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This paper describes a study exploring milling and subsequent heat treatments of pure IrO2 and Ta2O5 powders. Reactants were milled under Ar atmosphere in a SPEX 8000D mill, with structural, morphological, and compositional characterizations (during milling and after subsequent heat treatments) by X-ray diffraction, energy-dispersive spectroscopy, and transmission electron microscopy. Electrochemical stability of powders was evaluated by open circuit potential (OCP). Results showed that the mechanical energy transferred during this process induces a reaction between IrO2 and Ta2O5, forming metallic Ir and Ir(Ta)O2 saturated solid solution. The study additionally shows that this reaction can be thermally induced with previous mechanical activation of reactants. Electrochemical evaluations of milled powders immersed in H2SO4 solution revealed that OCP shifts negatively with increasing milling time, approaching that of pure Ir at 15 h milling. Resumen: Este trabajo describe la molienda y subsecuente tratamiento térmico de polvos de IrO2 y Ta2O5. Los reactantes fueron molidos bajo atmósfera de Ar en un molino SPEX 8000D. Los polvos fueron caracterizados mediante difracción de rayos X, espectroscopía de energía dispersiva de rayos X y microscopia electrónica de transmisión. La estabilidad electroquímica fue evaluada mediante potencial de circuito abierto. Los resultados obtenidos mostraron que la energía mecánica transferida durante el proceso de molienda induce la reacción entre el IrO2 y Ta2O5, formando Ir metálico y una solución sólida saturada Ir(Ta)O2. Adicionalmente, se demostró que esta reacción puede ser térmicamente inducida posterior a una activación mecánica de los reactantes. La evaluación electroquímica de los polvos inmersos en una solución de H2SO4, reveló que a medida que el tiempo de molienda aumenta, el potencial de circuito abierto disminuye, hasta alcanzar el potencial presentado por el Ir puro luego de las 15 h de molienda.

This work reports on the electrochemical kinetic analysis of carbon steel powders produced during the milling of carbon steel chips for 2, 3, and 5 h under an air atmosphere in a high-energy ball miller. This work aims to fill the gap in the literature regarding the transformation processes that affect carbon steel powder production. This information can be crucial for specific powder metallurgy systems. The results obtained using the Rietveld refinement method showed a decrease in the crystallite size, an increase in the microstrain, and no changes in the lattice parameter with the milling process. The electrochemical results revealed a strong influence of anodic electroactivity with milling time in NaCl solution, in contrast with NaOH, where the influence of the milling process was not significant. These results clearly show the significant role of chloride ions in preventing the formation of a passive film in milling with NaCl solution and in contrast to the formation of a passive film that notoriously inhibits both the anodic and cathodic reactions in milling with NaOH solution. The novelty of this work lies in the experimental demonstration of milling’s influence on the surface properties of carbon steel powders that directly affect their electrochemical response.

Este trabajo presenta la evolución microestructural del compuesto Mg2Ni0,5Co0,5 obtenido mediante aleado mecánico y el estudio de sus propiedades de hidruración. Los polvos elementales de Mg, Ni y Co con una relación atómica 2:0,5:0,5 se alearon mecánicamente en un molino de alta energía Spex 8000D por 36 h (muestra amorfa) y posteriormente se realizó un tratamiento térmico a 673 K por 15 min (muestra nanocristalina). La caracterización de las muestras amorfas y nanocristalinas se realizó mediante difracción de rayos-X. El proceso de hidruración fue realizado por técnica volumétrica Sievert a 363 K y una presión de H2 de 2 MPa. El proceso de desorción se evaluó por calorimetría diferencial de barrido. Basados en los resultados obtenidos podemos concluir que la estructura amorfa absorbe más hidrógeno, alcanzando un máximo de 3,6% en peso de H2. Los eventos presentes en el proceso de desorción depende de si la aleación es amorfa o nanocristalina.

In this study, weak acid in the curing and leaching stages of copper ore was incorporated, and we analyzed its effect on the dissolution of copper and final impurities. The weak acid corresponds to a wastewater effluent from sulfuric acid plants produced in the gas treatment of copper smelting processes. This effluent is basically water with high acidity (pH-value low at 1), which contains several toxic elements and some valuable metals. The results indicated that there is no positive or negative effect on the incorporation of the weak acid in the curing stage, while the case of the leaching stage is favored. Toxicity characteristic leaching procedure (TCLP) and synthetic precipitation leaching procedure (SPLP) toxicity tests were performed on the solid leaching residues, determining that they accomplish the stability ranges of the impurities (Pb, Cd, Hg, Cr, Ba, Se, As, and Ag).

Este trabajo tuvo como objetivo estudiar la relación existente entre la composición química y el volumen atómico en el sistema Ag – x % at Zn (x ≤ 20). Para este fin, se fabricaron 10 soluciones sólidas mediante fundición y aleado mecánico. La caracterización microestructural se llevó a cabo utilizando difracción de rayos-X. El parámetro reticular fue calculado mediante el método de Rietveld, mientras que la composición química se determinó utilizando espectroscopia de energía dispersiva de rayos-X. En base a los resultados obtenidos se puede concluir que existe una relación lineal inversa entre el volumen atómico de la solución sólida y su contenido Zn, presentando una desviación negativa de la ley de Vegard (-2,96%). Adicionalmente, se propuso una ecuación que vincula el contenido de Zn con el volumen atómico de la solución sólida, la cual presentó un error promedio de predicción menor al 12%.

The aim of this work was to study the synthesis and electrochemical properties of Ti 2 wt %-Si alloys prepared by mechanical alloying (MA) and heat treatment. The MA process was performed under Ar atmosphere. The structural, morphological, and compositional evolutions during the milling and subsequent heat treatment were investigated by X-ray diffraction, energy-dispersive spectroscopy, and scanning electron microscopy. The electrochemical behavior was evaluated by open circuit potential and linear sweep voltammetry measurements. The results showed that the MA process promotes the formation of a supersaturated α-Ti-Si solid solution. During heat treatment, the Si remaining in the mechanically alloyed powders and the Si from the α-Ti-Si supersaturated solid solution reacted with Ti to form Ti-Si intermetallic compounds. These compounds have a fine and homogeneous distribution in the α-Ti matrix, which cannot be achieved by conventional casting methods. Additionally, the electrochemical evaluations revealed that the mechanically alloyed and heat-treated Ti 2 wt %-Si powders have better corrosion resistance in 1.63 M H2SO4 than the pure Ti and MA Ti-Si samples. This is likely due to the particular microstructure produced during the milling and subsequent heat treatment.

Con el objetivo de estudiar el efecto de la activación mecánica sobre la lixiviación de CuFeS2, cuatro muestras de este mineral fueron sometidas a molienda durante 1, 5, 8, y 15 h en un molino Atritor. Los polvos obtenidos fueron caracterizados microestructuralmente y morfológicamente mediante difracción de Rayos-X (DRX) y microscopía electrónica de barrido (MEB), respectivamente. Posteriormente fueron lixiviados en una solución de H2SO4(0,54 M) a temperatura de 298 K. La concentración de Cu+2 en las soluciones fue determinada mediante espectrofotometría de absorción atómica. Los resultados obtenidos indicaron que el aumento del tiempo de molienda provoca un aumento en la recuperación de Cu, alcanzando un valor máximo de 38,2 % para una molienda de 15 h.

In order to study the effect of mechanical activation on the sulphuric acid leaching of CuFeS2, four samples were milled using an Atritor mill during 1, 5, 8, and 15 h. The powders were microstructural and morphologically characterized by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The samples were leached using a solution of H2SO4 (0.54 M) at 298 K. The Cu+2 concentration was determined by means of atomic absorption spectrophotometry. The results obtained indicated that the increase in milling time results in increased recovery of Cu. The maximum recovery of Cu was 38.2 % for a milling time of 15 h.

The manufacture of alloys in solid state has many differences with the conventional melting (casting) process. In the case of high energy milling or mechanical alloying, phase transformations of the raw materials are promoted by a large amount of energy that is introduced by impact with the grinding medium; there is no melting, but the microstructural changes go from microstructural refinement to amorphization in solid state. This work studies the behavior of pure metals (Cu and Ni), and different binary alloys (Cu-Ni and Cu-Zr), under the same milling/mechanical alloying conditions. After high-energy milling, X ray diffraction (XRD) patterns were analyzed to determine changes in the lattice parameter and find both microstrain and crystallite sizes, which were first calculated using the Williamson-Hall (W-H) method and then compared with the transmission electron microscope (TEM) images. Calculations showed a relatively appropriate approach to observations with TEM; however, in general, TEM observations detect heterogeneities, which are not considered for the W-H method. As for results, in the set of pure metals, we show that pure nickel undergoes more microstrain deformations, and is more abrasive than copper (and copper alloys). In binary systems, there was a complete solid solution in the Cu-Ni system and a glass-forming ability for the Cu-Zr, as a function of the Zr content. Mathematical methods cannot be applied when the systems have amorphization because there are no equations representing this process during milling. A general conclusion suggests that, under the same milling conditions, results are very different due to the significant impact of the composition: nickel easily forms a solid solution, while with a higher zirconium content there is a higher degree of glassforming ability.