Comportamiento mecánico de nuevas aleaciones de wolframio en función de la temperatura

La presente memoria de tesis tiene como objetivo principal la caracterización mecánica en función de la temperatura de nueve aleaciones de wolframio con contenidos diferentes en titanio, vanadio, itria y lantana. Las aleaciones estudiadas son las siguientes: W-0.5%Y2O3, W-2%Ti, W-2% Ti-0.5% Y2O3, W-4% Ti-0.5% Y2O3, W-2%V, W- 2%Vmix, W-4%V, W-1%La2O3 and W-4%V-1%La2O3. Todos ellos, además del wolframio puro se fabrican mediante compresión isostática en caliente (HIP) y son suministradas por la Universidad Carlos III de Madrid. La investigación se desarrolla a través de un estudio sistemático basado en ensayos físicos y mecánicos, así como el análisis post mortem de las muestras ensayadas. Para realizar dicha caracterización mecánica se aplican diferentes ensayos mecánicos, la mayoría de ellos realizados en el intervalo de temperatura de 25 a 1000 º C. Los ensayos de caracterización que se llevan a cabo son: • Densidad • Dureza Vicker • Módulo de elasticidad y su evolución con la temperatura • Límite elástico o resistencia a la flexión máxima, y su evolución con la temperatura • Resistencia a la fractura y su comportamiento con la temperatura. • Análisis microestructural • Análisis fractográfico • Análisis de la relación microestructura-comportamiento macroscópico. El estudio comienza con una introducción acerca de los sistemas en los que estos materiales son candidatos para su aplicación, para comprender las condiciones a las que los materiales serán expuestos. En este caso, el componente que determina las condiciones es el Divertor del reactor de energía de fusión por confinamiento magnético. Parece obvio que su uso en los componentes del reactor de fusión, más exactamente como materiales de cara al plasma (Plasma Facing Components o PFC), hace que estas aleaciones trabajen bajo condiciones de irradiación de neutrones. Además, el hecho de que sean materiales nuevos hace necesario un estudio previo de las características básicas que garantice los requisitos mínimos antes de realizar un estudio más complejo. Esto constituye la principal motivación de la presente investigación. La actual crisis energética ha llevado a aunar esfuerzos en el desarrollo de nuevos materiales, técnicas y dispositivos para la aplicación en la industria de la energía nuclear. El desarrollo de las técnicas de producción de aleaciones de wolframio, con un punto de fusión muy alto, requiere el uso de precursores de sinterizado para lograr densificaciones más altas y por lo tanto mejores propiedades mecánicas. Este es el propósito de la adición de titanio y vanadio en estas aleaciones. Sin embargo, uno de los principales problemas de la utilización de wolframio como material estructural es su alta temperatura de transición dúctil-frágil. Esta temperatura es característica de materiales metálicos con estructura cúbica centrada en el cuerpo y depende de varios factores metalúrgicos. El proceso de recristalización aumenta esta temperatura de transición. Los PFC tienen temperaturas muy altas de servicio, lo que facilita la recristalización del metal. Con el fin de retrasar este proceso, se dispersan partículas insolubles en el material permitiendo temperaturas de servicio más altas. Hasta ahora se ha utilizado óxidos de torio, lantano e itrio como partículas dispersas. Para entender cómo los contenidos en algunos elementos y partículas de óxido afectan a las propiedades de wolframio se estudian las aleaciones binarias de wolframio en comparación con el wolframio puro. A su vez estas aleaciones binarias se utilizan como material de referencia para entender el comportamiento de las aleaciones ternarias. Dada la estrecha relación entre las propiedades del material, la estructura y proceso de fabricación, el estudio se completa con un análisis fractográfico y micrográfico. El análisis fractográfico puede mostrar los mecanismos que están implicados en el proceso de fractura del material. Por otro lado, el estudio micrográfico ayudará a entender este comportamiento a través de la identificación de las posibles fases presentes. La medida del tamaño de grano es una parte de la caracterización microestructural. En esta investigación, la medida del tamaño de grano se llevó a cabo por ataque químico selectivo para revelar el límite de grano en las muestras preparadas. Posteriormente las micrografías fueron sometidas a tratamiento y análisis de imágenes. El documento termina con una discusión de los resultados y la compilación de las conclusiones más importantes que se alcanzan después del estudio. Actualmente, el desarrollo de nuevos materiales para aplicación en los componentes de cara al plasma continúa. El estudio de estos materiales ayudará a completar una base de datos de características que permita hacer una selección de ellos más fiable. The main goal of this dissertation is the mechanical characterization as a function of temperature of nine tungsten alloys containing different amounts of titanium, vanadium and yttrium and lanthanum oxide. The alloys under study were the following ones: W-0.5%Y2O3, W-2%Ti, W-2% Ti-0.5% Y2O3, W-4% Ti-0.5% Y2O3, W-2%V, W- 2%Vmix, W-4%V, W-1%La2O3 and W-4%V-1%La2O3. All of them, besides pure tungsten, were manufactured using a Hot Isostatic Pressing (HIP) process and they were supplied by the Universidad Carlos III de Madrid. The research was carried out through a systematic study based on physical and mechanical tests as well as the post mortem analysis of tested samples. Diverse mechanical tests were applied to perform this characterization; most of them were conducted at temperatures in the range 25-1000 ºC. The following characterization tests were performed: • Density • Vickers hardness • Elastic modulus • Yield strength or ultimate bending strength, and their evolution with temperature • Fracture toughness and its temperature behavior • Microstructural analysis • Fractographical analysis • Microstructure-macroscopic relationship analysis This study begins with an introduction regarding the systems where these materials could be applied, in order to establish and understand their service conditions. In this case, the component that defines the conditions is the Divertor of magnetic-confinement fusion reactors. It seems obvious that their use as fusion reactor components, more exactly as plasma facing components (PFCs), makes these alloys work under conditions of neutron irradiation. In addition to this, the fact that they are novel materials demands a preliminary study of the basic characteristics which will guarantee their minimum requirements prior to a more complex study. This constitutes the motivation of the present research. The current energy crisis has driven to join forces so as to develop new materials, techniques and devices for their application in the nuclear energy industry. The development of production techniques for tungsten-based alloys, with a very high melting point, requires the use of precursors for sintering to achieve higher densifications and, accordingly, better mechanical properties. This is the purpose of the addition of titanium and vanadium to these alloys. Nevertheless, one of the main problems of using tungsten as structural material is its high ductile-brittle transition temperature. This temperature is characteristic of metallic materials with body centered cubic structure and depends on several metallurgical factors. The recrystallization process increases their transition temperature. Since PFCs have a very high service temperature, this facilitates the metal recrystallization. In order to inhibit this process, insoluble particles are dispersed in the material allowing higher service temperatures. So far, oxides of thorium, lanthanum and yttrium have been used as dispersed particles. Tungsten binary alloys are studied in comparison with pure tungsten to understand how the contents of some elements and oxide particles affect tungsten properties. In turn, these binary alloys are used as reference materials to understand the behavior of ternary alloys. Given the close relationship between the material properties, structure and manufacturing process, this research is completed with a fractographical and micrographic analysis. The fractographical analysis is aimed to show the mechanisms that are involved in the process of the material fracture. Besides, the micrographic study will help to understand this behavior through the identification of present phases. The grain size measurement is a crucial part of the microstructural characterization. In this work, the measurement of grain size was carried out by chemical selective etching to reveal the boundary grain on prepared samples. Afterwards, micrographs were subjected to both treatment and image analysis. The dissertation ends with a discussion of results and the compilation of the most important conclusions reached through this work. The development of new materials for plasma facing components application is still under study. The analysis of these materials will help to complete a database of the features that will allow a more reliable materials selection.

Observation of crack initiation during hot tearing

While the general mechanisms of hot tearing are understood, i.e. the inability of liquid to feed imposed strain on the mushy material, work continues on improving the understanding of the mechanisms at play. A hot tear test rig that measures the temperature and load imposed on the mushy zone during solidification has been successfully used to study hot tearing. The mould has now been modified to incorporate a window above the hot spot region to allow observation of hot tear formation and growth. Combining information from visual observation with load and temperature data has led to a better understanding of the mechanism of hot tearing. Tests were carried out on an Al-0.5 wt-% Cu alloy. It was found that load development began at about 90% solid and a hot tear formed a short time later, at between 93% and 96% solid. Hot tearing started at a very low load.

Light alloy castings for automotive applications: The case of Al vs Mg

The economical and environmental effects of mass reduction through Al and Mg primary alloys substitutions for cast iron and steel in automotive components are discussed using MF. Ashby's penalty functions method The viability of Mg alloy substitutions for existing Al alloy cast components is also considered. The cost analysis shows that direct, equal-volume, Al alloy substitutions for cast iron and steel are the most feasible in terms of the CAFE liability, followed by substitutions involving flat panels of prescribed stiffness. When the creation of CO2 associated to the production of Al and Mg is considered, the potential gasoline savings over the lifespan of the car compensate for the intrinsic environmental burden of Al in all applications, while electrolytic Mg substitutions for cast iron and steel are feasible for equal volume and panels only. Magnesium produced by the Pidgeon thermal process appears to be too primary energy intensive to be competitive in structural applications. Magnesium substitutions for existing Al alloy beams and panels are generally unviable. The current higher recycling efficiency of Al casting alloys confers Al a significant advantage over Mg alloys.

Determination of strontium segregation in modified hypoeutectic Al-Si alloy by micro X-ray fluorescence analysis

Analysis of intra- and inter-phase distribution of modifying elements in aluminium-silicon alloys is difficult due to the low concentrations used. This research utilises a mu-XRF (X-ray fluorescence) technique at the SPring-8 synchrotron radiation facility X-ray source and reveals that the modifying element strontium segregates exclusively to the eutectic silicon phase and the distribution of strontium within this phase is relatively homogeneous. This has important implications for the fundamental mechanisms of eutectic modification in hypoeutectic aluminium-silicon alloys. (c) 2006 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Adição de policloreto de alumínio e remoção de peixes bentívoros como técnicas de restauração de lagos rasos do semiárido brasileiro

Eutrophication is the most common cause of water quality degradation in the world. This process occurs by excessive nutrients inputs, nitrogen and phosphorus, to the aquatic systems resulting in algal and cyanobacterial blooms. In shallow lakes these effects are pronounced due to the higher interaction of the lake with watershed, air and sediment. There are innumerous restoration techniques of eutrophied lakes with a range of successful results but there is only one case of successful lake restoration in Brazil: Paranoá Lake in Brasília city. The Brazilian semiarid region has many artificial lakes, named açudes, which are mostly eutrophic and shallow lakes. The eutrophication in these lakes is reported and the phytoplankton community is dominated by potentially toxic cyanobacteria species, mainly Cylindrospermopsis raciborskii. The aim of this thesis is to test techniques for water quality management which can be easily applied in Brazilian semiarid lakes. Results from a laboratory experiment suggest that the addition of a phosphorus sorbent clay associated with an aluminium based coagulant is an effective technique in removing soluble reactive phosphorus and reducing C. raciborskii growth rate – cyanobacteria potentially toxic dominant in reservoirs of Brazilian semiarid – but this effect is dependent on the biomass in the application moment. Results from a field experiment in mesocosm in a eutrophied lake showed that the addition of aluminium based coagulant and removal of benthivorous fish is more efficient in removing total phosphorus and chlorophyll-a from water column than the isolated application of one of the techniques. Lastly, laboratory tests showed that aluminium based coagulant exhibited good performance in removing turbidity and total phosphorus from water of six reservoirs but the efficiency was reduced by algal biomass and pH. The results of this study showed that the improvement in water quality of eutrophied reservoirs in semiarid region is possible through internal loading control by phosphorus precipitation and inactivation in sediments or inhibition of phosphorus release by benthivorous fishes, and also that these results show are additives in water quality improvement.

Adição de policloreto de alumínio e remoção de peixes bentívoros como técnicas de restauração de lagos rasos do semiárido brasileiro

Eutrophication is the most common cause of water quality degradation in the world. This process occurs by excessive nutrients inputs, nitrogen and phosphorus, to the aquatic systems resulting in algal and cyanobacterial blooms. In shallow lakes these effects are pronounced due to the higher interaction of the lake with watershed, air and sediment. There are innumerous restoration techniques of eutrophied lakes with a range of successful results but there is only one case of successful lake restoration in Brazil: Paranoá Lake in Brasília city. The Brazilian semiarid region has many artificial lakes, named açudes, which are mostly eutrophic and shallow lakes. The eutrophication in these lakes is reported and the phytoplankton community is dominated by potentially toxic cyanobacteria species, mainly Cylindrospermopsis raciborskii. The aim of this thesis is to test techniques for water quality management which can be easily applied in Brazilian semiarid lakes. Results from a laboratory experiment suggest that the addition of a phosphorus sorbent clay associated with an aluminium based coagulant is an effective technique in removing soluble reactive phosphorus and reducing C. raciborskii growth rate – cyanobacteria potentially toxic dominant in reservoirs of Brazilian semiarid – but this effect is dependent on the biomass in the application moment. Results from a field experiment in mesocosm in a eutrophied lake showed that the addition of aluminium based coagulant and removal of benthivorous fish is more efficient in removing total phosphorus and chlorophyll-a from water column than the isolated application of one of the techniques. Lastly, laboratory tests showed that aluminium based coagulant exhibited good performance in removing turbidity and total phosphorus from water of six reservoirs but the efficiency was reduced by algal biomass and pH. The results of this study showed that the improvement in water quality of eutrophied reservoirs in semiarid region is possible through internal loading control by phosphorus precipitation and inactivation in sediments or inhibition of phosphorus release by benthivorous fishes, and also that these results show are additives in water quality improvement.

Mineralogical, geochemical and magnetic signatures of surface sediments from the Canadian Beaufort Shelf and Amundsen Gulf (Canadian Arctic)

Mineralogical, geochemical, magnetic, and siliciclastic grain-size signatures of 34 surface sediment samples from the Mackenzie-Beaufort Sea Slope and Amundsen Gulf were studied in order to better constrain the redox status, detrital particle provenance, and sediment dynamics in the western Canadian Arctic. Redox-sensitive elements (Mn, Fe, V, Cr, Zn) indicate that modern sedimentary deposition within the Mackenzie-Beaufort Sea Slope and Amundsen Gulf took place under oxic bottom-water conditions, with more turbulent mixing conditions and thus a well-oxygenated water column prevailing within the Amundsen Gulf. The analytical data obtained, combined with multivariate statistical (notably, principal component and fuzzy c-means clustering analyses) and spatial analyses, allowed the division of the study area into four provinces with distinct sedimentary compositions: (1) the Mackenzie Trough-Canadian Beaufort Shelf with high phyllosilicate-Fe oxide-magnetite and Al-K-Ti-Fe-Cr-V-Zn-P contents; (2) Southwestern Banks Island, characterized by high dolomite-K-feldspar and Ca-Mg-LOI contents; (3) the Central Amundsen Gulf, a transitional zone typified by intermediate phyllosilicate-magnetite-K-feldspar-dolomite and Al-K-Ti-Fe-Mn-V-Zn-Sr-Ca-Mg-LOI contents; and (4) mud volcanoes on the Canadian Beaufort Shelf distinguished by poorly sorted coarse-silt with high quartz-plagioclase-authigenic carbonate and Si-Zr contents, as well as high magnetic susceptibility. Our results also confirm that the present-day sedimentary dynamics on the Canadian Beaufort Shelf is mainly controlled by sediment supply from the Mackenzie River. Overall, these insights provide a basis for future studies using mineralogical, geochemical, and magnetic signatures of Canadian Arctic sediments in order to reconstruct past variations in sediment inputs and transport pathways related to late Quaternary climate and oceanographic changes.

CHARACTERIZATION OF RADIATION DAMAGE TO A NOVEL PHOTONIC CRYSTAL SENSOR

New methods of nuclear fuel and cladding characterization must be developed and implemented to enhance the safety and reliability of nuclear power plants. One class of such advanced methods is aimed at the characterization of fuel performance by performing minimally intrusive in-core, real time measurements on nuclear fuel on the nanometer scale. Nuclear power plants depend on instrumentation and control systems for monitoring, control and protection. Traditionally, methods for fuel characterization under irradiation are performed using a “cook and look” method. These methods are very expensive and labor-intensive since they require removal, inspection and return of irradiated samples for each measurement. Such fuel cladding inspection methods investigate oxide layer thickness, wear, dimensional changes, ovality, nuclear fuel growth and nuclear fuel defect identification. These methods are also not suitable for all commercial nuclear power applications as they are not always available to the operator when needed. Additionally, such techniques often provide limited data and may exacerbate the phenomena being investigated. This thesis investigates a novel, nanostructured sensor based on a photonic crystal design that is implemented in a nuclear reactor environment. The aim of this work is to produce an in-situ radiation-tolerant sensor capable of measuring the deformation of a nuclear material during nuclear reactor operations. The sensor was fabricated on the surface of nuclear reactor materials (specifically, steel and zirconium based alloys). Charged-particle and mixed-field irradiations were both performed on a newly-developed “pelletron” beamline at Idaho State University's Research and Innovation in Science and Engineering (RISE) complex and at the University of Maryland's 250 kW Training Reactor (MUTR). The sensors were irradiated to 6 different fluences (ranging from 1 to 100 dpa), followed by intensive characterization using focused ion beam (FIB), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) to investigate the physical deformation and microstructural changes between different fluence levels, to provide high-resolution information regarding the material performance. Computer modeling (SRIM/TRIM) was employed to simulate damage to the sensor as well as to provide significant information concerning the penetration depth of the ions into the material.

Tailored specular reflectance properties of bulk Cu based novel intermetallic alloys

Significant research has been pursued to develop solar selective metallic coatings using a variety of coating deposition techniques, with limited attempts to assess the properties of bulk metallic materials for solar energy applications. In developing bulk solar reflectors with good reflectance in the entire solar range, we report a new class of reflector materials based on Cu-Sn intermetallics with tailored substitution of aluminium or zinc. Our experimental results suggest that the arc melted-suction cast Cu (78.8 at%)-Al (21.2 at%) alloy with nanoscale surface roughness can exhibit a combination of 89% bulk specular reflectance and 83% bulk solar reflectance, together with a hardness of 2 GPa. We show that the present alloy design approach paves the way for further opportunities of tuning the spectral properties of this new class of solar reflector material. (C) 2016 Elsevier B.V. All rights reserved.

Modelling and characterization of ultrasonic consolidation process of Aluminium alloys

Ultrasonic consolidation process is a rapid manufacturing process used to join thin layers of metal at low temperatures and low energy consumption. In this work, finite element method has been used to simulate the ultrasonic consolidation of Aluminium alloys 6061 (AA-6061) and 3003 (AA-3003). A thermomechanical material model has been developed in the framework of continuum cyclic plasticity theory which takes into account both volume (acoustic softening) and surface (thermal softening due to friction) effects. A friction model based on experimental studies has been developed, which takes into account the dependence of coefficient of friction upon contact pressure, amount of slip, temperature and number of cycles. Using the developed material and friction model ultrasonic consolidation (UC) process has been simulated for various combinations of process parameters involved. Experimental observations are explained on the basis of the results obtained in the present study. The current research provides the opportunity to explain the differences of the behaviour of AA-6061 and AA-3003 during the ultrasonic consolidation process. Finally, trends of the experimentally measured fracture energies of the bonded specimen are compared to the predicted friction work at the weld interface resulted from the simulation at similar process condition. Similarity of the trends indicates the validity of the developed model in its predictive capability of the process. © 2008 Materials Research Society.

Chemical composition modification of casting aluminium alloys for engine applications

The research activities were focused on evaluating the effect of Mo addition to mechanical properties and microstructure of A354 aluminium casting alloy. Samples, with increasing amount of Mo, were produced and heat treated. After heat treatment and exposition to high temperatures samples underwent microstructural and chemical analyses, hardness and tensile tests. The collected data led to the optimization of both casting parameters, for obtaining a homogeneous Mo distribution in the alloy, and heat treatment parameters, allowing the formation of Mo based strengthening precipitates stable at high temperature. Microstructural and chemical analyses highlighted how Mo addition in percentage superior to 0.1% wt. can modify the silicon eutectic morphology and hinder the formation of iron based β intermetallics. High temperature exposure curves, instead, showed that after long exposition hardness is slightly influenced by heat treatment while the effect of Mo addition superior to 0,3% is negligible. Tensile tests confirmed that the addition of 0.3%wt Mo induces an increase of about 10% of ultimate tensile strength after high temperature exposition (250°C for 100h) while heat treatments have slight influence on mechanical behaviour. These results could be exploited for developing innovative heat treatment sequence able to reduce residual stresses in castings produced with A354 modified with Mo.

High-temperature mechanical properties of aluminium alloys reinforced with titanium diboride (TiB2) particles

The physical and mechanical properties of metal matrix composites were improved by the addition of reinforcements. The mechanical properties of particulate-reinforced metal-matrix composites based on aluminium alloys (6061 and 7015) at high temperatures were studied. Titanium diboride (TiB2) particles were used as the reinforcement. All the composites were produced by hot extrusion. The tensile properties and fracture characteristics of these materials were investigated at room temperature and at high temperatures to determine their ultimate strength and strain to failure. The fracture surface was analysed by scanning electron microscopy. TiB2 particles provide high stability of the aluminium alloys (6061 and 7015) in the fabrication process. An improvement in the mechanical behaviour was achieved by adding TiB2 particles as reinforcement in both the aluminium alloys. Adding TiB2 particles reduces the ductility of the aluminium alloys but does not change the microscopic mode of failure, and the fracture surface exhibits a ductile appearance with dimples formed by coalescence.

Influence of the Lubrication Conditions on the Surface Finish of Turned Aeronautical Aluminium Alloys. A preliminary Study

Nowadays, one of the main objectives that affects the development of any new product is the respect for the environment. Until the late 80's, the development and manufacture of the most of the product were aimed to achieve maximum quality in time and costs with environmental issues relegated to secondary importance. On the other hand, in the 90's, the pressure from factors such as markets, financial and legislative factors, led to environmental considerations being taken into account. In this context, the current aeronautical industry strategies are based on the search for economic, environmental and energy efficiency considerations for all the processes involved in the aircraft manufacturing.

The creep properties of a series of zinc-rich zinc-aluminium alloys

The compressive creep behaviour of six sand cast zinc-rich alloys: No3 and No5, corresponding to BS 1004A and BS 1004B, respectively, alloy No2, ILZRO,.16 and two newer alloys ACuZinc5 and ACuZinc10 was investigated. The total creep contraction of the alloys was found to be well correlated using an empirical equation. On the basis of this equation, a parametrical relationship was derived which allowed the total creep contraction to be related to the applied stress, the temperature and the time of test, so that a quantitative assessment of compressive creep of the alloys could be made under different testing conditions. The primary creep and secondary creep rates were found for the alloys at different temperatures and stresses. Generally, the primary creep contraction was found to increase with copper content, whereas secondary creep rates decreased in the order No3, ACuZinc10, ACuZinc5 and No2. ILZRO.16 was tested only at the highest stress and two higher temperatures. The results showed that ILZRO.16 had higher creep resistance than all the other alloys. Thus, based on the above empirical equation, alloy No2 was found to have a substantially better total creep resistance than alloys No3 and No5, and slightly better than ACuZinc5 and ACuZinc10 for strains up to 1%. Both ACuZinc alloys had higher creep strength than commercial alloys No3 and No5. Alloy No5 had much higher creep resistance than alloy No3 under all conditions. The superior creep resistance of alloy No2 was considered to be due to the presence of small precipitates of -phase in the zinc matrix and a regular eutectic morphology. The stress exponents and activation energies for creep under different testing conditions were found to be consistent with some established creep-controlling mechanisms; i.e. dislocation climb for alloy No3, dislocation climb over second phase particles for alloys No5, No2, ACuZinc10, controlled by lattice diffusion in the zinc-rich phase. The lower creep resistance of alloy No3 was mainly due to the lower creep strength of copper-free primary particles having greater volume than eutectic in the microstructure. Alloys No5, ACuZinc5 and ACuZinc10 showed much better creep resistance than alloy No3, based on the precipitation-hardening due to the presence of small -phase precipitates. The primary dendrites in both ACuZinc alloys however were not of much benefit in improving the creep resistance of the alloys.