Relationship between residual stresses and mechanical behavior in ceramic composites

En este trabajo, materiales de tipo alúmina/Y-TZP (ZrO2 tetragonal, estabilizada con 3 mol. % Y2O3), como sistema cerámico popular por sus mejoradas propiedades mecánicas en comparación con las cerámicas de alúmina puras, han sido estudiados en términos de propiedades mecánicas y tensiones residuales. El novedoso método de colado en cinta, consistente en el apilamiento de cintas de cerámica verde a temperatura ambiente y el uso de bajas presiones, se ha escogido para la presente investigación con el fin de poder aprovechar al máximo el futuro desarrollo de materiales laminados de alúmina-óxido de circonio. Se han determinado las propiedades de los materiales obtenidos por este nuevo método de procesamiento comparándolas con las de los materiales obtenidos por “slip casting”, con el fin de analizar si el método propuesto afecta a la microestructura y, por tanto, a las propiedades mecánicas y tensiones residuales propias de estos materiales. Para analizar la idoneidad del proceso de fabricación, utilizado para evitar la presencia de discontinuidades en las intercaras entre las láminas así como otros fenómenos que puedan interferir con las propiedades mecánicas, se estudiaron materiales cerámicos con la misma composición en cintas. Por otra parte también se analizó el efecto de la adición de óxido de circonio sobre la aparición de tensiónes residuales en cerámicas Al2O3/Y-TZP, teniendo en cuenta su notable influencia sobre las propiedades microestructurales y mecánicas de los materiales, así como el requisito de co-sinterización de capas con diferentes materiales compuestos en materiales laminados. La caracterización del material incluye la determinación de la densidad, el análisis de la microestructura, la obtención de las propiedades mecánicas (módulo de elasticidad, dureza, resistencia a la flexión y tenacidad de fractura) así como de las tensiones residuales. En combinación con otros métodos de medida tradicionales, la nanoindentación también se empleó como una técnica adicional para la medida del módulo de elasticidad y de la dureza. Por otro lado, diferentes técnicas de difracción con neutrones, tanto las basadas en longitud de onda constante (CW) como en tiempo de vuelo (TOF), han sido empleadas para la medición fiable de la deformación residual a través del grosor en muestras a granel. Las tensiones residuales fueron determinadas con elevada precisión, aplicando además métodos de análisis apropiados, como por ejemplo el refinamiento de Rietveld. Las diferentes fases en cerámicas sinterizadas, especialmente las de zirconia, se examinaron con detalle mediante el análisis de Rietveld, teniendo en cuenta el complicado polimorfismo del Óxido de Zirconio (ZrO2) así como las posibles transformaciones de fase durante el proceso de fabricación. Los efectos del contenido de Y-TZP en combinación con el nuevo método de procesamiento sobre la microestructura, el rendimiento mecánico y las tensiones residuales de los materiales estudiados (Al2O3/Y-TZP) se resumen en el presente trabajo. Finalmente, los mecanismos de endurecimiento, especialmente los relacionados con las tensiones residuales, son igualmente discutidos. In present work, Alumina/Y-TZP (tetragonal ZrO2 stabilized with 3 mol% Y2O3) materials, as an popular ceramic system with improved mechanical properties compared with the pure alumina ceramics, have been studied in terms of mechanical properties and residual stresses. The novel tape casting method, which involved the stacking of green ceramics tapes at room temperature and using low pressures, is selected for manufacturing and investigation, in order to take full advantage of the future development of alumina-zirconia laminated materials. Features of materials obtained by the new processing method are determined and compared with those of materials obtained by conventional slip casting in a plaster mold, in order to study whether the proposed method of processing affects microstructure and thereby the mechanical properties and residual stresses characteristics of materials. To analyse the adequacy of the manufacturing process used to avoid the presence of discontinuities at the interfaces between the sheets and other phenomena that interfere with the mechanical properties, ceramic materials with the same composition in tapes were investigated. Moreover, the effect of addition of zirconia on residual stress development of Al2O3/Y-TZP ceramics were taken into investigations, considering its significantly influence on the microstructure and mechanical properties of materials as well as the requirement of co-sintering of layers with different composites in laminated materials. The characterization includes density, microstructure, mechanical properties (elastic modulus, hardness, flexure strength and fracture toughness) and residual stresses. Except of the traditional measurement methods, nanoindentation technique was also used as an additional measurement of the elastic modulus and hardness. Neutron diffraction, both the constant-wavelength (CW) and time-of-flight (TOF) neutron diffraction techniques, has been used for reliable through-thickness residual strain measurement in bulk samples. Residual stresses were precisely determined combined with appropriate analysis methods, e.g. the Rietveld refinement. The phase compositions in sintered ceramics especially the ones of zirconia were accurately examined by Rietveld analysis, considering the complex polymorph of ZrO2 and the possible phase transformation during manufacturing process. Effects of Y-TZP content and the new processing method on the microstructure, mechanical performance and residual stresses were finally summarized in present studied Al2O3/Y-TZP materials. The toughening mechanisms, especially the residual stresses related toughening, were theoretically discussed.

The effects of tantalum addition on the microtexture and mechanical behaviour of tungsten for ITER applications

Tungsten (W) and its alloys are very promising materials for producing plasma-facing components (PFCs) in the fusion power reactors of the near future, even as a structural part in them. However, whereas the properties of pure tungsten are suitable for a PFC, its structural applications are still limited due to its low toughness, ductile to brittle transition temperature and recrystallization behaviour. Therefore, many efforts have been made to improve its performance by alloying tungsten with other elements. Hence, in this investigation, the thermo-mechanical performance of two new tungsten-tantalum materials has been evaluated. Materials with We5wt.%Ta and We15wt.%Ta were processed by mechanical alloying (MA) and later consolidation by hot isostatic pressing (HIP), with distinct settings for each composition. Thus, it was possible to determine the relationship between the microstructure and the addition of Ta with the macroscopic mechanical properties. These were measured by means of hardness, flexural strength and fracture toughness, in the temperature range of 300e1473 K. The microstructure and the fracture surfaces features of the tested materials were analysed by Field Emission Scanning Electron Microscopy (FESEM).

Topographical and mechanical characterization of living eukaryotic cells on opaque substrates: development of a general procedure and its application to the study of non-adherent lymphocytes

The mechanical behavior of living murine T-lymphocytes was assessed by atomic force microscopy (AFM). A robust experimental procedure was developed to overcome some features of lymphocytes, in particular their spherical shape and non-adherent character. The procedure included the immobilization of the lymphocytes on amine-functionalized substrates, the use of hydrodynamic effects on the deflection of the AFM cantilever to monitor the approaching, and the use of the jumping mode for obtaining the images. Indentation curves were analyzed according to Hertz's model for contact mechanics. The calculated values of the elastic modulus are consistent both when considering the results obtained from a single lymphocyte and when comparing the curves recorded from cells of different specimens

Tyrosine replacement in P-selectin glycoprotein ligand-1 affects distinct kinetic and mechanical properties of bonds with P- and L-selectin

Selectins are adhesion molecules that initiate tethering and rolling of leukocytes on the vessel wall. Rolling requires rapid formation and breakage of selectin–ligand bonds that must have mechanical strength to resist premature dissociation by the forces applied in shear flow. P- and L-selectin bind to the N-terminal region of P-selectin glycoprotein ligand-1 (PSGL-1), a mucin on leukocytes. To define determinants on PSGL-1 that contribute to the kinetic and mechanical properties of bonds with selectins, we compared rolling of transfected preB cells expressing P- or L-selectin on transfected cell monolayers expressing wild-type PSGL-1 or PSGL-1 constructs with substitutions in targeted N-terminal residues. Rolling through P- or L-selectin required a Thr or Ser at a specific position on PSGL-1, the attachment site for an essential O-glycan, but required only one of three nearby Tyr residues, which are sites for Tyr-SO3 formation. The adhesive strengths and numbers of cells rolling through P- or L-selectin were similar on wild-type PSGL-1 and on each of the three PSGL-1 constructs containing only a single Tyr. However, the cells rolled more irregularly on the single-Tyr forms of PSGL-1. Analysis of the lifetimes of transient tethers on limiting densities of PSGL-1 revealed that L-selectin dissociated faster from single-Tyr than wild-type PSGL-1 at all shears examined. In sharp contrast, P-selectin dissociated faster from single-Tyr than wild-type PSGL-1 at higher shear but not at lower shear. Thus, tyrosine replacements in PSGL-1 affect distinct kinetic and mechanical properties of bonds with P- and L-selectin.

Solid-state synthesis and mechanical unfolding of polymers of T4 lysozyme

Recent advances in single molecule manipulation methods offer a novel approach to investigating the protein folding problem. These studies usually are done on molecules that are naturally organized as linear arrays of globular domains. To extend these techniques to study proteins that normally exist as monomers, we have developed a method of synthesizing polymers of protein molecules in the solid state. By introducing cysteines at locations where bacteriophage T4 lysozyme molecules contact each other in a crystal and taking advantage of the alignment provided by the lattice, we have obtained polymers of defined polarity up to 25 molecules long that retain enzymatic activity. These polymers then were manipulated mechanically by using a modified scanning force microscope to characterize the force-induced reversible unfolding of the individual lysozyme molecules. This approach should be general and adaptable to many other proteins with known crystal structures. For T4 lysozyme, the force required to unfold the monomers was 64 ± 16 pN at the pulling speed used. Refolding occurred within 1 sec of relaxation with an efficiency close to 100%. Analysis of the force versus extension curves suggests that the mechanical unfolding transition follows a two-state model. The unfolding forces determined in 1 M guanidine hydrochloride indicate that in these conditions the activation barrier for unfolding is reduced by 2 kcal/mol.

Structure and mechanical properties of sodium and calcium caseinate edible active films with carvacrol

Edible active films based on sodium caseinate (SC) and calcium caseinate (CC) plasticized with glycerol (G) at three different concentrations and carvacrol (CRV) as active agent were prepared by solvent casting. Transparent films were obtained and their surfaces were analysed by optical microscopy and scanning electron microscopy (SEM). The influence of the addition of three different plasticizer concentrations was studied by determining tensile properties, while Fourier transformed infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA) were used to evaluate the structural and thermal behavior of such films. The addition of glycerol resulted in a reduction in the elastic modulus and tensile strength, while some increase in the elongation at break was observed. In general terms, SC films showed flexibility higher than the corresponding CC counterparts. In addition, the presence of carvacrol caused further improvements in ductile properties suggesting the presence of stronger interactions between the protein matrix and glycerol, as it was also observed in thermal degradation studies. FTIR spectra of all films showed the characteristic bands and peaks corresponding to proteins as well as to primary and secondary alcohols. In summary, the best results regarding mechanical and structural properties for caseinates-based films containing carvacrol were found for the formulations with high glycerol concentrations.

Fire-resistance, physical, and mechanical characterization of particleboard containing Oceanic Posidonia waste

In this work, particleboards manufactured with Oceanic Posidonia waste and bonded with cement are investigated. The particleboards are made with 3/1.5/0.5 parts of cement per part of Posidonia waste. The physical properties of bulk density, swelling, surface absorption, and dimensional changes due to relative humidity as well as the mechanical properties of modulus of elasticity, bending strength, surface soundness, perpendicular tensile strength and impact resistance are studied. In terms of the above properties, the best results were obtained for particleboards with high cement content and when the waste “leaves” are treated (crushed) before board fabrication, due to internal changes to the board structure under these conditions. Based on the results of fire tests, the particleboard is non-flammable without any fire-resistant treatment.

Temperature influence on the physical and mechanical properties of a porous rock: San Julian's calcarenite

This work discusses the results from tests which were performed in order to study the effect of high temperatures in the physical and mechanical properties of a calcarenite (San Julian's stone). Samples, previously heated at different temperatures (from 105 °C to 600 °C), were tested. Non-destructive tests (porosity and ultrasonic wave propagation) and destructive tests (uniaxial compressive strength and slake durability test) were performed over available samples. Furthermore, the tests were carried out under different conditions (i.e. air-cooled and water-cooled) in order to study the effect of the fire off method. The results show that uniaxial compressive strength and elastic parameters (i.e. elastic modulus and Poisson's ratio), decrease as the temperature increases for the tested range of temperatures. A reduction of the uniaxial compressive strength up to 35% and 50% is observed in air-cooled and water-cooled samples respectively when the samples are heated to 600 °C. Regarding the Young's modulus, a fall over 75% and 78% in air-cooled and water-cooled samples respectively is observed. Poisson's ratio also declines up to 44% and 68% with the temperature in air-cooled and water-cooled samples respectively. Slake durability index also exhibits a reduction with temperature. Other physical properties, closely related with the mechanical properties of the stone, are porosity, attenuation and propagation velocity of ultrasonic waves in the material. All exhibit considerable changes with temperature.

Ethylene vinyl acetate/nanoclay-based pigment composites: Morphology, rheology, and mechanical, thermal, and colorimetric properties

In this study, a new type of nanopigment, obtained from a nanoclay (NC) and a dye, was synthesized in the laboratory, and these nanopigments were used to color an ethylene vinyl acetate (EVA) copolymer. Several of these nanoclay-based pigments (NCPs) were obtained through variations in the cation exchange capacity (CEC) percentage of the NC exchanged with the dye and also including an ammonium salt. Composites of EVA and different amounts of the as-synthesized nanopigments were prepared in a melt-intercalation process. Then, the morphological, mechanical, thermal, rheological, and colorimetric properties of the samples were assessed. The EVA/NCP composites developed much better color properties than the samples containing only the dye, especially when both the dye and the ammonium salt were exchanged with NC. Their other properties were similar to those of more conventional EVA/NC composites.

Linear low-density polyethylene colored with a nanoclay-based pigment: Morphology and mechanical, thermal, and colorimetric properties

In this study, a novel kind of hybrid pigment based on nanoclays and dyes was synthesized and characterized. These nanoclay-based pigments (NCPs) were prepared at the laboratory with sodium montmorillonite nanoclay (NC) and methylene blue (MB). The cation-exchange capacity of NC exchanged with MB was varied to obtain a wide color gamut. The synthesized nanopigments were thoroughly characterized. The NCPs were melt-mixed with linear low-density polyethylene (PE) with an internal mixer. Furthermore, samples with conventional colorants were prepared in the same way. Then, the properties (mechanical, thermal, and colorimetric) of the mixtures were assessed. The PE–NCP samples developed better color properties than those containing conventional colorants and used as references, and their other properties were maintained or improved, even at lower contents of dye compared to that with the conventional colorants.