Evaluating the reinforcement of inorganic fullerene-like nanoparticles in thermoplastic matrices by depth-sensing indentation

The reinforcing effect of inorganic fullerene-like tungsten disulfide (IF-WS2) nanoparticles in two different polymer matrices, isotactic polypropylene (iPP) and polyphenylene sulfide (PPS), has been investigated by means of dynamic depth-sensing indentation. The hardness and elastic modulus enhancement upon filler addition is analyzed in terms of two main contributions: changes in the polymer matrix nanostructure and intrinsic properties of the filler including matrix-particle load transfer. It is found that the latter mainly determines the overall mechanical improvement, whereas the nanostructural changes induced in the polymer matrix only contribute to a minor extent. Important differences are suggested between the mechanisms of deformation in the two nanocomposites, resulting in a moderate mechanical enhancement in case of iPP (20% for a filler loading of 1%), and a remarkable hardness increase in case of PPS (60% for the same filler content). The nature of the polymer amorphous phase, whether in the glassy or rubbery state, seems to play here an important role. Finally, nanoindentation and dynamic mechanical analysis measurements are compared and discussed in terms of the different directionality of the stresses applied.

Strain rate effect on semi‐crystalline plla mechanical properties measured by instrumented indentation tests

Poly(L‐lactide) is a widely studied biomaterial, currently approved for use in a range of medical devices. Its mechanical properties can be tailored giving the material different crystallinity degrees. PLLA presents a complex non‐linear behaviour that depends not only on structural parameters such as crystallinity degree but also on external parameters such as strain rate and temperature. Failure of polymeric implants is attributed to their intrinsic time‐dependent performance under static loading conditions.

Determining the elastic-plastic properties of metallic materials through instrumented indentation

En los últimos años, y asociado al desarrollo de la tecnología MEMS, la técnica de indentación instrumentada se ha convertido en un método de ensayo no destructivo ampliamente utilizado para hallar las características elástico-plásticas de recubrimientos y capas delgadas, desde la escala macroscópica a la microscópica. Sin embargo, debido al complejo mecanismo de contacto debajo de la indentación, es urgente proponer un método más simple y conveniente para obtener unos resultados comparables con otras mediciones tradicionales. En este estudio, el objetivo es mejorar el procedimiento analítico para extraer las propiedades elástico-plásticas del material mediante la técnica de indentación instrumentada. La primera parte se centra en la metodología llevada a cabo para medir las propiedades elásticas de los materiales elásticos, presentándose una nueva metodología de indentación, basada en la evolución de la rigidez de contacto y en la curva fuerza-desplazamiento del ensayo de indentación. El método propuesto permite discriminar los valores de indentación experimental que pudieran estar afectados por el redondeo de la punta del indentador. Además, esta técnica parece ser robusta y permite obtener valores fiables del modulo elástico. La segunda parte se centra en el proceso analítico para determinar la curva tensión-deformación a partir del ensayo de indentación, empleando un indentador esférico. Para poder asemejar la curva tension-deformación de indentación con la que se obtendría de un ensayo de tracción, Tabor determinó empíricamente un factor de constricción de la tensión () y un factor de constricción de la deformación (). Sin embargo, la elección del valor de y  necesitan una derivación analítica. Se describió analíticamente una nueva visión de la relación entre los factores de constricción de tensión y la deformación basado en la deducción de la ecuación de Tabor. Un modelo de elementos finitos y un diseño experimental se realizan para evaluar estos factores de constricción. A partir de los resultados obtenidos, las curvas tension-deformación extraidas de los ensayos de indentación esférica, afectadas por los correspondientes factores de constricción de tension y deformación, se ajustaron a la curva nominal tensión-deformación obtenida de ensayos de tracción convencionales. En la última parte, se estudian las propiedades del revestimiento de cermet Inconel 625-Cr3C2 que es depositado en el medio de una aleación de acero mediante un láser. Las propiedades mecánicas de la matriz de cermet son estudiadas mediante la técnica de indentación instrumentada, haciendo uso de las metodologías propuestas en el presente trabajo. In recent years, along with the development of MEMS technology, instrumented indentation, as one type of a non-destructive measurement technique, is widely used to characterize the elastic and plastic properties of metallic materials from the macro to the micro scale. However, due to the complex contact mechanisms under the indentation tip, it is necessary to propose a more convenient and simple method of instrumented indention to obtain comparable results from other conventional measurements. In this study, the aim is to improve the analytical procedure for extracting the elastic plastic properties of metallic materials by instrumented indentation. The first part focuses on the methodology for measuring the elastic properties of metallic materials. An alternative instrumented indentation methodology is presented. Based on the evolution of the contact stiffness and indentation load versus the depth of penetration, the possibility of obtaining the actual elastic modulus of an elastic-plastic bulk material through instrumented sharp indentation tests has been explored. The proposed methodology allows correcting the effect of the rounding of the indenter tip on the experimental indentation data. Additionally, this technique does not seem too sensitive to the pile-up phenomenon and allows obtaining convincing values of the elastic modulus. In the second part, an analytical procedure is proposed to determine the representative stress-strain curve from the spherical indentation. Tabor has determined the stress constraint factor (stress CF), and strain constraint factor (strain CF), empirically but the choice of a value for and is debatable and lacks analytical derivation. A new insight into the relationship between stress and strain constraint factors is analytically described based on the formulation of Tabor’s equation. Finite element model and experimental tests have been carried out to evaluate these constraint factors. From the results, representative stress-strain curves using the proposed strain constraint factor fit better with the nominal stress-strain curve than those using Tabor’s constraint factors. In the last part, the mechanical properties of an Inconel 625-Cr3C2 cermet coating which is deposited onto a medium alloy steel by laser cladding has been studied. The elastic and plastic mechanical properties of the cermet matrix are studied using depth-sensing indentation (DSI) on the micro scale.

Mapping of mechanical properties of cement paste microstructures

The presented study is related to the EU 7 th Framework Programme CODICE (COmputationally Driven design of Innovative CEment-based materials). The main aim of the project is the development of a multi-scale model for the computer based simulation of mechanical and durability performance of cementitious materials. This paper reports results of micro/nano scale characterisation and mechanical property mapping of cementitious skeletons formed by the cement hydration at different ages. Using the statistical nanoindentation and micro-mechanical property mapping technique, intrinsic properties of different hydrate phases, and also the possible interaction (or overlapping) of different phases (e.g. calcium-silcate-hydrates) has been studied. Results of the mapping and statistical indentation testing appear to suggest the possible existence of more hydrate phases than the commonly reported LD and HD C-S-H and CH phases

Bond modelling of prestressed concrete during the prestressing force release

This paper presents an analytical model for simulating the bond between steel and concrete, in precast prestressed concrete elements, during the prestressing force release. The model establishes a relationship between bond stress, steel and concrete stress and slip in such concrete structures. This relationship allows us to evaluate the bond stress in the transmission zone, where bond stress is not constant, along the whole prestressing force release process. The model is validated with the results of a series of tests, considering different steel indentation depths and concrete covers and is extended to evaluate the transmission length. This capability has been checked by comparing the transmission length predicted by the model and one measured experimentally in two series of tests.

Determination of the mechanical properties of amorphous materials through instrumented nanoindentation

A novel methodology based on instrumented indentation is developed to determine the mechanical properties of amorphous materials which present cohesive-frictional behaviour. The approach is based on the concept of a universal hardness equation, which results from the assumption of a characteristic indentation pressure proportional to the hardness. The actual universal hardness equation is obtained from a detailed finite element analysis of the process of sharp indentation for a very wide range of material properties, and the inverse problem (i.e. how to extract the elastic modulus, the compressive yield strength and the friction angle) from instrumented indentation is solved. The applicability and limitations of the novel approach are highlighted. Finally, the model is validated against experimental data in metallic and ceramic glasses as well as polymers, covering a wide range of amorphous materials in terms of elastic modulus, yield strength and friction angle.

Study of bond stress-slip relationship and radial dilation in prestressed concrete

This paper presents two test procedures for evaluating the bond stress–slip and the slip–radial dilation relationships when the prestressing force is transmitted by releasing the steel (wire or strand) in precast prestressed elements. The bond stress–slip relationship is obtained with short length specimens, to guarantee uniform bond stress, for three depths of the wire indentation (shallow, medium and deep). An analytical model for bond stress–slip relationship is proposed and compared with the experimental results. The model is also compared with the experimental results of other researchers. Since numerical models for studying bond-splitting problems in prestressed concrete require experimental data about dilatancy angle (radial dilation), a test procedure is proposed to evaluate these parameters. The obtained values of the radial dilation are compared with the prior estimated by numerical modelling and good agreement is reached

A novel methodology to determine the mechanical properties of amorphous materials through instrumented nanoindentation

A novel methodology based on instrumented indentation was developed to characterize the mechanical properties of amorphous materials. The approach is based on the concept of a universal postulate that assumes the existence of a characteristic indentation pressure proportional to the hardness. This hypothesis was numerically validated. This method overcomes the limitation of the conventional indentation models (pile-up effects and pressure sensitivity materials).

Cohesive-frictional modelling of bond and splitting action of prestressing wire

This work shows a numerical procedure for bond between indented wires and concrete, and the coupled splitting of the concrete. The bond model is an interface, non-associative, plasticity model. It is coupled with a cohesive fracture model for concrete to take into account the splitting of such concrete. The radial component of the prestressing force, increased by Poisson’s effect, may split the surrounding concrete, decreasing the wire confinement and diminishing the bonding. The combined action of the bond and the splitting is studied with the proposed model. The results of the numerical model are compared with the results of a series of tests, such as those which showed splitting induced by the bond between wire and concrete. Tests with different steel indentation depths were performed. The numerical procedure accurately reproduces the experimental records and improves knowledge of this complex process.

An analytical model for simulating the bond of prestressed concrete during the prestressed force release

A bond analytical model is proposed in this paper. The model is capable of reproducing the bond stress developed between the steel and concrete, in precast prestressed elements, during the entire process of prestressing force release. The bond stress developed in the transmission zone, where the bond stress is not constant, is also obtained. The steel and concrete stresses as well as the slip between both materials can be also estimated by means of the relation established in the model between these parameters and the bond stress. The model is validated with the results of a series of tests, considering different steel indentation depths and concrete covers and it is extended to evaluate the transmission length. This has been checked by comparing the transmission length predicted by the model and one measured experimentally in two series of tests.

An analytical model for simulating the bond of prestressed concrete during the prestressed force release

A bond analytical model is proposed in this paper. The model is capable of reproducing the bond stress developed between the steel and concrete, in precast prestressed elements, during the entire process of prestressing force release. The bond stress developed in the transmission zone, where the bond stress is not constant, is also obtained. The steel and concrete stresses as well as the slip between both materials can be also estimated by means of the relation established in the model between these parameters and the bond stress. The model is validated with the results of a series of tests, considering different steel indentation depths and concrete covers and it is extended to evaluate the transmission length. This has been checked by comparing the transmission length predicted by the model and one measured experimentally in two series of tests.

Mechanical properties up to 1900 K of Al2O3/Er3Al5O12/ZrO2 eutectic ceramics grown by the laser floating zone method

Directionally solidified Al2O3–Er3Al5O12–ZrO2 eutectic rods were processed using the laser floating zone method at growth rates of 25, 350and 750 mm/h to obtain microstructures with different domain size. The mechanical properties were investigated as a function of the processing rate. The hardness, 15.6 GPa, and the fracture toughness, 4 MPa m1/2, obtained from Vickers indentation at room temperature were practically independent of the size of the eutectic phases. However, the flexural strength increased as the domain size decreased, reaching outstanding strength values close to 3 GPa in the samples grown at 750 mm/h. A high retention of the flexural strength was observed up to 1500 K in the materials processed at 25 and 350 mm/h, while superplastic behaviour was observed at 1700 K in the eutectic rods solidified at the highest rate of 750 mm/h

Caracterización geométrica de huellas de dureza Brinell mediante equipos ópticos. Modelo con microscopía confocal

En esta tesis se desarrolla una metodología alternativa para la determinación de la dureza Brinell a partir de imágenes obtenidas mediante microscopía confocal, que se ha mostrado robusta para mejorar los resultados de medición del diámetro en condiciones de reproducibilidad. Las validaciones realizadas evidencian su posibilidad real de implementación, especialmente para la certificación de patrones de dureza. Los estudios experimentales realizados ponen de manifiesto que la medición del diámetro de una huella de dureza Brinell, siguiendo la metodología tradicional, depende de la posición del patrón, de las características del equipo empleado y del propio operador. Dicha medida resulta crítica y las dificultades para identificar el borde de la huella incorporan a menudo una fuente adicional de incertidumbre difícil de soslayar. En esta investigación se han desarrollado dos modelos matemáticos que permiten identificar de forma unívoca el diámetro de la huella en el punto donde se produce el límite de contacto entre el indentador y el material de la probeta durante la realización del ensayo. Ambos modelos han sido implementados en Matlab® y se ha verificado su validez mediante datos sintéticos. Asimismo, se ha realizado una validación experimental sobre patrones de dureza certificados, empleando un microscopio confocal marca Leica, modelo DCM 3D disponible en el Laboratorio de Investigación de Materiales de Interés Tecnológico (LIMIT) de la Escuela Técnica Superior de Ingeniería y Diseño Industrial de la Universidad Politécnica de Madrid (ETSIDI – UPM). Dicha validación ha puesto de manifiesto la utilidad de esta nueva metodología por cuanto permite caracterizar las huellas, estimar las incertidumbres de medida y garantizar la trazabilidad metrológica de los resultados. ABSTRACT This PhD thesis presents an alternative methodology to determine the Brinell hardness from the images obtained by confocal microscopy that has proved to be robust to improve the results of indentation diameter measurements in reproducibility conditions. The validations carried out show the real possibility of its implementation, especially for calibration of hardness reference blocks. Experimental studies performed worldwide show that the measurement of the indentation diameter in a Brinell hardness test depends, when the traditional methodology is applied, on the position of the test block, the equipment characteristics and the operator. This measurement is critical and the difficulties to identify the edge of the indentation often bring an additional source of uncertainty with them that is hard to avoid. In this research two specific mathematical models have been developed to identify unambiguously the indentation diameter at the point where the edge of the boundary between the indenter and the test block is found during the test. Both models have been implemented on Matlab® and their validity has been verified by synthetic data An additional experimental validation with calibrated hardness reference blocks has been carried out using a Leica-brand confocal microscope, model DCM 3D, available in the Laboratory for Research on Materials of Technological Interest (LIMIT in its Spanish acronym) of the Escuela Técnica Superior de Ingeniería y Diseño Industrial de la Universidad Politécnica de Madrid (ETSIDI-UPM). This validation has shown the utility of this new methodology since it allows to characterize the indentation, to estimate the measurement uncertainties and to ensure the metrological traceability of the results.

Physically-sound simulation of low-velocity impact on fiber reinforced laminates

A high-fidelity virtual tool for the numerical simulation of low-velocity impact damage in unidirectional composite laminates is proposed. A continuum material model for the simulation of intraply damage phenomena is implemented in a numerical scheme as a user subroutine of the commercially available Abaqus finite element package. Delaminations are simulated using of cohesive surfaces. The use of structured meshes, aligned with fiber directions allows the physically-sound simulation of matrix cracks parallel to fiber directions, and their interaction with the development of delaminations. The implementation of element erosion criteria and the application of intraply and interlaminar friction allow for the simulation of fiber splits and their entanglement, which in turn results in permanent indentation in the impacted laminate. It is shown that this simulation strategy gives sound results for impact energies bellow and above the Barely Visible Impact Damage threshold, up to laminate perforation conditions

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