Obtaining and stability verification of superconducting phases of the Nb-Al and Nb-Sn systems by mechanical alloying and low-temperature heat treatments

The development of Nb(3)Al and Nb(3)Sn superconductors is of great interest for the applied superconductivity area. These intermetallics composites are obtained normally by heat treatment reactions at high temperature. Processes that allow formation of the superconducting phases at lower temperatures (<1000 degrees C), particularly for Nb(3)Al, are of great interest. The present work studies phase formation and stability of Nb(3)Al and Nb(3)Sn superconducting phases using mechanical alloying (high energy ball milling). Our main objective was to form composites near stoichiometry, which could be transformed into the superconducting phases using low-temperature heat treatments. High purity Nb-Sn and Nb-Al powders were mixed to generate the required superconducting phases (Nb-25at.%Sn and Nb-25at.%Al) in an argon atmosphere glove-box. After milling in a Fritsch mill, the samples were compressed in a hydraulic uniaxial press and encapsulated in evacuated quartz tubes for heat treatment. The compressed and heat treated samples were characterized using X-ray diffractometry. Microstructure and chemical analysis were accomplished using scanning electron microscopy and energy dispersive spectrometry. Nb(3)Al XRD peaks were observed after the sintering at 800 degrees C for the sample milled for 30 h. Nb(3)Sn XRD peaks could be observed even before the heat treatment. (C) 2009 Elsevier B.V. All rights reserved.

Thermal expansion of the V(5)Si(3) and T(2) phases of the V-Si-B system investigated by high-temperature X-ray diffraction

The thermal expansion anisotropy of the V(5)Si(3) and T(2)-phase of the V-Si-B system were determined by high-temperature X-ray diffraction from 298 to 1273 K. Alloys with nominal compositions V(62.5)Si(37.5) (V5Si3 phase) and V(63)Si(12)B(25) (T(2)-phase) were prepared from high-purity materials through arc-melting followed by heat-treatment at 1873 K by 24 h, under argon atmosphere. The V(5)Si(3) phase exhibits thermal expansion anisotropy equals to 1.3, with thermal expansion coefficients along the a and c-axis equal to 9.3 x 10(-6) K(-1) and 11.7 x 10(-6) K(-1), respectively. Similarly, the thermal expansion anisotropy value of the T(2)-phase is 0.9 with thermal expansion coefficients equal to 8.8 x 10(-6) K(-1) and 8.3 x 10(-6) K(-1) along the, a and c-axis respectively. Compared to other isostructural silicides of the 5:3 type and the Ti(5)Si(3) phase, the V(5)Si(3) phase presents lower thermal expansion anisotropy. The T(2)-phase present in the V-Si-B system exhibits low thermal expansion anisotropy, as the T(2)-phase of the Mo-Si-B, Nb-Si-B and W-Si-B systems. (C) 2009 Elsevier Ltd. All rights reserved.

Thermal, structural and optical properties of Al(2)CoO(4)-Crocoite composite nanoparticles used as pigments

Al(2)CoO(4)-PbCrO(4) and Al(2)CoO(4)-Pb(2)CrO(5) crystalline powders in different proportions were obtained by the polymeric precursor method. Differential scanning calorimetry (DSC) and thermogravimetry (TG) techniques were used to accurately characterize the distinct thermal events occurring during synthesis. The TG and DSC results revealed a series of overlapping decomposition reactions due to different exothermal events, which were identified as H(2)O and NO(x) elimination and polymer pyrolysis. The X-ray diffraction patterns of the xAl(2)CoO(4)-(1 - x)PbCrO(4) and xAl(2)CoO(4)-(1 - x)Pb(2)CrO(5) mixed compounds, with x = 1, 0.75, 0.5, 0.25 and 0, were obtained in the crystalline form with their respective phases, and proved consistent with the nominal compositions. The synthesis of these two systems yielded nine different colors and shades.

Modification of surface properties of Ti-16Si-4B powder alloy by plasma immersion ion implantation

Results of the surface modification of Ti-16Si-4B powder alloy by nitrogen ion implantation are presented, together with the experimental description of the preparation of that powder by high-energy ball milling and hot pressing. The phase structure, chemical composition and morphology of sample surfaces were observed by utilizing X-ray diffractometer (XRD), atomic force microscope (AFM) and scanning electron microscopy (SEM). A tribological characterization was carried out with a ball-on-disc tribometer and an SEM. Friction coefficient is compared with the one obtained for Ti-6Al-4V alloy and the wear scars characterized by SEM/EDS (energy dispersive spectroscopy). The concentration profile of the detected elements have been investigated using Auger electron spectroscopy (AES) depth profiling. Our results show that a shallow implanted layer of oxygen and nitrogen ions were obtained at the Ti-16Si -4B alloy surface, sufficient to modify slightly its tribological properties. Crown Copyright (C) 2011 Published by Elsevier Ltd. All rights reserved.

Crystallisation behaviour and glass-forming ability in Al-La-Ni system

The crystallisation behaviour for alloys in the Al-rich corner in the Al-La-Ni system is reported in this paper Alloys were selected based on the topological instability criterion (lambda criterion) calculated from the alloy composition and metallic radii of the alloying elements and aluminum Amorphous ribbons were produced by melt-spinning and the crystallisation reactions were analysed by X-ray diffraction and calorimetry The results showed that increasing the values of lambda from 0.072 to 0.16 resulted in the following changes in the crystallisation behaviour, as predicted by the lambda criterion (a) nanocrystallisation of alpha-Al for the alloy composition corresponding to lambda = 0 072 and (b) detection of the glass transition temperature, T(g), for the alloys with composition close to lambda approximate to 0.1 line. For compositions corresponding to both ends of the lambda approximate to 0 1 line (near the binaries lines) T(g) could be detected only in the ""intermediary"" central region, and the alloy we produced in this region was considered the best glass former for the Al-rich corner Also, except for the alloys with the highest NI content, crystallisation proceeded by two distinct exothermic peaks which are typical of nanocrystallisation transformation. These behaviours are discussed in terms of compositional (lambda parameter) and topological aspects to account for cluster formation in the amorphous phase. Crown Copyright (C) 2009 Published by Elsevier B V All rights reserved

Study of soils by thermal analysis

The study of soils is very important in the geological and geological engineering researches. A study of ten samples of soils was carried out by thermal analysis, and X-Ray Fluorescence Spectrometry to understand soil evolution in Angra dos Reis region, Rio de Janeiro State, Brazil. The sample collection sites were chosen based on geological characteristics, the soil layer thickness, the soil composition pattern, and whether or not it was moved either by erosion or by gravitational shifts. Because of the humid tropical climatic condition, natural soils tend to show great thickness of weathered mantles with formation of saprolites and saprolite soils. Kaolinite is an important secondary mineral which can be formed from many different minerals, like k-mica and k-feldspar and can be weathered to gibbsite. The results from TG/DTG and DTA indicated which soils had more weathering, and the same results were obtained by XRF, when silica/aluminum ratios from samples are compared with thermal analysis results.

Hydrogen production from soft-drink wastewater in an upflow anaerobic packed-bed reactor

The production of hydrogen from soft-drink wastewater in two upflow anaerobic packed-bed reactors was evaluated. The results show that soft-drink wastewater is a good source for hydrogen generation. Data from both reactors indicate that the reactor without medium containing macro- and micronutrients (R2) provided a higher hydrogen yield (3.5 mol H(2) mol(-1) of sucrose) as compared to the reactor (R1) with a nutrient-containing medium (3.3 mol H(2) mol(-1) of sucrose). Reactor R2 continuously produced hydrogen, whereas reactor R1 exhibited a short period of production and produced lower amounts of hydrogen. Better hydrogen production rates and percentages of biogas were also observed for reactor R2, which produced 0.4 L h(-1) L(-1) and 15.8% of H(2), compared to reactor R1, which produced 0.2 L h(-1) L(-1) and 2.6% of H(2). The difference in performance between the reactors was likely due to changes in the metabolic pathway for hydrogen production and decreases in bed porosity as a result of excessive biomass growth in reactor R1. Molecular biological analyses of samples from reactors R1 and R2 indicated the presence of several microorganisms, including Clostridium (91% similarity), Enterobacter (93% similarity) and Klebsiella (97% similarity). Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.

Fermentative hydrogen production by microbial consortium

Heat pre-treatment of the inoculum associated to the pH control was applied to select hydrogen-producing bacteria and endospores-forming bacteria. The source of inoculum to the heat pre-treatment was from a UASB reactor used in the slaughterhouse waste treatment. The molecular biology analyses indicated that the microbial consortium presented microorganisms affiliated with Enterobacter cloacae (97% and 98%), Clostridium sp. (98%) and Clostridium acetobutyricum (96%), recognized as H, and volatile acids` producers. The following assays were carried out in batch reactors in order to verify the efficiencies of sucrose conversion to H-2 by the microbial consortium: (1) 630.0 mg sucrose/L, (2) 1184.0 mg sucrose/L, (3) 1816.0 mg sucrose/L and (4) 4128.0 mg sucrose/L. The subsequent yields were obtained as follows: 15% (1.2 mol H-2/mol sucrose), 20% (1.6 mol H-2/mol sucrose), 15% (1.2 mol H-2/mol sucrose) and 4% (0.3 mol H-2/mol sucrose), respectively. The intermediary products were acetic acid, butyric acid, methanol and ethanol in all of the anaerobic reactors. (C) 2008 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.

Glass formation of alloys selected by lambda and electronegativity criteria in the Ti-Zr-Fe-Co system

This work evaluates the glass formation of selected alloys based on the Ti-Zr-Fe-Co system, assuming the synergy of two distinct criteria: minimum topological instability and average electronegativity plots. Combining the minimum topological instability and the average electronegativity values result in a plot in which the most probable good glass former compositions are identified Ti-Zr rich alloys with Fe and Co additions were produced, compared against the final plot, and the best glass forming alloy composition was found to be very close the theoretically predicted ones on the Ti-Zr rich side, for both Ti-Zr-Fe and Ti-Zr-Co systems. (C) 2009 Elsevier B V All rights reserved

Crystallisation behaviours of Al-based metallic glasses: Compositional and topological aspects

The different types of thermal crystallisation behaviours observed during continuous heating of M-based metallic glasses have been successfully associated with the topological instability. criterion, which is simply calculated from the alloy composition and metallic radii of the alloying elements and aluminium. In the present work, we report on new results evidencing the correlation between the values of X and the crystallisation behaviours in Al-based alloys of the Al-Ni-Ce system and we compare the glass-forming abilities of alloys designed with compositions corresponding to the same topological instability condition. The results are discussed in terms of compositional and topological aspects emphasizing the relevance of the different types of clusters in the amorphous phase in defining the stability of the glass and the types of thermal crystallisation. (C) 2008 Elsevier B.V. All rights reserved.

Topological instability, average electronegativity difference and glass forming ability of amorphous alloys

In this paper, we report the remarkable agreement of the glass forming ability of binary alloys with a new criterion that combines the topological instability parameter (lambda) and the average electronegativity difference among the elements of an alloy, assuming both exert a synergetic effect. The best glass forming compositions for Zr-Cu and Ti-Ni systems are well predicted by this new approach. Although the new criterion needs further refinement, it is concluded that the proposed approach is a promising and simple tool to guide and reduce the tedious and labour intensive work to find good glass former compositions in metallic systems. (C) 2008 Elsevier Ltd. All rights reserved.

Thermodynamic and topological instability approaches for forecasting glass-forming ability in the ternary Al-Ni-Y system

A thermodynamic approach to predict bulk glass-forming compositions in binary metallic systems was recently proposed. In this approach. the parameter gamma* = Delta H-amor/(Delta H-inter - Delta H-amor) indicates the glass-forming ability (GFA) from the standpoint of the driving force to form different competing phases, and Delta H-amor and Delta H-inter are the enthalpies for-lass and intermetallic formation, respectively. Good glass-forming compositions should have a large negative enthalpy for glass formation and a very small difference for intermetallic formation, thus making the glassy phase easily reachable even under low cooling rates. The gamma* parameter showed a good correlation with GFA experimental data in the Ni-Nb binary system. In this work, a simple extension of the gamma* parameter is applied in the ternary Al-Ni-Y system. The calculated gamma* isocontours in the ternary diagram are compared with experimental results of glass formation in that system. Despite sonic misfitting, the best glass formers are found quite close to the highest gamma* values, leading to the conclusion that this thermodynamic approach can lie extended to ternary systems, serving as a useful tool for the development of new glass-forming compositions. Finally the thermodynamic approach is compared with the topological instability criteria used to predict the thermal behavior of glassy Al alloys. (C) 2007 Elsevier B. V. All rights reserved.

Predicting glass-forming compositions in the Al-La and Al-La-Ni systems

In this work, a criterion considering the topological instability (lambda) and the differences in the electronegativity of the constituent elements (Delta e) was applied to the Al-La and Al-Ni-La systems in order to predict the best glass-forming compositions. The results were compared with literature data and with our own experimental data for the Al-La-Ni system. The alloy described in the literature as the best glass former in the Al-La system is located near the point with local maximum for the lambda.Delta e criterion. A good agreement was found between the predictions of the lambda.Delta e criterion and literature data in the Al-La-Ni system, with the region of the best glass-forming ability (GFA) and largest supercooled liquid region (Delta T(x)) coinciding with the best compositional region for amorphization indicated by the lambda.Delta e criterion. Four new glassy compositions were found in the Al-La-Ni system, with the best predicted composition presenting the best glass-forming ability observed so far for this system. Although the lambda.Delta e criterion needs further refinements for completely describe the glass-forming ability in the Al-La and Al-La-Ni systems, the results demonstrated that this criterion is a good tool to predict new glass-forming compositions. (C) 2010 Elsevier B. V. All rights reserved.

Anaerobic fluidized bed reactor with expanded clay as support for hydrogen production through dark fermentation of glucose

This study evaluated hydrogen production in an anaerobic fluidized bed reactor (AFBR) fed with glucose-based synthetic wastewater. Particles of expanded clay (2.8-3.35 mm) were used as a support material for biomass immobilization. The reactor was operated with hydraulic retention times (HRT) ranging from 8 to 1 h. The hydrogen yield production increased from 1.41 to 2.49 mol H(2) Mol(-1) glucose as HRT decreased from 8 to 2 h. However, when HRT was 1 h, there was a slight decrease to 2.41 mol H(2) Mol(-1) glucose. The biogas produced was composed of H(2) and CO(2), and the H(2) content increased from 8% to 35% as HRT decreased. The major soluble metabolites during H(2) fermentation were acetic acid (HAc) and butyric acid (HBu), accounting for 36.1-53.3% and 37.7-44.9% of total soluble metabolites, respectively. Overall, the results demonstrate the potential of using expanded clay as support material for hydrogen production in AFBRs. (c) 2008 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.

TiAlN coatings deposited by triode magnetron sputtering varying the bias voltage

TiAlN films were deposited on AISI O1 tool steel using a triode magnetron sputtering system. The bias voltage effect on the composition, thickness, crystallography, microstructure, hardness and adhesion strength was investigated. The coatings thickness and elemental composition analyses were carried out using scanning electron microscopy (SEM) together with energy dispersive X-ray (EDS). The re-sputtering effect due to the high-energy ions bombardment on the film surface influenced the coatings thickness. The films crystallography was investigated using X-ray diffraction characterization. The X-ray diffraction (XRD) data show that TiAlN coatings were crystallized in the cubic NaCl B1 structure, with orientations in the {111}, {200} {220} and {311} crystallographic planes. The surface morphology (roughness and grain size) of TiAlN coatings was investigated by atomic force microscopy (AFM). By increasing the substrate bias voltage from -40 to -150 V, hardness decreased from 32 GPa to 19 GPa. Scratch tester was used for measuring the critical loads and for measuring the adhesion. (C) 2011 Elsevier B. V. All rights reserved.