Papers by Author: Ricardo Mendes Leal Neto

Abstract: The aim of this work is to investigate the influence of some processes variables on the microstructure and hydrogen absorption kinetics of MgH₂ - X wt.% TiFe composites. Samples were synthesized by high-energy ball milling in a planetary (X = 40, 50, 60) and shaker mill (X = 40) under high-purity argon atmosphere. Commercial MgH₂ instead of Mg powder was used in order to reduce adherence on the vial and balls. TiFe powder was previously produced by ball milling a mixture of TiH₂ and Fe powders followed by a reaction synthesis at 600oC. Milled composites samples were characterized by XRD and SEM analysis. Milling time was preliminary investigated (X = 40) in the planetary ball mill (6 to 36h). TiFe particle size reduction was shown to be difficult since they are surrounded by MgH2 matrix. Strong particle reduction was obtained by using a shaker mill only for 2 hours and adding cyclohexane as process control agent. No reaction between MgH₂ and TiFe compound was observed in any milled sample. Hydrogen absorption kinetics measurements of the as-milled samples were conducted on an Sieverts' type apparatus at room temperature after hydrogen desorption at 350oC under vacuum. The best hydrogen kinetics (3 wt% at the first hour) was attained by the planetary milled sample (36 h). Higher hydrogen capacity was observed for the sample milled in the shaker mill (4.0 wt.%), but only after 13h.

Abstract: Tungsten carbide is potentially attractive for development of catalysts and widely used for fabrication of cutting tools due to its high hardness and wear resistance while the ball milling can improve the mechanical properties from the metastable structures and nanomaterials. The aim of this work was to evaluate the phase transformations during milling of the W-50at%C elemental powder mixture under argon atmosphere in a planetary P-5 ball mill using WC-Co balls (10 mm diameter) and vials (225 mL), 200 rpm, and a ball-to-powder weight ratio of 10:1. Samples were collected into the vial after different times: 20, 60, 300 and 600 min. The as-milled W-50at%C powders were characterized by X-ray diffraction (XRD). Only peaks of W were identified in W-50at%C powders milled up to 600 min, which were broadened and moved to the direction of smaller diffraction angle. In addition, the lattice parameter and cell volume of W were reduced during ball milling of W-50at%C powders, indicating that the C atoms dissolved into the W lattice in order to form metastable structures. Carbon atoms were interstitially dissolved into the W lattice during the initial milling times, and its preferential substitutional dissolution was identified for longer times due to the larger amounts of crystallographic defects during ball milling.

Abstract: TiFe compound was produced by high-energy ball milling of TiH₂ and Fe powders, followed by heating under vacuum. TiH₂ was used instead of Ti in order to avoid the strong particles adhesion to grinding balls and vial walls. Mixtures of TiH₂ and Fe powders were dry-milled in a planetary mill for times ranging from 5 to 40 hours. The amount of sample, number and diameter of the balls were kept constant in all experiments. After milling, samples were heated under dynamic high-vacuum for the synthesis reaction. As-milled and heat-treated materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and differential thermal analysis (DTA). The mean crystallite sizes and microstrains were determined by XRD line profile analysis using the Warren-Averbach method. As-milled materials presented only Fe and TiH₂ phases. Nanostructured TiFe compound was formed after heat treatment. TiH₂ was effective for providing low adherence of the powders during milling.

Abstract: For the last 30 years high uranium density dispersion fuels have been developed in order to accomplish the low enrichment goals of the Reduced Enrichment for Research and Test Reactors (RERTR) Program. Gamma U-Mo alloys, particularly with 7 to 10 wt% Mo, as a fuel phase dispersed in aluminum matrix, have shown good results concerning its performance under irradiation tests. Thats why this fissile phase is considered to be used in the nuclear fuel of the Brazilian Multipurpose Research Reactor (RMB), currently being designed. Powder production from these ductile alloys has been attained by atomization, mechanical (machining, grinding, cryogenic milling) and chemical (hydriding-dehydriding) methods. This work is a part of the efforts presently under way at IPEN to investigate the feasibility of these methods. Results on alloy fabrication by induction melting and γ-stabilization of U-10Mo alloys are presented. Some results on powder production and characterization are also discussed.

Abstract: The effect of mechanical activation procedures on the combustion synthesis of NbAl3 was investigated. The activation was carried out by a two-step high energy ball milling procedure. In the first milling, aluminum and niobium were milled separately (pre-activation). The mixture of pre-activated powders was then activated in the second milling. Reaction synthesis, by simultaneous combustion mode, was conducted on compacted pellets made of powder mixtures with and without pre-activation. The thermal behavior of the compacted pellets upon heating was recorded and the main thermal combustion reaction characteristics were evaluated. The two-step procedure produced aggregates with a globular dispersion of niobium due to increased particle hardness and decreasing mean particle size during pre-activation milling. Analysis of pellet thermal behavior showed the two-step milling procedure could enhance reaction performance by increasing maximum reaction heating rate and temperature gain during reaction.

Abstract: This work reports the efforts to obtain TiFe intermetallic compound by high-energy ball milling of Ti and Fe powder mixtures. This process route has been used to provide a better hydrogen intake in this compound. Milling was carried out in a SPEX mill at different times. Strong adherence of material at the vial walls was seen to be the main problem at milling times higher than 1 hour. Attempts to solve this problem were accomplished by adding different process control agents, like ethanol, stearic acid, low density polyethylene, benzene and cyclohexane at variable quantities and keeping constant other milling parameters like ball to powder ration and balls size. Better results were attained with benzene and cyclohexane, but with partial formation of TiFe compound even after a heat treatment (annealing) of the milled samples.

Abstract: The behavior of different process control agents (PCAs) during mechanical activation of Nb75Al powder mixtures was investigated. Mechanical activation by high-energy ball milling was carried out on a shaker mill (SPEX®8000) for 1 hour. Each PCA (Stearic acid, ethanol and methanol) was added to the powder charge in two proportions (1 and 2 wt%). Shape and microstructure of activated powders (aggregates) were analyzed by scanning electron microscopy. Milled powder mixtures were uniaxially pressed in cylindrical compacts that were further vacuum reacted at a constant heating rate (30°C/min) in order to produce NbAl3 intermetallic compound. The temperature of the samples was monitored by an S-type thermocouple. The results show that the shape and the microstructure of the milled powders were strongly affected by the type and quantity of PCAs, therefore changing the reaction behavior and the densification of the produced pellets. Although ethanol was more effective to control aggregate size, best densification results were attained with 2 wt% of stearic acid.

Abstract: In this work shake milling were used to mechanically activate Nb – Al powder mixtures at different relative proportions (Nb80Al, Nb65Al, Nb54Al e Nb42Al). All milling process parameters were unchanged, e.g., powders mass, ball/powder mass ratio, balls diameter, quantity and kind of process control agent. Uniaxially compacted cylindrical pellets of milled powders were vacuum reacted. After a two-step degassing treatment (290°C for 0.5 h and 400°C for 4 h), samples were heated at 30°C/min. Ignition and combustion temperatures were measured by a thermocouple inserted in a hole drilled into the pellets. The microstructure of milled powders and reacted pellets were characterized by X-ray diffraction and SEM analysis. Bulk density of the pellets was measured by water immersion (Archimedes). The results showed a decrease of both ignition and combustion temperature with mechanical activation as seen by comparison with reacted pellets of the same composition not mechanically activated (simple mixtures). By increasing the heating hate the completeness of the reactions were improved. The lower the aluminum contents the lower the ignition and combustion temperatures and also the densification. The decrease on ignition temperature was caused by a more effective dispersion (and so more activation) attained by samples with lower aluminum content.

Abstract: It is well known that colloidal powder particles (between 1 mm and 0.001 mm) tend to agglomerate due to electrostatic forces. Then assuring an optimal dispersion condition is essential for good particle-size analysis results, since aggregates or weak agglomerates can be measured as single particles. In this paper the particle size distribution of an alumina powder A1000SG (ALCOA) was measured using distinct dispersion procedures. Distilled water was used as dispersant liquid in the pure state and with additives (citric acid and Duramax D-3005). Dispersion by supersonic vibration was also investigated, but only the application time was varied. Particle size analysis was accomplished by laser scattering technique and the dispersion condition was evaluated through zeta potential. The results showed that the Duramax’s electrosteric impediment is more efficient than citric acid’s electrostatic force, thereby providing better dispersion. Although useful, the supersonic vibration was not good enough to assure an optimal dispersion, at least for the material tested here.