Síntese de pigmentos cerâmicos inorgânicos nanométricos e encapsulados com estrutura core-shell pela rota dos precursores poliméricos

The present work has as objective the development of ceramic pigments based in iron oxides and cobalt through the polymeric precursor method, as well as study their characteristics and properties using methods of physical, chemical, morphological and optical characterizations.In this work was used iron nitrate, and cobalt citrate as precursor and nanometer silica as a matrix. The synthesis was based on dissolving the citric acid as complexing agent, addition of metal oxides, such as chromophores ions and polymerization with ethylene glycol. The powder obtained has undergone pre-ignition, breakdown and thermal treatments at different calcination temperatures (700 °C, 800 °C, 900 °C, 1000 °C and 1100 °C). Thermogravimetric analyzes were performed (BT) and Differential Thermal Analysis (DTA), in order to evaluate the term decomposition of samples, beyond characterization by techniques such as BET, which classified as microporous materials samples calcined at 700 ° C, 800 º C and 900 º C and non-porous when annealed at 1000 ° C and 1100 º C, X-ray diffraction (XRD), which identified the formation of two crystalline phases, the Cobalt Ferrite (CoFe2O4) and Cristobalite (SiO2), Scanning Electron Microscopy (SEM) revealed the formation of agglomerates of particles slightly rounded;and Analysis of Colorimetry, temperature of 700 °C, 800 °C and 900 °C showed a brown color and 1000 °C and 1100 °C violet

Comportamento magnético de compósitos de matriz polimérica com adição de ferritas

Polymer matrix composites offer advantages for many applications due their combination of properties, which includes low density, high specific strength and modulus of elasticity and corrosion resistance. However, the application of non-destructive techniques using magnetic sensors for the evaluation these materials is not possible since the materials are non-magnetizable. Ferrites are materials with excellent magnetic properties, chemical stability and corrosion resistance. Due to these properties, these materials are promising for the development of polymer composites with magnetic properties. In this work, glass fiber / epoxy circular plates were produced with 10 wt% of cobalt or barium ferrite particles. The cobalt ferrite was synthesized by the Pechini method. The commercial barium ferrite was subjected to a milling process to study the effect of particle size on the magnetic properties of the material. The characterization of the ferrites was carried out by x-ray diffraction (XRD), field emission gun scanning electron microscopy (FEG-SEM) and vibrating sample magnetometry (VSM). Circular notches of 1, 5 and 10 mm diameter were introduced in the composite plates using a drill bit for the non-destructive evaluation by the technique of magnetic flux leakage (MFL). The results indicated that the magnetic signals measured in plates with barium ferrite without milling and cobalt ferrite showed good correlation with the presence of notches. The milling process for 12 h and 20 h did not contribute to improve the identification of smaller size notches (1 mm). However, the smaller particle size produced smoother magnetic curves, with fewer discontinuities and improved signal-to-noise ratio. In summary, the results suggest that the proposed approach has great potential for the detection of damage in polymer composites structures

Síntese de pigmento cerâmico ferrita de cobalto utilizando planejamento experimental

Synthetic inorganic pigments are the most widely used in ceramic applications because they have excellent chemical and thermal stability and also, in general, a lower toxicity to man and to the environment. In the present work, the ceramic black pigment CoFe2O4 was synthesized by the polymerization Complex method (MPC) in order to form a material with good chemical homogeneity. Aiming to optimize the process of getting the pigment through the MPC was used a fractional factorial design 2(5-2), with resolution III. The factors studied in mathematical models were: citric acid concentration, the pyrolysis time, temperature, time and rate of calcination. The response surfaces using the software statistica 7.0. The powders were characterized by thermal analysis (TG/DSC), x-ray diffraction (XRD), scanning electron microscopy (SEM) and spectroscopy in the UV-visible. Based on the results, there was the formation of phase cobalt ferrite (CoFe2O4) with spinel structure. The color of the pigments obtained showed dark shades, from black to gray. The model chosen was appropriate since proved to be adjusted and predictive. Planning also showed that all factors were significant, with a confidence level of 95%

Síntese e caracterização de ferrita ni-zn pelo método dos precursores poliméricos calcinada por energia de microondas

Magnetic ceramics have been widely investigated, especially with respect to intrinsic and extrinsic characteristics of these materials. Among the magnetic ceramic materials of technological interest, there are the ferrites. On the other hand, the thermal treatment of ceramic materials by microwave energy has offered various advantages such as: optimization of production processes, high heat control, low consumption of time and energy among others. In this work were synthesized powders of Ni-Zn ferrite with compositions Ni1- xZnxFe2O4 (0.25 ≤ x ≤ 0.75 mols) by the polymeric precursor route in two heat treatment conditions, conventional oven and microwave energy at 500, 650, 800 and 950°C and its structural, and morphological imaging. The materials were characterized by thermal analysis (TG/ DSC), X-ray diffraction (XRD), absorption spectroscopy in the infrared (FTIR), scanning electron microscopy (SEM), X-ray spectroscopy and energy dispersive (EDS) and vibrating sample magnetometry (VSM). The results of X-ray diffraction confirmed the formation of ferrite with spinel-type cubic structure. The extrinsic characteristics of the powders obtained by microwave calcination and influence significantly the magnetic behavior of ferrites, showing particles ferrimagnéticas characterized as soft magnetic materials (soft), is of great technological interest. The results obtained led the potential application of microwave energy for calcining powders of Ni-Zn ferrite

Estudo da síntese e propriedade magnética de ferritas de manganês/cobalto dopadas com níquel

For the chemical method of synthesis of co-precipitation were produced ferrite powders manganese-cobalt equal stoichiometric formula Mn (1-x) Co (x) Fe2O4, for 0 < x < 1, first reagent element using as the hydroxide ammonium and second time using sodium hydroxide. The obtained powders were calcined at 400 ° C, 650 ° C, 900 ° C and 1150 ° C in a conventional oven type furnace with an air atmosphere for a period of 240 minutes. Other samples were calcined at a temperature of 900 ° C in a controlled atmosphere of argon, to evaluate the possible influence of the atmosphere on the final results the structure and morphology. The samples were also calcined in a microwave oven at 400 ° C and 650 ° C for a period of 45 minutes possible to evaluate the performance of this type of heat treatment furnace. It was successfully tested the ability of this group include isomorphic ferrite with the inclusion of nickel cations in order to evaluate the occurrence of disorder in the crystalline structures and their changes in magnetic characteristics.To identify the structural, morphological, chemical composition and proportions, as well as their magnetic characteristics were performed characterization tests of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDX), thermogravimetric (TG), vibrating sample magnetometry (MAV) and Mössbauer spectroscopy. These tests revealed the occurrence of distortion in the crystal lattice, changes in magnetic response, occurrence of nanosized particles and superparamagnetism

Multifuncionalização de nanopartículas de CoFe2O4 pela incorporação da prata na sua superfície : síntese e caracterização

Tese (doutorado)—Universidade de Brasília, Instituto de Física, 2015.

Recrystallization kinetic study of copper-bearing strip cast steels

The effects of copper on as-cast structure, recrystallization and precipitation kinetics of strip cast low carbon steel were investigated. As-cast microstructure mainly consists of polygonal ferrite and Widmanstatten ferrite. Recrystallization responses were strongly dependent on initial microstructure and Cu content. Precipitation strengthening was observed in high copper content alloys.

Effects of microstructure on the variation of the unloading behavior of DP780 steels

The nonlinear unloading behavior of three different commercial dual-phase steels (DP780 grade equivalent) was examined. These steels exhibited small variations in chemical composition (0.07 to 0.10 mass percent carbon) and martensite volume fraction (0.23 to 0.28), and they demonstrated similar hardening behavior. Uniaxial loading-unloading-loading tests were conducted at room temperature and quasi-static strain rates between engineering strains of 0.5 and 8%. Steel microstructures were examined using electron backscatter diffraction and nanoindentation techniques. The microplastic component of the unloading strain exhibited no dependence on the martensite volume fraction or the ferrite grain size within the small range encountered in this investigations. Instead, the magnitude of the microplastic component of the unloading strain increased as the strength ratio between the martensite and ferrite phases increased. Correspondingly, the apparent unloading modulus, or chord modulus, exhibited a greater reduction for equivalent increments of strain hardening as the strength ratio increased. These results suggest that springback can be reduced in structures containing two ductile phases if the strength ratio between the harder and softer phases is reduced.

Microstructure and hardness evolution during simulated coiling of a direct strip cast low carbon low niobium steel

This paper examines the impact of coiling temperature and duration on the phase transformation and precipitation behavior of a low carbon and low niobium direct strip cast steel. Coiling was performed at three carefully chosen temperatures: (1) in the ferrite (600°C), (2) during the austenite decomposition (700°C) and (3) in the austenite (850°C). The coiling conditions were found to strongly affect the final microstructure and hardness response, thus highlighting the necessity to judiciously design the coiling treatment. Optical microscopy, and scanning and transmission electron microscopy were used to characterize the microstructural constituents (polygonal ferrite, bainite and pearlite) and the NbC precipitates. Vickers macrohardness measurements are utilized to quantify the mechanical properties. The differences in hardening kinetics for the three different temperatures are shown to come from a complex combination of strengthening contributions.

Investigation on decomposition behavior of austenite under continuous cooling in vanadium microalloyed steel (30MSV6)

In the present study, investigations are focused on microstructural evolution and the resulting hardness during continuous cooling transformation (CCT) in a commercial vanadium microalloyed steel (30MSV6). Furthermore, the effects of cooling rate and austenite grain size (AGS) on CCT behavior of the steel have been studied by employing high-resolution dilatometry. Quantitative metallography accompanied with scanning electron microscopy (SEM) has efficiently confirmed the dilatometric measurements of transformation kinetics and austenite decomposition products. A semi-empirical model has been proposed for prediction of microstructural development during austenite decomposition of the steel and the resultant hardness. The model consists of 8 sub-models including ferrite transformation start temperature, ferrite growth, pearlite start temperature, pearlite growth, bainite start temperature, bainite growth, martensite start temperature and hardness. The transformed fractions of ferrite, pearlite and bainite have been described using semi-empirical Johnson-Mehl-Avrami-Kolmogorov (JMAK) approach in combination with Scheil's equation of additivity. The JMAK rate parameter for bainite has been formulated using a diffusion-controlled model. Predictions of the proposed model were found to be in close agreement with the experimental measurements.

Dependence of deformation behavior on grain size and strain rate in an ultrahigh strength-ductile Mn-based TRIP alloy

A novel ultra-high strength TRIP (transformation induced plasticity) steel, with ~1.5. GPa strength and good ductility of ~26% has been produced. The microstructure consists of ultrafine ferrite, and a large volume fraction of austenite. The flow stress was significantly increased by a reduction in the grain size, but the effect of strain rate on the flow stress was negligible. The formation of stress induced martensite was found to increase linearly with strain, and a reduction in the grain size correlated with an increase in the stress required to form the martensite.

The microstructure evolution and softening processes during high-temperature deformation of a 21Cr-10Ni-3Mo duplex stainless steel

The austenite and ferrite microstructure evolution and softening mechanisms have been investigated in a 21Cr-10Ni-3Mo duplex stainless steel, containing about 60% austenite, deformed in torsion at 1200°C using a strain rate of 0.7 s-1. The above experimental conditions led to the formation of a small volume fraction of new austenite grains through discontinuous dynamic recrystallization (DDRX), which could not account for the observed large softening on the flow curve. DDRX grains mainly formed through the strain-induced migration of the pre-existing austenite grain boundaries, known to dominate in single-phase austenite, complemented by subgrain growth in the interface regions with ferrite. A significant portion of austenite dynamic softening has been attributed to the large-scale subgrain coalescence, the extent of which increased with strain, which seems to have contributed substantially to the observed flow stress decrease. The above process thus appears to represent an alternative mode of austenite dynamic softening to the classical DDRX in the duplex austenite/ferrite microstructure, characterised by limited availability of the pre-existing austenite/austenite high-angle boundaries, deformed at a high temperature. The softening mechanism within ferrite has been classified as "continuous DRX", characterised by a gradual increase in misorientations between neighbouring subgrains with strain and resulting in the progressive conversion of subgrains into "crystallites" bounded partly by low-angle and partly by large-angle boundaries.

The role of thermomechanical routes on the distribution of grain boundary and interface plane orientations in transformed microstructures

In the current study, a series of thermomechanical routes were used to produce different microstructures (i.e., ferrite and martensite) in low-carbon low alloy steels. The five-parameter grain boundary character distribution was measured for all microstructures. The thermomechanical processing route altered the texture of the fully ferritic microstructure and significantly influenced the anisotropy of the grain boundary character distribution. Generally, the population of (111) planes increased with an increase in the γ-fiber texture for the ferritic microstructure, but it did not change the shape of the grain boundary plane distribution at specific misorientations. The most commonly observed boundaries in the fully ferritic structures produced through different routes were {112} symmetric tilt boundaries with the Σ3 = 60 deg/[111] misorientation; this boundary also had a low energy. However, the grain boundary plane distribution was significantly changed by the phase transformation path (i.e., ferrite vs martensite) for a given misorientation. In the martensitic steel, the most populous Σ3 boundary was the {110} symmetric tilt boundary. This results from the crystallographic constraints associated with the shear transformation (i.e., martensite) rather than the low-energy interface that dominates in the diffusional phase transformation (i.e., ferrite).

In situ synchrotron X-ray diffraction studies of the effect of microstructure on tensile behavior and retained austenite stability of thermo-mechanically processed transformation induced plasticity steel

Transmission electron microscopy and in situ synchrotron high-energy X-ray diffraction were used to investigate the martensitic transformation and lattice strains under uniaxial tensile loading of Fe-Mn-Si-C-Nb-Mo-Al Transformation Induced Plasticity (TRIP) steel subjected to different thermo-mechanical processing schedules. In contrast with most of the diffraction analysis of TRIP steels reported previously, the diffraction peaks from the martensite phase were separated from the peaks of the ferrite-bainite α-matrix. The volume fraction of retained γ-austenite, as well as the lattice strain, were determined from the diffraction patterns recorded during tensile deformation. Although significant austenite to martensite transformation starts around the macroscopic yield stress, some austenite grains had already experienced martensitic transformation. Hooke's Law was used to calculate the phase stress of each phase from their lattice strain. The ferrite-bainite α-matrix was observed to yield earlier than austenite and martensite. The discrepancy between integrated phase stresses and experimental macroscopic stress is about 300 MPa. A small increase in carbon concentration in retained austenite at the early stage of deformation was detected, but with further straining a continuous slight decrease in carbon content occurred, indicating that mechanical stability factors, such as grain size, morphology and orientation of the retained austenite, played an important role during the retained austenite to martensite transformation.

Hydrogen permeation in nanostructured bainitic steel

Hydrogen permeation of nanostructured bainitic steel, produced at two different transformation temperatures, i.e., 473.15 K (200 °C) BS-200 and 623.15 K (350 °C) BS-350, was determined using Devanathan–Stachurski hydrogen permeation cell and compared with that of mild steel. Nanostructured bainitic steel showed lower effective diffusivity of hydrogen as compared to the mild steel. The BS-200 steel, which exhibited higher volume fraction of bainitic ferrite phase, showed lower effective diffusivity than BS-350 steel. The finer microstructural constituents (bainitic ferrite laths and retained austenite films) and higher dislocation density in the bainitic ferrite phase of BS-200 steel can be attributed to its lower effective diffusivity as compared to BS-350 steel and mild steel.