Crack mechanical failure in ceramic materials under ion irradiation: case of lithium niobate crystal

Swift heavy ion irradiation (ions with mass heavier than 15 and energy exceeding MeV/amu) transfer their energy mainly to the electronic system with small momentum transfer per collision. Therefore, they produce linear regions (columnar nano-tracks) around the straight ion trajectory, with marked modifications with respect to the virgin material, e.g., phase transition, amorphization, compaction, changes in physical or chemical properties. In the case of crystalline materials the most distinctive feature of swift heavy ion irradiation is the production of amorphous tracks embedded in the crystal. Lithium niobate is a relevant optical material that presents birefringence due to its anysotropic trigonal structure. The amorphous phase is certainly isotropic. In addition, its refractive index exhibits high contrast with those of the crystalline phase. This allows one to fabricate waveguides by swift ion irradiation with important technological relevance. From the mechanical point of view, the inclusion of an amorphous nano-track (with a density 15% lower than that of the crystal) leads to the generation of important stress/strain fields around the track. Eventually these fields are the origin of crack formation with fatal consequences for the integrity of the samples and the viability of the method for nano-track formation. For certain crystal cuts (X and Y), these fields are clearly anisotropic due to the crystal anisotropy. We have used finite element methods to calculate the stress/strain fields that appear around the ion- generated amorphous nano-tracks for a variety of ion energies and doses. A very remarkable feature for X cut-samples is that the maximum shear stress appears on preferential planes that form +/-45º with respect to the crystallographic planes. This leads to the generation of oriented surface cracks when the dose increases. The growth of the cracks along the anisotropic crystal has been studied by means of novel extended finite element methods, which include cracks as discontinuities. In this way we can study how the length and depth of a crack evolves as function of the ion dose. In this work we will show how the simulations compare with experiments and their application in materials modification by ion irradiation.

Detailed damage mechanisms assessment in composite materials by means of X-ray tomography

This research focused on the evaluation of damage formation on ±45º carbon fiber laminates subjected to tensile tests. The damage was evaluated by means of X-ray tomography. A high density of cracks developed during the plateau of the stress-strain curve and were qualitatively analyzed, showing that the inner plies eventually developed a higher crack concentration than the outer plies. Delamination started to occur in the outermost ply interface when the slope after the plateau of the stress-strain curve began to increase.

A level set approach for the analysis of flow and compaction during resin infusion in composite materials

Fluid flow and fabric compaction during vacuum assisted resin infusion (VARI) of composite materials was simulated using a level set-based approach. Fluid infusion through the fiber preform was modeled using Darcy’s equations for the fluid flow through a porous media. The stress partition between the fluid and the fiber bed was included by means of Terzaghi’s effective stress theory. Tracking the fluid front during infusion was introduced by means of the level set method. The resulting partial differential equations for the fluid infusion and the evolution of flow front were discretized and solved approximately using the finite differences method with a uniform grid discretization of the spatial domain. The model results were validated against uniaxial VARI experiments through an [0]8 E-glass plain woven preform. The physical parameters of the model were also independently measured. The model results (in terms of the fabric thickness, pressure and fluid front evolution during filling) were in good agreement with the numerical simulations, showing the potential of the level set method to simulate resin infusion

Analytical bearing capacity of strip footing in weightless materials with power-law failure criteria

Sokolovskii’s method of characteristics is extended to provide analytical solutions for the ultimate load at the moment of plastic failure under plane-strain conditions of shallow strip foundations on weightless rigid-plastic media with a noncohesive power-law failure envelope. The formulation is made parametrically in terms of the instantaneous friction angle, and the key idea to obtain the bearing capacity is that information can be transmitted from the free surface (where external loads are known) to the contact plane of the foundation. The methodology can consider foundations adjacent to a slope, external surcharges at the free surface, and inclined loads (both on the slope and on the foundation). Sensitivity analyses illustrate the influence on bearing capacity of changes in the different geometrical parameters involved. An application example is presented and design plots are provided, and model predictions are compared with results of bearing capacity tests under low gravity.

Estudios de especiación de arsénico y acumulación de metales en muestras de interés medioambiental : Arsenic speciation and metal accumulation studies in environmental samples

Se ha estudiado la determinación de especies de arsénico y de contenidos totales de arsénico y metales pesados, específicamente cadmio, cromo, cobre, níquel, plomo y cinc, en muestras de interés medioambiental por su elevada capacidad acumuladora de metales, concretamente algas marinas comestibles y plantas terrestres procedentes de suelos contaminados por la actividad minera. La determinación de contenidos totales se ha llevado a cabo mediante espectrometría de emisión atómica con plasma de acoplamiento inductivo (ICP‐AES), así como por espectrometría de fluorescencia atómica con generación de hidruros (HG‐AFS), para bajos contenidos de arsénico. Las muestras fueron mineralizadas en medio ácido y calentamiento en horno de microondas. Los métodos fueron validados a través de su aplicación a materiales de referencia de matriz similar a la de las muestras, certificados en contenidos totales de los elementos seleccionados. Los resultados obtenidos mostraron su elevada capacidad de bioabsorción, especialmente en relación a los elevados contenidos de arsénico encontrados en algunas especies de algas pardas (Phaeophytas). En las plantas, se calcularon los factores de translocación, acumulación y biodisponibilidad de los elementos estudiados, permitiendo identificar a la especie Corrigiola telephiifolia como posible acumuladora de plomo e hiperacumuladora de arsénico. La determinación de especies de arsénico hidrosolubles en las muestras objeto de estudio, se llevó a cabo por cromatografía líquida de alta eficacia (HPLC) acoplado a ICP‐AES, HG‐ICP‐AES y HG‐AFS, incluyendo una etapa previa de foto‐oxidación. Los métodos desarrollados, mediante intercambio aniónico y catiónico, permitieron la diferenciación de hasta once especies de arsénico. Para el análisis de las muestras, fue necesaria la optimización de métodos de extracción, seleccionándose la extracción asistida por microondas (MAE) con agua desionizada. Asimismo, se realizaron estudios de estabilidad de arsénico total y de las especies hidrosolubles presentes en las algas, tanto sobre la muestra sólida como en sus extractos acuosos, evaluando las condiciones de almacenamiento adecuadas. En el caso de las plantas, la aplicación del diseño factorial de experimentos permitió optimizar el método de extracción y diferenciar entre las especies de arsénico presentes en forma de iones sencillos de mayor movilidad y el arsénico más fuertemente enlazado a componentes estructurales. Los resultados obtenidos permitieron identificar la presencia de arseniato (As(V)) y arsenito (As(III)) en las plantas, así como de ácido monometilarsónico (MMA) y óxido de trimetilarsina (TMAO) en algunas especies. En la mayoría de las algas se encontraron especies tóxicas, tanto mayoritarias (arseniato) como minoritarias (ácido dimetilarsínico (DMA)), así como hasta cuatro arsenoazúcares. Los resultados obtenidos y su estudio a través de la legislación vigente, mostraron la necesidad de desarrollar una reglamentación específica para el control de este tipo de alimentos. La determinación de especies de arsénico liposolubles en las muestras de algas se llevó a cabo mediante HPLC, en modo fase inversa, acoplado a espectrometría de masas con plasma de acoplamiento inductivo (ICP‐MS) y con ionización por electrospray (ESI‐MS), permitiendo la elucidación estructural de estos compuestos a través de la determinación de sus masas moleculares. Para ello, fue necesaria la puesta a punto de métodos extracción y purificación de los extractos. La metodología desarrollada permitió identificar hasta catorce especies de arsénico liposolubles en las algas, tres de ellas correspondientes a hidrocarburos que contienen arsénico, y once a arsenofosfolípidos, además de dos especies desconocidas. Las masas moleculares de las especies identificadas fueron confirmadas mediante cromatografía de gases acoplada a espectrometría de masas (GC‐MS) y espectrometría de masas de alta resolución (HR‐MS). ABSTRACT The determination of arsenic species and total arsenic and heavy metal contents (cadmium, chromium, cooper, nickel, lead and zinc) in environmental samples, with high metal accumulator capacity, has been studied. The samples studied were edible marine algae and terrestrial plants from soils polluted by mining activities. The determination of total element contents was performed by inductively coupled plasma atomic emission spectrometry (ICP‐AES), as well as by hydride generation atomic fluorescence spectrometry (HG‐AFS) for low arsenic contents. The samples studied were digested in an acidic medium by heating in a microwave oven. The digestion methods were validated against reference materials, with matrix similar to sample matrix and certified in total contents of the elements studied. The results showed the high biosorption capacity of the samples studied, especially regarding the high arsenic contents in some species of brown algae (Phaeophyta division). In terrestrial plants, the translocation, accumulation and bioavailability factors of the elements studied were calculated. Thus, the plant species Corrigiola telephiifolia was identified as possible lead accumulator and arsenic hyperaccumulator. The determination of water‐soluble arsenic species in the samples studied was carried out by high performance liquid chromatography (HPLC) coupled to ICP‐AES, HG‐ICP‐AES and HG‐AFS, including a prior photo‐oxidation step. The chromatographic methods developed, by anion and cation exchange, allowed us to differentiate up to eleven arsenic species. The sample analysis required the optimization of extraction methods, choosing the microwave assisted extraction (MAE) with deionized water. On the other hand, the stability of total arsenic and water‐soluble arsenic species in algae, both in the solid samples and in the water extracts, was studied, assessing the suitable storage conditions. In the case of plant samples, the application of a multivariate experimental design allowed us to optimize the extraction method and differentiate between the arsenic species present as simple ions of higher mobility and the arsenic more strongly bound to structural components. The presence of arsenite (As(III)) and arsenate (As(V)) was identified in plant samples, as well as monomethylarsonic acid (MMA) and trimethylarsine oxide (TMAO) in some cases. Regarding algae, toxic arsenic species were found in most of them, both As(V) and dimethylarsinic acid (DMA), as well as up to four arsenosugars. These results were discussed according to the current legislation, showing the need to develop specific regulations to control this kind of food products. The determination of lipid‐soluble arsenic species in alga samples was performed by reversed‐phase HPLC coupled to inductively coupled plasma and electrospray mass spectrometry (ICP‐MS and ESI‐MS), in order to establish the structure of these compounds by determining the corresponding molecular masses. For this purpose, it was necessary to develop an extraction method, as well as a clean‐up method of the extracts. The method developed permitted the identification of fourteen lipid‐soluble arsenic compounds in algae, corresponding to three arsenic‐hydrocarbons and eleven arsenosugarphospholipids, as well as two unknown compounds. Accurate mass measurements of the identified compounds were performed by gas chromatography coupled to mass spectrometry (GC‐MS) and high resolution mass spectrometry (HR‐MS).

D-depth profiling in as-implanted and annealed Li-based breeder blanket ceramics

In future power plants (i.e. DEMO), the nuclear fusion of hydrogen isotopes will be used for energy production. The behaviour of hydrogen isotopes in lithium-enriched ceramics for breeder blankets (BBs) is one of the most important items to be understood. In this paper we present the chemical, microstructural and morphological features of Li4SiO4, Li2TiO3 and a third ceramic candidate with a higher Li:Si proportion (3:1), implanted with D at an energy of 100 keV and at room temperature at a fluence of 1 × 1017 cm−2. The D depth-profile in as-implanted and annealed ceramics (at T ⩽ 200 °C) was characterised by Resonance Nuclear Reaction Analysis (RNRA). The RNRA data indicate that the total amount of D is retained at room temperature, while annealing at 100 °C promotes D release and annealing at T ⩾ 150 °C drives D to completely desorb from all the studied ceramics. D release will be discussed as a function of the microstructurural and morphological features of each material.

Damage localization and failure locus under biaxial loading in glass-fiber nonwoven felts

The pattern of damage localization and fracture under uniaxial and biaxial tension was studied in glass–fiber nonwoven felts. The analyses were carried out within the framework of the finite-element simulation of plain and notched specimens in which the microstructure of the felt, made up of fiber bundles connected at the cross point through an organic binder, was explicitly represented. Following previous experimental observations, fracture by interbundle decohesion and energy dissipation by frictional sliding between the bundles were included in the model. It was found that the failure path in these materials was controlled by the maximum applied normal stress, regardless of the loading path, and that the failure locus under biaxial tension was well represented by the von Mises failure criteria. The notch sensitivity of the nonwoven felts was limited and the presence of a notch did not modify the failure path.

Three dimensional (3D) microstructure-based modeling of interfacial decohesion in particle reinforced metal matrix composites

Modeling and prediction of the overall elastic–plastic response and local damage mechanisms in heterogeneous materials, in particular particle reinforced composites, is a very complex problem. Microstructural complexities such as the inhomogeneous spatial distribution of particles, irregular morphology of the particles, and anisotropy in particle orientation after secondary processing, such as extrusion, significantly affect deformation behavior. We have studied the effect of particle/matrix interface debonding in SiC particle reinforced Al alloy matrix composites with (a) actual microstructure consisting of angular SiC particles and (b) idealized ellipsoidal SiC particles. Tensile deformation in SiC particle reinforced Al matrix composites was modeled using actual microstructures reconstructed from serial sectioning approach. Interfacial debonding was modeled using user-defined cohesive zone elements. Modeling with the actual microstructure (versus idealized ellipsoids) has a significant influence on: (a) localized stresses and strains in particle and matrix, and (b) far-field strain at which localized debonding takes place. The angular particles exhibited higher degree of load transfer and are more sensitive to interfacial debonding. Larger decreases in stress are observed in the angular particles, because of the flat surfaces, normal to the loading axis, which bear load. Furthermore, simplification of particle morphology may lead to erroneous results.

Study of the temperature distribution in Si nanowires under microscopic laser beam excitation

The use of laser beams as excitation sources for the characterization of semiconductor nanowires (NWs) is largely extended. Raman spectroscopy and photoluminescence (PL) are currently applied to the study of NWs. However, NWs are systems with poor thermal conductivity and poor heat dissipation, which result in unintentional heating under the excitation with a focused laser beam with microscopic size, as those usually used in microRaman and microPL experiments. On the other hand, the NWs have subwavelength diameter, which changes the optical absorption with respect to the absorption in bulk materials. Furthermore, the NW diameter is smaller than the laser beam spot, which means that the optical power absorbed by the NW depends on its position inside the laser beam spot. A detailed analysis of the interaction between a microscopic focused laser beam and semiconductor NWs is necessary for the understanding of the experiments involving laser beam excitation of NWs. We present in this work a numerical analysis of the thermal transport in Si NWs, where the heat source is the laser energy locally absorbed by the NW. This analysis takes account of the optical absorption, the thermal conductivity, the dimensions, diameter and length of the NWs, and the immersion medium. Both free standing and heat-sunk NWs are considered. Also, the temperature distribution in ensembles of NWs is discussed. This analysis intends to constitute a tool for the understanding of the thermal phenomena induced by laser beams in semiconductor NWs.

Mechanical properties enhancement of high reliability metallic materials by laser shock processing

Laser shock processing (LSP) is being increasingly applied as an effective technology for the improvement of metallic materials surface properties in different types of components as a means of enhancement of their corrosion and fatigue life behavior. As reported in previous contributions by the authors, a main effect resulting from the application of the LSP technique consists on the generation of relatively deep compression residual stresses field into metallic alloy pieces allowing an improved mechanical behaviour, explicitly the life improvement of the treated specimens against wear, crack growth and stress corrosion cracking. Additional results accomplished by the authors in the line of practical development of the LSP technique at an experimental level (aiming its integral assessment from an interrelated theoretical and experimental point of view) are presented in this paper. Concretely, follow-on experimental results on the residual stress profiles and associated surface properties modification successfully reached in typical materials (especially Al and Ti alloys) under different LSP irradiation conditions are presented along with a practical correlated analysis on the protective character of the residual stress profiles obtained under different irradiation strategies and the evaluation of the corresponding induced properties as material specific volume reduction at the surface, microhardness and wear resistance. Additional remarks on the improved character of the LSP technique over the traditional “shot peening” technique in what concerns depth of induced compressive residual stresses fields are also made through the paper.

Effect of Thermal Treatments on the Mechanical Properties Enhancement of High Reliability Metallic Materials by Laser Shock Processing

Laser shock processing (LSP) is increasingly applied as an effective technology for the improvement of metallic materials mechanical properties in different types of components as a means of enhancement of their fatigue life behavior. As reported in previous contributions by the authors, a main effect resulting from the application of the LSP technique consists on the generation of relatively deep compression residual stresses fields into metallic components allowing an improved mechanical behaviour, explicitly the life improvement of the treated specimens against wear, crack growth and stress corrosion cracking. Additional results accomplished by the authors in the line of practical development of the LSP technique at an experimental level (aiming its integral assessment from an interrelated theoretical and experimental point of view) are presented in this paper. Concretely, experimental results on the residual stress profiles and associated mechanical properties modification successfully reached in typical materials under different LSP irradiation conditions are presented. In this case, the specific behavior of a widely used material in high reliability components (especially in nuclear and biomedical applications) as AISI 316L is analyzed, the effect of possible “in-service” thermal conditions on the relaxation of the LSP effects being specifically characterized. I.

Discrete (MD) and continuum (DD) simulations of void growth in single crystals.

Void growth in ductile materials is an important problem from the fundamental and technological viewpoint. Most of the models developed to quantify and understand the void growth process did not take into account two important factors: the anisotropic nature of plastic flow in single crystals and the size effects that appear when plastic flow is confined into very small regions.

High fidelity simulations of failure in fiber-reinforced composites

Los ensayos virtuales de materiales compuestos han aparecido como un nuevo concepto dentro de la industria aeroespacial, y disponen de un vasto potencial para reducir los enormes costes de certificación y desarrollo asociados con las tediosas campañas experimentales, que incluyen un gran número de paneles, subcomponentes y componentes. El objetivo de los ensayos virtuales es sustituir algunos ensayos por simulaciones computacionales con alta fidelidad. Esta tesis es una contribución a la aproximación multiescala desarrollada en el Instituto IMDEA Materiales para predecir el comportamiento mecánico de un laminado de material compuesto dadas las propiedades de la lámina y la intercara. La mecánica de daño continuo (CDM) formula el daño intralaminar a nivel constitutivo de material. El modelo de daño intralaminar se combina con elementos cohesivos para representar daño interlaminar. Se desarrolló e implementó un modelo de daño continuo, y se aplicó a configuraciones simples de ensayos en laminados: impactos de baja y alta velocidad, ensayos de tracción, tests a cortadura. El análisis del método y la correlación con experimentos sugiere que los métodos son razonablemente adecuados para los test de impacto, pero insuficientes para el resto de ensayos. Para superar estas limitaciones de CDM, se ha mejorado la aproximación discreta de elementos finitos enriqueciendo la cinemática para incluir discontinuidades embebidas: el método extendido de los elementos finitos (X-FEM). Se adaptó X-FEM para un esquema explícito de integración temporal. El método es capaz de representar cualitativamente los mecanismos de fallo detallados en laminados. Sin embargo, los resultados muestran inconsistencias en la formulación que producen resultados cuantitativos erróneos. Por último, se ha revisado el método tradicional de X-FEM, y se ha desarrollado un nuevo método para superar sus limitaciones: el método cohesivo X-FEM estable. Las propiedades del nuevo método se estudiaron en detalle, y se concluyó que el método es robusto para implementación en códigos explícitos dinámicos escalables, resultando una nueva herramienta útil para la simulación de daño en composites. Virtual testing of composite materials has emerged as a new concept within the aerospace industry. It presents a very large potential to reduce the large certification costs and the long development times associated with the experimental campaigns, involving the testing of a large number of panels, sub-components and components. The aim of virtual testing is to replace some experimental tests by high-fidelity numerical simulations. This work is a contribution to the multiscale approach developed in Institute IMDEA Materials to predict the mechanical behavior of a composite laminate from the properties of the ply and the interply. Continuum Damage Mechanics (CDM) formulates intraply damage at the the material constitutive level. Intraply CDM is combined with cohesive elements to model interply damage. A CDM model was developed, implemented, and applied to simple mechanical tests of laminates: low and high velocity impact, tension of coupons, and shear deformation. The analysis of the results and the comparison with experiments indicated that the performance was reasonably good for the impact tests, but insuficient in the other cases. To overcome the limitations of CDM, the kinematics of the discrete finite element approximation was enhanced to include mesh embedded discontinuities, the eXtended Finite Element Method (X-FEM). The X-FEM was adapted to an explicit time integration scheme and was able to reproduce qualitatively the physical failure mechanisms in a composite laminate. However, the results revealed an inconsistency in the formulation that leads to erroneous quantitative results. Finally, the traditional X-FEM was reviewed, and a new method was developed to overcome its limitations, the stable cohesive X-FEM. The properties of the new method were studied in detail, and it was demonstrated that the new method was robust and can be implemented in a explicit finite element formulation, providing a new tool for damage simulation in composite materials.

Decoupling of soil nutrient cycles as a function of aridity in global drylands

The biogeochemical cycles of carbon (C), nitrogen (N) and phosphorus (P) are interlinked by primary production, respiration and decomposition in terrestrial ecosystems. It has been suggested that the C, N and P cycles could become uncoupled under rapid climate change because of the different degrees of control exerted on the supply of these elements by biological and geochemical processes. Climatic controls on biogeochemical cycles are particularly relevant in arid, semi-arid and dry sub-humid ecosystems (drylands) because their biological activity is mainly driven by water availability. The increase in aridity predicted for the twenty-first century in many drylands worldwide may therefore threaten the balance between these cycles, differentially affecting the availability of essential nutrients. Here we evaluate how aridity affects the balance between C, N and P in soils collected from 224 dryland sites from all continents except Antarctica. We find a negative effect of aridity on the concentration of soil organic C and total N, but a positive effect on the concentration of inorganic P. Aridity is negatively related to plant cover, which may favour the dominance of physical processes such as rock weathering, a major source of P to ecosystems, over biological processes that provide more C and N, such as litter decomposition. Our findings suggest that any predicted increase in aridity with climate change will probably reduce the concentrations of N and C in global drylands, but increase that of P. These changes would uncouple the C, N and P cycles in drylands and could negatively affect the provision of key services provided by these ecosystems.

Effect of Thermal Treatments on the Mechanical Properties Enhancement of High Reliability Metallic Materials by Laser Shock Processing

Laser shock processing (LSP) is increasingly applied as an effective technology for the improvement of metallic materials mechanical properties in different types of components as a means of enhancement of their fatigue life behavior. As reported in previous contributions by the authors, a main effect resulting from the application of the LSP technique consists on the generation of relatively deep compression residual stresses fields into metallic components allowing an improved mechanical behaviour, explicitly the life improvement of the treated specimens against wear, crack growth and stress corrosion cracking. Additional results accomplished by the authors in the line of practical development of the LSP technique at an experimental level (aiming its integral assessment from an interrelated theoretical and experimental point of view)are presented in this paper. Concretely, experimental results on the residual stress profiles and associated mechanical properties modification successfully reached in typical materials under different LSP irradiation conditions are presented. In this case, the specific behavior of a widely used material in high reliability components (especially in nuclear and biomedical applications) as AISI 316L is analyzed, the effect of possible “in-service” thermal conditions on the relaxation of the LSP effects being specifically characterized.