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.

The study of multi-phase diffusion in three-component metallic systems

"This report was prepared by University of Florida, Gainesville, Florida, under USAF Contract no. F 33615-67-C-1227."

Polyethylene multiwalled carbon nanotube composites

Polyethylene (PE) multiwalled carbon nanotubes (MWCNTs) with weight fractions ranging from 0.1 to 10 wt% were prepared by melt blending using a mini-twin screw extruder. The morphology and degree of dispersion of the MWCNTs in the PE matrix at different length scales was investigated using scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM) and wide-angle X-ray diffraction (WAXD). Both individual and agglomerations of MWCNTs were evident. An up-shift of 17 cm(-1) for the G band and the evolution of a shoulder to this peak were obtained in the Raman spectra of the nanocomposites, probably due to compressive forces exerted on the MWCNTs by PE chains and indicating intercalation of PE into the MWCNT bundles. The electrical conductivity and linear viscoelastic behaviour of these nanocomposites were investigated. A percolation threshold of about 7.5 wt% was obtained and the electrical conductivity of PE was increased significantly, by 16 orders of magnitude, from 10(-20) to 10(-4) S/cm. The storage modulus (G') versus frequency curves approached a plateau above the percolation threshold with the formation of an interconnected nanotube structure, indicative of 'pseudo-solid-like' behaviour. The ultimate tensile strength and elongation at break of the nanocomposites decreased with addition of MWCNTs. The diminution of mechanical proper-ties of the nanocomposites, though concomitant with a significant increase in electrical conductivity, implies the mechanism for mechanical reinforcement for PE/MWCNT composites is filler-matrix interfacial interactions and not filler percolation. The temperature of crystallisation (T.) and fraction of PE that was crystalline (F-c) were modified by incorporating MWCNTs. The thermal decomposition temperature of PE was enhanced by 20 K on addition of 10 wt% MWCNT. (c) 2005 Elsevier Ltd. All rights reserved.

Role of reinforcement/matrix interfacial strength in fatigue crack propagation in particulate SiC reinforced aluminum alloy 8090

A study has been made of the influence of the reinforcement/matrix interfacial strength on fatigue crack propagation in a powder metallurgy aluminum alloy 8090-SiC particulate composite. The interfacial region has been altered by two separate routes, the first involving aging of the 8090 matrix, with the subsequent formation of precipitate free zones at the boundaries, and the second consisting of oxidizing the surface of the SiC particles before their incorporation into the composite. In the naturally aged condition, oxidation of the SiC leads to a reduction in fatigue crack growth resistance at higher values of stress intensity range ΔK. This is due to a proportion of the crack growth occurring through voids formed in association with many of the weak SiC interfaces which have retained a layer of thick surface oxide after processing. On overaging no difference in crack growth rate is discernible between the oxidized and unoxidized SiC composites. It is proposed that this is due to similar levels of interfacial weakening having occurred in both composites, indicating that this is an important factor in the reduction of the high ΔK crack growth resistance of the unoxidized SiC composite on aging.

Fatigue in SiC-particulate-reinforced aluminium alloy composites

The fatigue behaviour in SiC-particulate-reinforced aluminium alloy composites has been briefly reviewed. The improved fatigue life reported in stress-controlled test results from the higher stiffness of the composites; therefore it is generally inferior to monolithic alloys at a constant strain level. The role of SiC particulate reinforcement has been examined for fatigue crack initiation, short-crack growth and long-crack growth. Crack initiation is observed to occur at matrix-SiC interface in cast composites and either at or near the matrix-SiC interface or at cracked SiC particles in powder metallurgy processed composites depending on particle size and morphology. The da/dN vs ΔK relationship in the composites is characterized by crack growth rates existing within a narrow range of ΔK and this is because of the lower fracture toughness and relatively high threshold values in composites compared with those in monolithic alloys. An enhanced Paris region slope attributed to the monotonic fracture contribution are reported and the extent of this contribution is found to depend on particle size. The effects of the aging condition on crack growth rates and particle size dependence of threshold values are also treated in this paper. © 1991.

Fatigue in metallic alloys containing non-metallic particles

This paper examines the effects of non-metallic particles on fatigue performance and, in particular, their influence on fatigue crack propagation at high ΔK (Kmax) levels. The nature and properties of a number of common non-metallic particles found in Fe- and Al- based alloys are described, and consideration is given to the consequences of mismatch of physical and chemical properties between particle and matrix. Effects of particles on fatigue in conventional alloys are illustrated and compared with the behaviour of Al/SiCp MMC. The problems associated with developing particulate reinforced MMC with adequate fatigue crack growth resistance and toughness for structural applications are discussed. © 1991.

Hydroxyapatite-nanotube composites and coatings for orthopedic applications

Hydroxyapatite (HA) has received wide attention in orthopedics, due to its biocompatibility and osseointegration ability. Despite these advantages, the brittle nature and low fracture toughness of HA often results in rapid wear and premature fracture of implant. Hence, there is a need to improve the fracture toughness and wear resistance of HA without compromising its biocompatibility. ^ The aim of the current research is to explore the potential of nanotubes as reinforcement to HA for orthopedic implants. HA- 4 wt.% carbon nanotube (CNT) composites and coatings are synthesized by spark plasma sintering and plasma spraying respectively, and investigated for their mechanical, tribological and biological behavior. CNT reinforcement improves the fracture toughness (>90%) and wear resistance (>66%) of HA for coating and free standing composites. CNTs have demonstrated a positive influence on the proliferation, differentiation and matrix mineralization activities of osteoblasts, during in-vitro biocompatibility studies. In-vivo exposure of HA-CNT coated titanium implant in animal model (rat) shows excellent histocompatibility and neobone integration on the implant surface. The improved osseointegration due to presence of CNTs in HA is quantified by the adhesion strength measurement of single osteoblast using nano-scratch technique. ^ Considering the ongoing debate about cytotoxicity of CNTs in the literature, the present study also suggests boron nitride nanotube (BNNT) as an alternative reinforcement. BNNT with the similar elastic modulus and strength as CNT, were added to HA. The resulting composite having 4 wt.% BNNTs improved the fracture toughness (∼85%) and wear resistance (∼75%) of HA in the similar range as HA-CNT composites. BNNTs were found to be non-cytotoxic for osteoblasts and macrophages. In-vitro evaluation shows positive role of BNNT in osteoblast proliferation and viability. Apatite formability of BNNT surface in ∼4 days establishes its osseointegration ability.^

Projected equations of motion approach to hybrid quantum/classical dynamics in dielectric-metal composites

We introduce a hybrid method for dielectric-metal composites that describes the dynamics of the metallic system classically whilst retaining a quantum description of the dielectric. The time-dependent dipole moment of the classical system is mimicked by the introduction of projected equations of motion (PEOM) and the coupling between the two systems is achieved through an effective dipole-dipole interaction. To benchmark this method, we model a test system (semiconducting quantum dot-metal nanoparticle hybrid). We begin by examining the energy absorption rate, showing agreement between the PEOM method and the analytical rotating wave approximation (RWA) solution. We then investigate population inversion and show that the PEOM method provides an accurate model for the interaction under ultrashort pulse excitation where the traditional RWA breaks down.

Modelling the crush behaviour of thermoplastic composites

Thermoplastic composites are likely to emerge as the preferred solution for meeting the high-volume production demands of passenger road vehicles. Substantial effort is currently being directed towards the development of new modelling techniques to reduce the extent of costly and time consuming physical testing. Developing a high-fidelity numerical model to predict the crush behaviour of composite laminates is dependent on the accurate measurement of material properties as well as a thorough understanding of damage mechanisms associated with crush events. This paper details the manufacture, testing and modelling of self-supporting corrugated-shaped thermoplastic composite specimens for crashworthiness assessment. These specimens demonstrated a 57.3% higher specific energy absorption compared to identical specimen made from thermoset composites. The corresponding damage mechanisms were investigated in-situ using digital microscopy and post analysed using Scanning Electron Microscopy (SEM). Splaying and fragmentation modes were the 2 primary failure modes involving fibre breakage, matrix cracking and delamination. A mesoscale composite damage model, with new non-linear shear constitutive laws, which combines a range of novel techniques to accurately capture the material response under crushing, is presented. The force-displacement curves, damage parameter maps and dissipated energy, obtained from the numerical analysis, are shown to be in a good qualitative and quantitative agreement with experimental results. The proposed approach could significantly reduce the extent of physical testing required in the development of crashworthy structures.  

Development of functionalised multiwalled carbon nanotube/polyaniline composites for electrical applications

Combining intrinsically conducting polymers with carbon nanotubes (CNT) helps in creating composites with superior electrical and thermal characteristics. These composites are capable of replacing metals and semiconductors as they possess unique combination of electrical conductivity, flexibility, stretchability, softness and bio-compatibility. Their potential for use in various organic devices such as super capacitors, printable conductors, optoelectronic devices, sensors, actuators, electrochemical devices, electromagnetic interference shielding, field effect transistors, LEDs, thermoelectrics etc. makes them excellent substitutes for present day semiconductors.However, many of these potential applications have not been fully exploited because of various open–ended challenges. Composites meant for use in organic devices require highly stable conductivity for the longevity of the devices. CNT when incorporated at specific proportions, and with special methods contributes quite positively to this end.The increasing demand for energy and depleting fossil fuel reserves has broadened the scope for research into alternative energy sources. A unique and efficient method for harnessing energy is thermoelectric energy conversion method. Here, heat is converted directly into electricity using a class of materials known as thermoelectric materials. Though polymers have low electrical conductivity and thermo power, their low thermal conductivity favours use as a thermoelectric material. The thermally disconnected, but electrically connected carrier pathways in CNT/Polymer composites can satisfy the so-called “phonon-glass/electron-crystal” property required for thermoelectric materials. Strain sensing is commonly used for monitoring in engineering, medicine, space or ocean research. Polymeric composites are ideal candidates for the manufacture of strain sensors. Conducting elastomeric composites containing CNT are widely used for this application. These CNT/Polymer composites offer resistance change over a large strain range due to the low Young‟s modulus and higher elasticity. They are also capable of covering surfaces with arbitrary curvatures.Due to the high operating frequency and bandwidth of electronic equipments electromagnetic interference (EMI) has attained the tag of an „environmental pollutant‟, affecting other electronic devices as well as living organisms. Among the EMI shielding materials, polymer composites based on carbon nanotubes show great promise. High strength and stiffness, extremely high aspect ratio, and good electrical conductivity of CNT make it a filler of choice for shielding applications. A method for better dispersion, orientation and connectivity of the CNT in polymer matrix is required to enhance conductivity and EMI shielding. This thesis presents a detailed study on the synthesis of functionalised multiwalled carbon nanotube/polyaniline composites and their application in electronic devices. The major areas focused include DC conductivity retention at high temperature, thermoelectric, strain sensing and electromagnetic interference shielding properties, thermogravimetric, dynamic mechanical and tensile analysis in addition to structural and morphological studies.

Fabrication, Optical Analysis and Photonic Applications of Certain Metallic Nanostructure-Integrated Dye Doped Polymer Optical Fibers” submitted by Ms. Suneetha Sebastian

Polymer Optical Fibers have occupied historically a place for large core flexible fibers operating in short distances. In addition to their practical passive application in short-haul communication they constitute a potential research field as active devices with organic dopants. Organic dyes are preferred as dopants over organic semiconductors due to their higher optical cross section. Thus organic dyes as gain media in a polymer fiber is used to develop efficient and narrow laser sources with a tunability throughout the visible region or optical amplifier with high gain. Dyes incorporated in fiber form has added advantage over other solid state forms such as films since the pump power required to excite the molecules in the core of the fiber is less thereby utilising the pump power effectively. In 1987, Muto et.al investigated a dye doped step index polymer fiber laser. Afterwards, numerous researches have been carried out in this area demonstrating laser emission from step index, graded index and hollow optical fibers incorporating various dyes. Among various dyes, Rhodamine6G is the most widely and commonly used laser dye for the last four decades. Rhodamine6G has many desirable optical properties which make it preferable over other organic dyes such as Coumarin, Nile Blue, Curcumin etc. The research focus on the implementation of efficient fiber lasers and amplifiers for short fiber distances. Developing efficient plastic lasers with electrical pumping can be a new proposal in this field which demands lowest possible threshold pump energy of the gain medium in the cavity as an important parameter. One way of improving the efficiency of the lasers, through low threshold pump energy, is by modifying the gain of the amplifiers in the resonator/cavity. Success in the field of Radiative Decay Engineering can pave way to this problem. Laser gain media consisting of dye-nanoparticle composites can improve the efficiency by lowering the lasing threshold and enhancing the photostability. The electric field confined near the surface of metal nanoparticles due to Localized Surface Plasmon Resonance can be very effective for the excitation of active centers to impart high optical gain for lasing. Since the Surface Plasmon Resonance of nanoparticles of gold and silver lies in the visible range, it can affect the spectral emission characteristics of organic dyes such as Rhodamine6G through plasmon field generated by the particles. The change in emission of the dye placed near metal nanoparticles depend on plasmon field strength which in turn depends on the type of metal, size of nanoparticle, surface modification of the particle and the wavelength of incident light. Progress in fabrication of different types of nanostructures lead to the advent of nanospheres, nanoalloys, core-shell and nanowires to name a few. The thesis deals with the fabrication and characterisation of polymer optical fibers with various metallic and bimetallic nanostructures incorporated in the gain media for efficient fiber lasers with low threshold and improved photostability.

POLYMER-NANOPARTICLE COMPOSITES FOR APPLICATIONS IN FLEXIBLE ELECTRONICS

The aim of this dissertation was to investigate flexible polymer-nanoparticle composites with unique magnetic and electrical properties. Toward this goal, two distinct projects were carried out. The first project explored the magneto-dielectric properties and morphology of flexible polymer-nanoparticle composites that possess high permeability (µ), high permittivity (ε) and minimal dielectric, and magnetic loss (tan δε, tan δµ). The main materials challenges were the synthesis of magnetic nanoparticle fillers displaying high saturation magnetization (Ms), limited coercivity, and their homogeneous dispersion in a polymeric matrix. Nanostructured magnetic fillers including polycrystalline iron core-shell nanoparticles, and constructively assembled superparamagnetic iron oxide nanoparticles were synthesized, and dispersed uniformly in an elastomer matrix to minimize conductive losses. The resulting composites have demonstrated promising permittivity (22.3), permeability (3), and sustained low dielectric (0.1), magnetic (0.4) loss for frequencies below 2 GHz. This study demonstrated nanocomposites with tunable magnetic resonance frequency, which can be used to develop compact and flexible radio frequency devices with high efficiency. The second project focused on fundamental research regarding methods for the design of highly conductive polymer-nanoparticle composites that can maintain high electrical conductivity under tensile strain exceeding 100%. We investigated a simple solution spraying method to fabricate stretchable conductors based on elastomeric block copolymer fibers and silver nanoparticles. Silver nanoparticles were assembled both in and around block copolymer fibers forming interconnected dual nanoparticle networks, resulting in both in-fiber conductive pathways and additional conductive pathways on the outer surface of the fibers. Stretchable composites with conductivity values reaching 9000 S/cm maintained 56% of their initial conductivity after 500 cycles at 100% strain. The developed manufacturing method in this research could pave the way towards direct deposition of flexible electronic devices on any shaped substrate. The electrical and electromechanical properties of these dual silver nanoparticle network composites make them promising materials for the future construction of stretchable circuitry for displays, solar cells, antennas, and strain and tactility sensors.

Experimental Modeling of Twin-Screw Extrusion Processes to Predict Properties of Extruded Composites

Twin-screw extrusion is used to compound fillers into a polymer matrix in order to improve the properties of the final product. The resultant properties of the composite are determined by the operating conditions used during extrusion processing. Changes in the operating conditions affect the physics of the melt flow, inducing unique composite properties. In the following work, the Residence Stress Distribution methodology has been applied to model both the stress behavior and the property response of a twin-screw compounding process as a function of the operating conditions. The compounding of a pigment into a polymer melt has been investigated to determine the effect of stress on the degree of mixing, which will affect the properties of the composite. In addition, the pharmaceutical properties resulting from the compounding of an active pharmaceutical ingredient are modeled as a function of the operating conditions, indicating the physical behavior inducing the property responses.

MOLECULAR MODELING OF EPON 862-DETDA / CARBON COMPOSITES

The thermoset epoxy resin EPON 862, coupled with the DETDA hardening agent, are utilized as the polymer matrix component in many graphite (carbon fiber) composites. Because it is difficult to experimentally characterize the interfacial region, computational molecular modeling is a necessary tool for understanding the influence of the interfacial molecular structure on bulk-level material properties. The purpose of this research is to investigate the many possible variables that may influence the interfacial structure and the effect they will have on the mechanical behavior of the bulk level composite. Molecular models are established for EPON 862-DETDA polymer in the presence of a graphite surface. Material characteristics such as polymer mass-density, residual stresses, and molecular potential energy are investigated near the polymer/fiber interface. Because the exact degree of crosslinking in these thermoset systems is not known, many different crosslink densities (degrees of curing) are investigated. It is determined that a region exists near the carbon fiber surface in which the polymer mass density is different than that of the bulk mass density. These surface effects extend ~10 Å into the polymer from the center of the outermost graphite layer. Early simulations predict polymer residual stress levels to be higher near the graphite surface. It is also seen that the molecular potential energy in polymer atoms decreases with increasing crosslink density. New models are then established in order to investigate the interface between EPON 862-DETDA polymer and graphene nanoplatelets (GNPs) of various atomic thicknesses. Mechanical properties are extracted from the models using Molecular Dynamics techniques. These properties are then implemented into micromechanics software that utilizes the generalized method of cells to create representations of macro-scale composites. Micromechanics models are created representing GNP doped epoxy with varying number of graphene layers and interfacial polymer crosslink densities. The initial micromechanics results for the GNP doped epoxy are then taken to represent the matrix component and are re-run through the micromechanics software with the addition of a carbon fiber to simulate a GNP doped epoxy/carbon fiber composite. Micromechanics results agree well with experimental data, and indicate GNPs of 1 to 2 atomic layers to be highly favorable. The effect of oxygen bonded to the surface of the GNPs is lastly investigated. Molecular Models are created for systems with varying graphene atomic thickness, along with different amounts of oxygen species attached to them. Models are created for graphene containing hydroxyl groups only, epoxide groups only, and a combination of epoxide and hydroxyl groups. Results show models of oxidized graphene to decrease in both tensile and shear modulus. Attaching only epoxide groups gives the best results for mechanical properties, though pristine graphene is still favored.

MULTISCALE MODELING OF LIQUID CRYSTALLINE/NANOTUBE COMPOSITES

The objective of this research is to synthesize structural composites designed with particular areas defined with custom modulus, strength and toughness values in order to improve the overall mechanical behavior of the composite. Such composites are defined and referred to as 3D-designer composites. These composites will be formed from liquid crystalline polymers and carbon nanotubes. The fabrication process is a variation of rapid prototyping process, which is a layered, additive-manufacturing approach. Composites formed using this process can be custom designed by apt modeling methods for superior performance in advanced applications. The focus of this research is on enhancement of Young's modulus in order to make the final composite stiffer. Strength and toughness of the final composite with respect to various applications is also discussed. We have taken into consideration the mechanical properties of final composite at different fiber volume content as well as at different orientations and lengths of the fibers. The orientation of the LC monomers is supposed to be carried out using electric or magnetic fields. A computer program is modeled incorporating the Mori-Tanaka modeling scheme to generate the stiffness matrix of the final composite. The final properties are then deduced from the stiffness matrix using composite micromechanics. Eshelby's tensor, required to calculate the stiffness tensor using Mori-Tanaka method, is calculated using a numerical scheme that determines the components of the Eshelby's tensor (Gavazzi and Lagoudas 1990). The numerical integration is solved using Gaussian Quadrature scheme and is worked out using MATLAB as well. . MATLAB provides a good deal of commands and algorithms that can be used efficiently to elaborate the continuum of the formula to its extents. Graphs are plotted using different combinations of results and parameters involved in finding these results