCs) by employing the impedance spectroscopy (IS) technique. Six compositions of CPCs were prepared from mixtures of commercial dicalcium phosphate anhydrous (DCPA) and synthesized tetracalcium phosphate (TTCP) as the solid phases. Two TTCP/DCPA molar ratios (1/1 and 1/2) and three liquid phases (aqueous solutions of Na(2)HPO(4), tartaric acid (TA) and oxalic acid (OA), 5% volume fraction) were employed. Initial (I) and final (F) setting times of the cement pastes were determined with Gillmore needles (ASTM standard C266-99). The hardened samples were characterized by X-ray powder diffraction (XRD), Fourier transformed infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and apparent density measurements. The IS technique was employed as a non-destructive tool to obtain information related to porosity, tortuosity and homogeneity of the cement microstructures. The formulation prepared from a TTCP/DCPA equimolar mixture and OA as the liquid phase presented the shortest I and F (12 and 20 min, respectively) in comparison to the other studied systems. XRD analyses revealed the formation of low-crystallinity hydroxyapatite (HA) (as the main phase) as well as the presence of little amounts of unreacted DCPA and TTCP after 24 h hardening in 100% relative humidity. This was related to the proposed mechanisms of dissolution of the reactants. The bands observed by FTIR allowed identifying the presence of calcium tartrate and calcium oxalate in the samples prepared from TA and OA, in addition to the characteristic bands of HA. High degree of entanglement of the formed crystals was observed by SEM in samples containing OA. SEM images were also correlated to the apparent densities of the hardened cements. Changes in porosity, tortuosity and microstructural homogeneity were determined in all samples, from IS results, when the TTCP/DCPA ratio was changed from 1/1 to 1/2. The cement formulated from an equimolar mixture of TTCP/DCPA and OA as the liquid phase presented setting times, degree of conversion to low-crystallinity HA and microstructural features suitable to be used as potential bone cement in clinical applications. The IS technique was shown to be a very sensitive and non-destructive tool to relate the paste composition to the developed microstructures. This approach could be very useful to develop calcium phosphate bone cements for specific clinical demands.

An overview of the microstructures present in high-speed steel - Carbides crystallography

The aim of the work was to prepare an overview about the microstructures present in high-speed steel, focused on the crystallography of the carbides. High-speed steels are currently obtained by casting, powder metallurgy and more recently spray forming. High-speed steels have a high hardness resulting from a microstructure, which consists of a steel matrix (martensite and ferrite), in which embedded carbides of different crystal structure, chemical composition, morphology and size, exist. These carbides are commonly named MxC, where M represents one or more metallic atoms. These carbides can be identified by X-ray diffraction considering M as a unique metallic atom. In this work, it is discussed, in basis of the first principles of physics crystallography, the validation of this identification when it is considered that other atoms in the structure are substitutional. Further, it is discussed some requirements for data acquisition that allows the Rietveld refinement to be applied on carbide crystallography and phase amount determination.

Indirect doping of microstructures fabricated by two-photon polymerization with gold nanoparticles

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Macro- and microstructural organization of the rabbit's celiac-mesenteric ganglion complex (Oryctolagus cuniculus)

The macro- and microstructures of the rabbit celiac-mesenteric ganglion complex are described in 20 young animals. We found ten celiac ganglia, twenty-seven cranial mesenteric ganglia and eleven celiac-mesenteric ganglia. The celiac ganglia had a rectangular shape in nine cases (90%) and a circular one in one case (10%). The cranial mesenteric ganglia presented triangular (66.7%), rectangular (11.1%), L-shape (18.5%) and semilunar (3.7%) arrangements. The celiac-mesenteric ganglia were organized in three patterns: a single left celiac-mesenteric ganglion having a caudal portion (72.7%); celiac-mesenteric ganglia without a caudal portion (18.2%) and a single celiac-mesenteric ganglion with two portions: left and right (9.1%).The microstructure was investigated in nine celiac-mesenteric ganglia. The results showed that the celiac-mesenteric ganglion is actually a ganglion complex constituted of an agglomerate of ganglionic units separated by nerve fibers, capillaries and septa of connective tissue. Using the semi-thin section method we described the cellular organization of the celiac-mesenteric ganglion complex. Inside of each ganglionic unit, there were various cell types: principal ganglion neurons (PGN), glial cells (satellite cells) and SIF cells (small intensely fluorescent cells or small granular cells), which are the cytologic basis for each ganglionic unit of the rabbit's celiac-mesenteric ganglion complex.

Análises térmicas e processo de sinterização da cerâmica KSr2Nb5O15 dopada com CuO

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

A metallurgical study of aluminium alloys used as aircraft components

The effects of heat treatment on morphologies and microstructures of Al 2024 and Al 7050 alloys, used as aircraft components, were studied by metallographic techniques. Light microscopy (LM) and quantitative image analysis were used to characterize the precipitate dispersion and morphology for these alloys. The application of the scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) combined techniques for studying these multiphase systems makes it possible to distinguish and quantify the different phases in the surface structure. Xray diffraction also permitted a qualitative comparison of the structures before and after heat treatments.

Preparation of Ni-Ti-Mo and Ni-Ti-Mo-Zr Alloys by High-Energy Ball Milling and Subsequent Hot Pressing

This work discusses on the preparation of Ni-45Ti-5Mo, Ni-40Ti-10Mo and Ni-46Ti-2Mo-2Zr (at-%) alloys by high-energy ball milling and hot pressing, which are potentially attractive for dental and medical applications. The milling process was performed in stainless steel balls (19mm diameter) and vials (225 mL) using a rotary speed of 300rpm and a ball-to-powder weight ratio of 10:1. Hot pressing under vacuum was performed in a BN-coated graphite crucible at 900 degrees C for 1 h using a load of 20 MPa. The milled and hot-pressed materials were characterized by X-ray diffraction, electron scanning microscopy, and electron dispersive spectrometry. Peaks of B2-NiTi and Ni4Ti3 were identified in XRD patterns of Ni-45Ti-5Mo, Ni-40Ti-10Mo and Ni-46Ti-2Mo-2Zr powders milled for 1h. The NiTi compound dissolved small Mo amounts lower than 4 at%, which were measured by EDS analysis. Moreover, it was identified the existence of an unknown Mo-rich phase in microstructures of the hot-pressed Ni-Ti-Mo alloys.

Wear resistance of experimental titanium alloys for dental applications

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

Three-Dimensional Characterization of Pores in Ti-6Al-4V Alloy

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Evaluation of strip rolling directly from the semi-solid state

defect metal alloy strip when thixorolling directly from the semi-solid state. To facilitate the study lead/tin alloys were chosen for their relatively low operating temperature. The objective is to extrapolate these findings to the higher temperature aluminium, alloys. Three alloys (70%Pb30%Sn, 60%Pb-40%Sn, 50%Pb-50%wtSn) were used particularly to study the influence of the solidification interval. The equipment consists of a two roll mill arranged as an upper and lower roller, where both rollers are driven at a controlled speed. The lower roller is fed with semi solid alloy through a ceramic nozzle attached to the lower end of a cooling slope. Several types of nozzle and their position at the roller were tested. This produced different solidifications and consequently different finished strip. The alloys were first cast and then poured onto the cooling slope through a tundish in order to create a continuous laminar flow of slurry and uniformity of metal strip quality. The pouring was tested at different positions along the slope. The cooling slope was coated with colloidal graphite to promote a smooth slurry flow and avoid the problem of adherence and premature solidification. The metallic slurry not only cools along the slope but is also initially super-cooled to a mush by the lower roller whilst at room temperatures, thus enabling thixorolling. It was also found that the nozzle position could be adjusted to enable the upper roller to also contribute to the solidification of the metallic slurry. However the rollers and the cooling slope naturally heat up. Temperature distribution in these zones was analysed by means of three thermocouples positioned along the cooling slope and a fourth in the base of the semi solid pool within the nozzle. The objective being to design an optimum pouring and cooling system. The formed strip was cooled down to room temperature with a shower of water. Microstructures of the thixorolling process were analysed. The differences in solidification conditions resulted in differing qualities of finished strip and corresponding defect types, all of which are a serious quality issue for the rolled product.

Micro Welding of Ni-based Alloy Monel 400 Thin Foil by Pulsed Nd:YAG laser

In this study a pulsed Nd:YAG laser was used to join Monel 400 thin foil with 100 mu m thickness. Pulse energy was varied from 1.0 to 2.25J at small increments of 0.25J. The macro and microstructures were analyzed by optical microscopy, tensile shear test and microhardness. Sound laser welds without discontinuities were obtained with 1.5 J pulse energy. Results indicate that using a precise control of the pulse energy, and so a control of the bottom foil dilution rate, it is possible to weld Monel 400 thin foil. The process appeared to be very sensitive to the gap between couples.

Pulsed Nd:YAG laser welding of Ni-alloy Hastelloy C-276 foils

In this study a pulsed Nd:YAG laser was used to join Hastelloy C-276 thin foil with 100 microns thickness. Pulse energy was varied from 1.0 to 2.25 J at small increments of 0.25 J with a 4 ms pulse duration. The macro and microstructures of the welds were analyzed by optical and electronic microscopy, tensile shear test and microhardness. Sound laser welds without discontinuities were obtained with 1.5 J pulse energy. Results indicate that using a precise control of the pulse energy, and so a control of the dilution rate, it is possible to weld Hastelloy C-276 thin foil by pulsed Nd: YAG laser. (C) 2012 Published by Elsevier B. V. Selection and/or review under responsibility of Bayerisches Laserzentrum GmbH

Study of Densification Process and Microstructure for Highly Dense Doped MgB2 Bulk Samples

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Role of enthalpy and entropy in moisture sorption behavior of pineapple pulp powder produced by different drying methods

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