Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 34

Search results for: nanoindentation

34 Identification of the Orthotropic Parameters of Cortical Bone under Nanoindentation

Authors: D. Remache, M. Semaan, C. Baron, M. Pithioux, P. Chabrand, J. M. Rossi, J. L. Milan


A good understanding of the mechanical properties of the bone implies a better understanding of its various diseases, such as osteoporosis. Berkovich nanoindentation tests were performed on the human cortical bone to extract its orthotropic parameters. The nanoindentation experiments were then simulated by the finite element method. Different configurations of interactions between the tip indenter and the bone were simulated. The orthotropic parameters of the material were identified by the inverse method for each configuration. The friction effect on the bone mechanical properties was then discussed. It was found that the inverse method using the finite element method is a very efficient method to predict the mechanical behavior of the bone.

Keywords: mechanical behavior of bone, nanoindentation, finite element analysis, inverse optimization approaches

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33 Stress-Strain Relation for Human Trabecular Bone Based on Nanoindentation Measurements

Authors: Marek Pawlikowski, Krzysztof Jankowski, Konstanty Skalski, Anna Makuch


Nanoindentation or depth-sensing indentation (DSI) technique has proven to be very useful to measure mechanical properties of various tissues at a micro-scale. Bone tissue, both trabecular and cortical one, is one of the most commonly tested tissues by means of DSI. Most often such tests on bone samples are carried out to compare the mechanical properties of lamellar and interlamellar bone, osteonal bone as well as compact and cancellous bone. In the paper, a relation between stress and strain for human trabecular bone is presented. The relation is based on the results of nanoindentation tests. The formulation of a constitutive model for human trabecular bone is based on nanoindentation tests. In the study, the approach proposed by Olivier-Pharr is adapted. The tests were carried out on samples of trabecular tissue extracted from human femoral heads. The heads were harvested during surgeries of artificial hip joint implantation. Before samples preparation, the heads were kept in 95% alcohol in temperature 4 Celsius degrees. The cubic samples cut out of the heads were stored in the same conditions. The dimensions of the specimens were 25 mm x 25 mm x 20 mm. The number of 20 samples have been tested. The age range of donors was between 56 and 83 years old. The tests were conducted with the indenter spherical tip of the diameter 0.200 mm. The maximum load was P = 500 mN and the loading rate 500 mN/min. The data obtained from the DSI tests allows one only to determine bone behoviour in terms of nanoindentation force vs. nanoindentation depth. However, it is more interesting and useful to know the characteristics of trabecular bone in the stress-strain domain. This allows one to simulate trabecular bone behaviour in a more realistic way. The stress-strain curves obtained in the study show relation between the age and the mechanical behaviour of trabecular bone. It was also observed that the bone matrix of trabecular tissue indicates an ability of energy absorption.

Keywords: constitutive model, mechanical behaviour, nanoindentation, trabecular bone

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32 Neutron Irradiated Austenitic Stainless Steels: An Applied Methodology for Nanoindentation and Transmission Electron Microscopy Studies

Authors: P. Bublíkova, P. Halodova, H. K. Namburi, J. Stodolna, J. Duchon, O. Libera


Neutron radiation-induced microstructural changes cause degradation of mechanical properties and the lifetime reduction of reactor internals during nuclear power plant operation. Investigating the effects of neutron irradiation on mechanical properties of the irradiated material (hardening, embrittlement) is challenging and time-consuming. Although the fast neutron spectrum has the major influence on microstructural properties, the thermal neutron effect is widely investigated owing to Irradiation-Assisted Stress Corrosion Cracking firstly observed in BWR stainless steels. In this study, 300-series austenitic stainless steels used as material for NPP's internals were examined after neutron irradiation at ~ 15 dpa. Although several nanoindentation experimental publications are available to determine the mechanical properties of ion irradiated materials, less is available on neutron irradiated materials at high dpa tested in hot-cells. In this work, we present particular methodology developed to determine the mechanical properties of neutron irradiated steels by nanoindentation technique. Furthermore, radiation-induced damage in the specimens was investigated by High Resolution - Transmission Electron Microscopy (HR-TEM) that showed the defect features, particularly Frank loops, cavity microstructure, radiation-induced precipitates and radiation-induced segregation. The results of nanoindentation measurements and associated nanoscale defect features showed the effect of irradiation-induced hardening. We also propose methodologies to optimized sample preparation for nanoindentation and microscotructural studies.

Keywords: nanoindentation, thermal neutrons, radiation hardening, transmission electron microscopy

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31 Mechanical Cortical Bone Characterization with the Finite Element Method Based Inverse Method

Authors: Djamel Remache, Marie Semaan, Cécile Baron, Martine Pithioux, Patrick Chabrand, Jean-Marie Rossi, Jean-Louis Milan


Cortical bone is a complex multi-scale structure. Even though several works have contributed significantly to understanding its mechanical behavior, this behavior remains poorly understood. Nanoindentation testing is one of the primary testing techniques for the mechanical characterization of bone at small scales. The purpose of this study was to provide new nanoindentation data of cortical bovine bone in different directions and at different bone microstructures (osteonal, interstitial and laminar bone), and then to identify anisotropic properties of samples with FEM (finite element method) based inverse method. Experimentally and numerical results were compared. Experimental and numerical results were compared. The results compared were in good agreement.

Keywords: mechanical behavior of bone, nanoindentation, finite element analysis, inverse optimization approach

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30 Effect of Annealing Temperature on Microstructural Evolution of Nanoindented Cu/Si Thin Films

Authors: Woei-Shyan Lee, Yu-Liang Chuang


The nano-mechanical properties of as-deposited Cu/Si thin films indented to a depth of 2000 nm are investigated using a nanoindentation technique. The nanoindented specimens are annealed at a temperature of either 160 °C or 210°C, respectively. The microstructures of the as-deposited and annealed samples are then examined via transmission electron microscopy (TEM). The results show that both the loading and the unloading regions of the load-displacement curve are smooth and continuous, which suggests that no debonding or cracking occurs during nanoindentation. In addition, the hardness and Young’s modulus of the Cu/Si thin films are found to vary with the nanoindentation depth, and have maximum values of 2.8 GPa and 143 GPa, respectively, at the maximum indentation depth of 2000 nm. The TEM observations show that the region of the Cu/Si film beneath the indenter undergoes a phase transformation during the indentation process. In the case of the as-deposited specimens, the indentation pressure induces a completely amorphous phase within the indentation zone. For the specimens annealed at a temperature of 160°C, the amorphous nature of the microstructure within the indented zone is maintained. However, for the specimens annealed at a higher temperature of 210°C, the indentation affected zone consists of a mixture of amorphous phase and nanocrystalline phase. Copper silicide (η-Cu3Si) precipitates are observed in all of the annealed specimens. The density of the η-Cu3Si precipitates is found to increase with an increasing annealing temperature.

Keywords: nanoindentation, Cu/Si thin films, microstructural evolution, annealing temperature

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29 Nanoindentation Behaviour and Microstructural Evolution of Annealed Single-Crystal Silicon

Authors: Woei-Shyan Lee, Shuo-Ling Chang


The nanoindentation behaviour and phase transformation of annealed single-crystal silicon wafers are examined. The silicon specimens are annealed at temperatures of 250, 350 and 450ºC, respectively, for 15 minutes and are then indented to maximum loads of 30, 50 and 70 mN. The phase changes induced in the indented specimens are observed using transmission electron microscopy (TEM) and micro-Raman scattering spectroscopy (RSS). For all annealing temperatures, an elbow feature is observed in the unloading curve following indentation to a maximum load of 30 mN. Under higher loads of 50 mN and 70 mN, respectively, the elbow feature is replaced by a pop-out event. The elbow feature reveals a complete amorphous phase transformation within the indented zone, whereas the pop-out event indicates the formation of Si XII and Si III phases. The experimental results show that the formation of these crystalline silicon phases increases with an increasing annealing temperature and indentation load. The hardness and Young’s modulus both decrease as the annealing temperature and indentation load are increased.

Keywords: nanoindentation, silicon, phase transformation, amorphous, annealing

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28 A Nanoindentation Study of Thin Film Prepared by Physical Vapor Deposition

Authors: Dhiflaoui Hafedh, Khlifi Kaouther, Ben Cheikh Larbi Ahmed


Monolayer and multilayer coatings of CrN and AlCrN deposited on 100Cr6 (AISI 52100) substrate by PVD magnetron sputtering system. The micro structures of the coatings were characterized using atomic force microscopy (AFM). The AFM analysis revealed the presence of domes and craters which are uniformly distributed over all surfaces of the various layers. Nano indentation measurement of CrN coating showed maximum hardness (H) and modulus (E) of 14 GPa and 240 GPa, respectively. The measured H and E values of AlCrN coatings were found to be 30 GPa and 382 GPa, respectively. The improved hardness in both the coatings was attributed mainly to a reduction in crystallite size and decrease in surface roughness. The incorporation of Al into the CrN coatings has improved both hardness and Young’s modulus.

Keywords: CrN, AlCrN coatings, hardness, nanoindentation

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27 Nanoindentation Studies of Metallic Cu-CuZr Composites Synthesized by Accumulative Roll Bonding

Authors: Ehsan Alishahi, Chuang Deng


Materials with microstructural heterogeneity have recently attracted dramatic attention in the materials science community. Although most of the metals are identified as crystalline, the new class of amorphous alloys, sometimes are known as metallic glasses (MGs), exhibited remarkable properties, particularly high mechanical strength and elastic limit. The unique properties of MGs led to the wide range of studies in developing and characterizing of new alloys or composites which met the commercial desires. In spite of applicable properties of MGs, commercializing of metallic glasses was limited due to a major drawback, the lack of ductility and sudden brittle failure mode. Hence, crystalline-amorphous (C-A) composites were introduced almost in 2000s as a toughening strategy to improve the ductility of MGs. Despite the considerable progress reported in previous studies, there are still challenges in both synthesis and characterization of metallic C-A composites. In this study, accumulative roll bonding (ARB) was used to synthesize bulk crystalline-amorphous composites starting from crystalline Cu-Zr multilayers. Due to the severe plastic deformation state, new CuZr phases were formed during the rolling process which was reflected in SEM-EDS analysis. EDS elemental analysis showed the variation in the composition of CuZr phases such as 38-62, 50-50 to 68-32 at Cu-Zr % respectively. Moreover, TEM with electron diffraction analysis indicated the presence of both crystalline and amorphous structures for the new formed CuZr phases. In addition to the microstructural analysis, the mechanical properties of the synthesized composites were studied using the nanoindentation technique. Hysitron Nanoindentation instrument was used to conduct nanoindentation tests with cube corner tip. The maximum load of 5000 µN was applied in load control mode to measure the elastic modulus and hardness of different phases. The trend of results indicated three distinct regimes of hardness and elastic modulus including pure Cu, pure Zr, and new formed CuZr phases. More specifically, pure Cu regions showed the lowest values for both nanoindentation hardness and elastic modulus while the CuZr phases take the highest values. Consequently, pure Zr was placed in the intermediate range which is harder than pure Cu but softer than CuZr phases. In overall, it was found that CuZr phases with higher hardness were nucleated during ARB process as a result of mechanical alloying phenomenon.

Keywords: ARB, crystalline-amorphous composites, mechanical alloying, nanoindentation hardness

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26 Microstructural Mechanical Properties of Human Trabecular Bone Based on Nanoindentation Test

Authors: K. Jankowski, M. Pawlikowski, A. Makuch, K. Skalski


Depth-sensing indentation (DSI) or nanoindentation is becoming a more and more popular method of measuring mechanical properties of various materials and tissues at a micro-scale. This technique allows measurements without complicated sample preparation procedures which makes this method very useful. As a result of measurement force and displacement of the intender are obtained. It is also possible to determine three measures of hardness i.e. Martens hardness (HM), nanohardness (HIT), Vickers hardness (HV) and Young modulus EIT. In this work trabecular bone mechanical properties were investigated. The bone samples were harvested from human femoral heads during hip replacement surgery. Patients were of different age, sexes and stages of tissue degeneration caused by osteoarthritis. The specimens were divided into three groups. Each group contained samples harvested from patients of different range of age. All samples were investigated with the same measurement conditions. The maximum load was Pmax=500 mN and the loading rate was 500 mN/min. The tests were held without hold at the peak force. The tests were conducted with indenter Vickers tip and spherical tip of the diameter 0.2 mm. Each trabecular bone sample was tested 7 times in a close area of the same trabecula. The measured loading P as a function of indentation depth allowed to obtain hysteresis loop and HM, HIT, HV, EIT. Results for arbitrarily chosen sample are HM=289.95 ± 42.31 MPa, HIT=430.75 ± 45.37 MPa, HV=40.66 ± 4.28 Vickers, EIT=7.37 ± 1.84 GPa for Vickers tip and HM=115.19 ± 15.03 MPa, HIT=165.80 ± 19.30 MPa, HV=16.90 ± 1.97 Vickers, EIT=5.30 ± 1.31 GPa for spherical tip. Results of nanoindentation tests show that this method is very useful and is perfect for obtaining mechanical properties of trabecular bone. Estimated values of elastic modulus are similar. The differences between hardness are significant but it is a result of using two different types of tips. However, it has to be emphasised that the differences in the values of elastic modulus and hardness result from different testing protocols, anisotropy and asymmetry of the micro-samples and the hydration of bone.

Keywords: human bone, mechanical properties, nano hardness nanoindentation, trabecular bone

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25 Nanoindentation and Physical Properties of Polyvinyl Chloride/Styrene Co-Maleic Anhydride Blend Reinforced by Organo-Bentonite

Authors: D. E. Abulyazied, S. M. Mokhtar, A. M. Motawie


Polymer blends represent an important class of materials in engineering applications. The incorporation of clay nanofiller may provide new opportunities for this type of materials to enhance their applications. This article reports on the effects of clay on the structure and properties of polymer blends nanocomposites, based on Polyvinyl chloride PVC and styrene co-maleic anhydride SMA blend. Modification of the Egyptian Bentonite EB was carried out using organo-modifier namely; octadecylamine ODA. Before the modification, the cation exchange capacity CEC of the EB was measured. The octadecylamine bentonite ODA-B was characterized using Fourier transform infrared Spectroscopy FTIR, X-Ray Diffraction XRD, and Transition Electron Microscope TEM. A blend of Polyvinyl chloride PVC and styrene co-maleic anhydride SMA (50:50) was prepared in Tetra Hydro Furan (THF). Then nanocomposites of PVC/SMA/ODA-B were prepared by solution intercalation polymerization from 0.50% up to 5% by weight of ODA-B. The nanocomposites are characterized by XRD, TEM. Thermal, nanoindentation, swelling and electrical properties of the nanocomposites were measured. The morphology of the nanocomposites showed that ODA-B achieved good dispersion in the PVC/SMA matrix. Incorporation of 0.5 %, 1%, 3% and 5% by weight nanoclay into the PVC/SMA blends results in an improvement in nanohardness of 16%, 76%, 92%, and 68% respectively. The elastic modulus increased from 4.59 GPa for unreinforced PVC/SMA blend to 6.30 GPa (37% increase) with the introduction of 3% by weight nanoclay. The cross-link density of the nanocomposites increases with increasing the content of ODA-B.

Keywords: PVC, SMA, nanocomposites, nanoindentation, organo-bentonite

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24 Nanomechanical Properties of Coconut Shell Ash Blended Cement Mortar

Authors: Kumator Taku, Bilkisu Amartey


This research used Grid indentation technique to investigate the effect of the addition of Coconut Shell Ash (CSA) on the nanomechanical properties of the main phases of the hydrated cement paste. Portland cement was partially replaced with 15% CSA at a water-binder ratio of 0.5 and cubes casted and cured for 28 days after which they were polished to reduce surface roughness to the barest minimum. The result of nanoindentation shows that addition of 15% CSA to cement paste transforms portlandite to C-S-H by the pozzolanic reaction. More so, there is reduced porosity and a reduction in the volume of CH by the addition of the CSA. Even though the addition of 15% CSA does not drastically change the average values of the hardness and elastic modulus of the two phases of the C-S-H, it greatly modifies their relative proportions, leading to the production of more HD C-S-H. Overall, incorporating 15%CSA to cement mortar improves the Nanomechanical properties of the four main phases of the hydrated cement paste.

Keywords: Coconut Shell Ash, Elastic Modulus, Hardness, Nanoindentation, Porosity

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23 Mechanical Properties of CNT Reinforced Composite Using Berkovich Nanoindentation Analysis

Authors: Khondaker Sakil Ahmed, Ang Kok Keng, Shah Md Muniruzzaman


Spherical and Berkovich indentation tests are carried out numerically using finite element method for uniformly dispersed Carbon Nanotube (CNT) in the polymer matrix in which perfectly bonded CNT/matrix interface is considered. The Large strain elasto-plastic analysis is performed to investigate the actual scenario of nanoindentation test. This study investigates how the addition of CNT in polymer matrix influences the mechanical properties like hardness, elastic modulus of the nanocomposite. Since the wall thickness to radius ratio (t/r) is significantly small for SWCNT there is a huge possibility of lateral buckling which is a function of the location of indentation tip as well as the mechanical properties of matrix. Separate finite element models are constructed to compare the result with Berkovich indentation. This study also investigates the buckling behavior of different nanotube in a different polymer matrix.

Keywords: carbon nanotube, elasto-plastic, finite element model, nano-indentation

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22 Nanoindentation Behavior and Physical Properties of Polyvinyl Chloride /Styrene Co-Maleic Anhydride Blend Reinforced by Nano-Bentonite

Authors: Dalia Elsawy Abulyazied, Samia Mohamad Mokhtar, Ahmed Magdy Motawie


This article studies the effects of nano-bentonite on the structure and properties of polymer blends nanocomposites, based on polyvinyl chloride (PVC) and styrene co-maleic anhydride (SMA) blend. Modification of Egyptian bentonite (EB) is carried out using organo-modifier namely; octadecylamine (ODA). Octadecylamine bentonite (ODA-B) is characterized using FTIR, XRD and TEM. Nanocomposites of PVC/SMA/ODA-B are prepared by solution intercalation polymerization from 0.50 up to 5 phr. The nanocomposites are characterized by XRD and TEM. Thermal behavior of the nanocomposites is studied. The effect of different content of ODA-B on the nano-mechanical properties is investigated by a nano-indentation test method. Also the swelling and electrical properties of the nanocomposites are measured. The morphology of the nanocomposites shows that ODA-B achieved good dispersion in the PVC/SMA matrix. The thermal stability of the nanocomposites is enhanced due to the presence of the ODA-B. Incorporation of 0.5, 1, 3 and 5 phr. ODA-B into the PVC/SMA blends results in an improvement in nano-hardness of 16%, 76%, 92%, and 68% respectively. The elastic modulus increased by 37% from 4.59 GPa for unreinforced PVC/SMA blend to 6.30 GPa for 3 phr. The cross-link density and the electrical conductivity of the nanocomposites are increased with increasing the content of ODA-B.

Keywords: PVC, SMA, nanocomposites, nano-bentonite, nanoindentation, crosslink density

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21 Molecular Dynamics Study on Mechanical Responses of Circular Graphene Nanoflake under Nanoindentation

Authors: Jeong-Won Kang


Graphene, a single-atom sheet, has been considered as the most promising material for making future nanoelectromechanical systems as well as purely electrical switching with graphene transistors. Graphene-based devices have advantages in scaled-up device fabrication due to the recent progress in large area graphene growth and lithographic patterning of graphene nanostructures. Here we investigated its mechanical responses of circular graphene nanoflake under the nanoindentation using classical molecular dynamics simulations. A correlation between the load and the indentation depth was constructed. The nanoindented force in this work was applied to the center point of the circular graphene nanoflake and then, the resonance frequency could be tuned by a nanoindented depth. We found the hardening or the softening of the graphene nanoflake during its nanoindented-deflections, and such properties were recognized by the shift of the resonance frequency. The calculated mechanical parameters in the force vs deflection plot were in good agreement with previous experimental and theoretical works. This proposed schematics can detect the pressure via the deflection change or/and the resonance frequency shift, and also have great potential for versatile applications in nanoelectromechanical systems.

Keywords: graphene, pressure sensor, circular graphene nanoflake, molecular dynamics

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20 Austempered Compacted Graphite Irons: Influence of Austempering Temperature on Microstructure and Microscratch Behavior

Authors: Rohollah Ghasemi, Arvin Ghorbani


This study investigates the effect of austempering temperature on microstructure and scratch behavior of the austempered heat-treated compacted graphite irons. The as-cast was used as base material for heat treatment practices. The samples were extracted from as-cast ferritic CGI pieces and were heat treated under austenitising temperature of 900°C for 60 minutes which followed by quenching in salt-bath at different austempering temperatures of 275°C, 325°C and 375°C. For all heat treatments, an austempering holding time of 30 minutes was selected for this study. Light optical microscope (LOM) and scanning electron microscope (SEM) and electron back scattered diffraction (EBSD) analysis confirmed the ausferritic matrix formed in all heat-treated samples. Microscratches were performed under the load of 200, 600 and 1000 mN using a sphero-conical diamond indenter with a tip radius of 50 μm and induced cone angle 90° at a speed of 10 μm/s at room temperature ~25°C. An instrumented nanoindentation machine was used for performing nanoindentation hardness measurement and microscratch testing. Hardness measurements and scratch resistance showed a significant increase in Brinell, Vickers, and nanoindentation hardness values as well as microscratch resistance of the heat-treated samples compared to the as-cast ferritic sample. The increase in hardness and improvement in microscratch resistance are associated with the formation of the ausferrite matrix consisted of carbon-saturated retained austenite and acicular ferrite in austempered matrix. The maximum hardness was observed for samples austempered at 275°C which resulted in the formation of very fine acicular ferrite. In addition, nanohardness values showed a quite significant variation in the matrix due to the presence of acicular ferrite and carbon-saturated retained austenite. It was also observed that the increase of austempering temperature resulted in increase of volume of the carbon-saturated retained austenite and decrease of hardness values.

Keywords: austempered CGI, austempering, scratch testing, scratch plastic deformation, scratch hardness

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19 In situ High Temperature Characterization of Diamond-Like Carbon Films

Authors: M. Rouhani, F. C. N. Hong, Y. R. Jeng


The tribological performance of DLC films is limited by graphitization at elevated temperatures. Despite of numerous studies on the thermal stability of DLC films, a comprehensive in-situ characterization at elevated temperature is still lacking. In this study, DLC films were deposited using filtered cathodic arc vacuum method. Thermal stability of the films was characterized in-situally using a synchronized technique integrating Raman spectroscopy and depth-sensing measurements. Tests were performed in a high temperature chamber coupled with feedback control to make it possible to study the temperature effects in the range of 21 – 450 ̊C. Co-located SPM and Raman microscopy maps at different temperature over a specific area on the surface of the film were prepared. The results show that the thermal stability of the DLC films depends on their sp3 content. Films with lower sp3 content endure graphitization during the temperature-course used in this study. The graphitization is accompanied with significant changes in surface roughness and Raman spectrum of the film. Surface roughness of the films start to change even before graphitization transformation could be detected using Raman spectroscopy. Depth-sensing tests (nanoindentation, nano-scratch and wear) endorse the surface roughness change seen before graphitization occurrence. This in-situ study showed that the surface of the films is more sensitive to temperature rise compared to the bulk. We presume the changes observed in films hardness, surface roughness and scratch resistance with temperature rise, before graphitization occurrence, is due to surface relaxation.

Keywords: DLC film, nanoindentation, Raman spectroscopy, thermal stability

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18 Laser Shock Peening of Additively Manufactured Nickel-Based Superalloys

Authors: Michael Munther, Keivan Davami


One significant roadblock for additively manufactured (AM) parts is the buildup of residual tensile stresses during the fabrication process. These residual stresses are formed due to the intense localized thermal gradients and high cooling rates that cause non-uniform material expansion/contraction and mismatched strain profiles during powder-bed fusion techniques, such as direct metal laser sintering (DMLS). The residual stresses adversely affect the fatigue life of the AM parts. Moreover, if the residual stresses become higher than the material’s yield strength, they will lead to acute geometric distortion. These are limiting the applications and acceptance of AM components for safety-critical applications. Herein, we discuss laser shock peening method as an advanced technique for the manipulation of the residual stresses in AM parts. An X-ray diffraction technique is used for the measurements of the residual stresses before and after the laser shock peening process. Also, the hardness of the structures is measured using a nanoindentation technique. Maps of nanohardness and modulus are obtained from the nanoindentation, and a correlation is made between the residual stresses and the mechanical properties. The results indicate that laser shock peening is able to induce compressive residual stresses in the structure that mitigate the tensile residual stresses and increase the hardness of AM IN718, a superalloy, almost 20%. No significant changes were observed in the modulus after laser shock peening. The results strongly suggest that laser shock peening can be used as an advanced post-processing technique to optimize the service lives of critical components for various applications.

Keywords: additive manufacturing, Inconel 718, laser shock peening, residual stresses

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17 Analysis of Solvent Effect on the Mechanical Properties of Poly(Ether Ether Ketone) Using Nano-Indentation

Authors: Tanveer Iqbal, Saima Yasin, Muhammad Zafar, Ahmad Shakeel, Fahad Nazir, Paul F. Luckham


The contact performance of polymeric composites is dependent on the localized mechanical properties of materials. This is particularly important for fiber oriented polymeric materials where self-lubrication from top layers has been the basic requirement. The nanoindentation response of fiber reinforced poly(etheretherketone), PEEK, composites have been evaluated to determine the near-surface mechanical characteristics. Load-displacement compliance, hardness and elastic modulus data based on contact compliance mode (CSM) indentation of carbon fiber oriented and glass fiber oriented PEEK composites are reported as a function of indentation contact displacement. The composite surfaces were indented to a maximum penetration depth of 5µm using Berkovich tip indenter. A typical multiphase response of the composite surface is depicted from analysis of the indentation data for the composites, showing presence of polymer matrix, fibers, and interphase regions. The observed experimental results show that although the surface mechanical properties of carbon fiber based PEEK composite were comparatively higher, the properties of matrix material were seen to be increased in the presence of glass fibers. The experimental methodology may provide a convenient means to understand morphological description of the multimodal polymeric composites.

Keywords: nanoindentation, PEEK, modulus, hardness, plasticization

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16 Tuning Nanomechanical Properties of Stimuli-Responsive Hydrogel Nanocomposite Thin Films for Biomedical Applications

Authors: Mallikarjunachari Gangapuram


The design of stimuli-responsive hydrogel nanocomposite thin films is gaining significant attention in these days due to its wide variety of applications. Soft microrobots, drug delivery, biosensors, regenerative medicine, bacterial adhesion, energy storage and wound dressing are few advanced applications in different fields. In this research work, the nanomechanical properties of composite thin films of 20 microns were tuned by applying homogeneous external DC, and AC magnetic fields of magnitudes 0.05 T and 0.1 T. Polyvinyl alcohol (PVA) used as a matrix material and elliptical hematite nanoparticles (ratio of the length of the major axis to the length of the minor axis is 140.59 ± 1.072 nm/52.84 ± 1.072 nm) used as filler materials to prepare the nanocomposite thin films. Both quasi-static nanoindentation, Nano Dynamic Mechanical Analysis (Nano-DMA) tests were performed to characterize the viscoelastic properties of PVA, PVA+Hematite (0.1% wt, 2% wt and 4% wt) nanocomposites. Different properties such as storage modulus, loss modulus, hardness, and Er/H were carefully analyzed. The increase in storage modulus, hardness, Er/H and a decrease in loss modulus were observed with increasing concentration and DC magnetic field followed by AC magnetic field. Contact angle and ATR-FTIR experiments were conducted to understand the molecular mechanisms such as hydrogen bond formation, crosslinking density, and particle-particle interactions. This systematic study is helpful in design and modeling of magnetic responsive hydrogel nanocomposite thin films for biomedical applications.

Keywords: hematite, hydrogel, nanoindentation, nano-DMA

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15 A Comparative Study of the Tribological Behavior of Bilayer Coatings for Machine Protection

Authors: Cristina Diaz, Lucia Perez-Gandarillas, Gonzalo Garcia-Fuentes, Simone Visigalli, Roberto Canziani, Giuseppe Di Florio, Paolo Gronchi


During their lifetime, industrial machines are often subjected to chemical, mechanical and thermal extreme conditions. In some cases, the loss of efficiency comes from the degradation of the surface as a result of its exposition to abrasive environments that can cause wear. This is a common problem to be solved in industries of diverse nature such as food, paper or concrete industries, among others. For this reason, a good selection of the material is of high importance. In the machine design context, stainless steels such as AISI 304 and 316 are widely used. However, the severity of the external conditions can require additional protection for the steel and sometimes coating solutions are demanded in order to extend the lifespan of these materials. Therefore, the development of effective coatings with high wear resistance is of utmost technological relevance. In this research, bilayer coatings made of Titanium-Tantalum, Titanium-Niobium, Titanium-Hafnium, and Titanium-Zirconium have been developed using magnetron sputtering configuration by PVD (Physical Vapor Deposition) technology. Their tribological behavior has been measured and evaluated under different environmental conditions. Two kinds of steels were used as substrates: AISI 304, AISI 316. For the comparison with these materials, titanium alloy substrate was also employed. Regarding the characterization, wear rate and friction coefficient were evaluated by a tribo-tester, using a pin-on-ball configuration with different lubricants such as tomato sauce, wine, olive oil, wet compost, a mix of sand and concrete with water and NaCl to approximate the results to real extreme conditions. In addition, topographical images of the wear tracks were obtained in order to get more insight of the wear behavior and scanning electron microscope (SEM) images were taken to evaluate the adhesion and quality of the coating. The characterization was completed with the measurement of nanoindentation hardness and elastic modulus. Concerning the results, thicknesses of the samples varied from 100 nm (Ti-Zr layer) to 1.4 µm (Ti-Hf layer) and SEM images confirmed that the addition of the Ti layer improved the adhesion of the coatings. Moreover, results have pointed out that these coatings have increased the wear resistance in comparison with the original substrates under environments of different severity. Furthermore, nanoindentation hardness results showed an improvement of the elastic strain to failure and a high modulus of elasticity (approximately 200 GPa). As a conclusion, Ti-Ta, Ti-Zr, Ti-Nb, and Ti-Hf are very promising and effective coatings in terms of tribological behavior, improving considerably the wear resistance and friction coefficient of typically used machine materials.

Keywords: coating, stainless steel, tribology, wear

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14 Viscoelastic Behavior of Human Bone Tissue under Nanoindentation Tests

Authors: Anna Makuch, Grzegorz Kokot, Konstanty Skalski, Jakub Banczorowski


Cancellous bone is a porous composite of a hierarchical structure and anisotropic properties. The biological tissue is considered to be a viscoelastic material, but many studies based on a nanoindentation method have focused on their elasticity and microhardness. However, the response of many organic materials depends not only on the load magnitude, but also on its duration and time course. Depth Sensing Indentation (DSI) technique has been used for examination of creep in polymers, metals and composites. In the indentation tests on biological samples, the mechanical properties are most frequently determined for animal tissues (of an ox, a monkey, a pig, a rat, a mouse, a bovine). However, there are rare reports of studies of the bone viscoelastic properties on microstructural level. Various rheological models were used to describe the viscoelastic behaviours of bone, identified in the indentation process (e. g Burgers model, linear model, two-dashpot Kelvin model, Maxwell-Voigt model). The goal of the study was to determine the influence of creep effect on the mechanical properties of human cancellous bone in indentation tests. The aim of this research was also the assessment of the material properties of bone structures, having in mind the energy aspects of the curve (penetrator loading-depth) obtained in the loading/unloading cycle. There was considered how the different holding times affected the results within trabecular bone.As a result, indentation creep (CIT), hardness (HM, HIT, HV) and elasticity are obtained. Human trabecular bone samples (n=21; mean age 63±15yrs) from the femoral heads replaced during hip alloplasty were removed and drained from alcohol of 1h before the experiment. The indentation process was conducted using CSM Microhardness Tester equipped with Vickers indenter. Each sample was indented 35 times (7 times for 5 different hold times: t1=0.1s, t2=1s, t3=10s, t4=100s and t5=1000s). The indenter was advanced at a rate of 10mN/s to 500mN. There was used Oliver-Pharr method in calculation process. The increase of hold time is associated with the decrease of hardness parameters (HIT(t1)=418±34 MPa, HIT(t2)=390±50 MPa, HIT(t3)= 313±54 MPa, HIT(t4)=305±54 MPa, HIT(t5)=276±90 MPa) and elasticity (EIT(t1)=7.7±1.2 GPa, EIT(t2)=8.0±1.5 GPa, EIT(t3)=7.0±0.9 GPa, EIT(t4)=7.2±0.9 GPa, EIT(t5)=6.2±1.8 GPa) as well as with the increase of the elastic (Welastic(t1)=4.11∙10-7±4.2∙10-8Nm, Welastic(t2)= 4.12∙10-7±6.4∙10-8 Nm, Welastic(t3)=4.71∙10-7±6.0∙10-9 Nm, Welastic(t4)= 4.33∙10-7±5.5∙10-9Nm, Welastic(t5)=5.11∙10-7±7.4∙10-8Nm) and inelastic (Winelastic(t1)=1.05∙10-6±1.2∙10-7 Nm, Winelastic(t2) =1.07∙10-6±7.6∙10-8 Nm, Winelastic(t3)=1.26∙10-6±1.9∙10-7Nm, Winelastic(t4)=1.56∙10-6± 1.9∙10-7 Nm, Winelastic(t5)=1.67∙10-6±2.6∙10-7)) reaction of materials. The indentation creep increased logarithmically (R2=0.901) with increasing hold time: CIT(t1) = 0.08±0.01%, CIT(t2) = 0.7±0.1%, CIT(t3) = 3.7±0.3%, CIT(t4) = 12.2±1.5%, CIT(t5) = 13.5±3.8%. The pronounced impact of creep effect on the mechanical properties of human cancellous bone was observed in experimental studies. While the description elastic-inelastic, and thus the Oliver-Pharr method for data analysis, may apply in few limited cases, most biological tissues do not exhibit elastic-inelastic indentation responses. Viscoelastic properties of tissues may play a significant role in remodelling. The aspect is still under an analysis and numerical simulations. Acknowledgements: The presented results are part of the research project founded by National Science Centre (NCN), Poland, no.2014/15/B/ST7/03244.

Keywords: bone, creep, indentation, mechanical properties

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13 Effect of Irradiation on Nano-Indentation Properties and Microstructure of X-750 Ni-Based Superalloy

Authors: Pooyan Changizian, Zhongwen Yao


The purpose of current study is to make an excellent correlation between mechanical properties and microstructures of ion irradiated X-750 Ni-based superalloy. Towards this end, two different irradiation procedures were carried out, including single Ni ion irradiation and pre-helium implantation with subsequent Ni ion irradiation. Nano-indentation technique was employed to evaluate the mechanical properties of irradiated material. The nano-hardness measurements depict highly different results for two irradiation procedures. Single ion irradiated X-750 shows softening behavior; however, pre-helium implanted specimens present significant hardening compared to the un-irradiated material. Cross-section TEM examination demonstrates that softening is attributed to the γ׳-precipitate instability (disordering/dissolution) which overcomes the hardening effect of irradiation-induced defects. In contrast, the presence of cavities or helium bubbles is probably the main cause for irradiation-induced hardening of helium implanted samples.

Keywords: Inconel X-750, nanoindentation, helium bubbles, defects

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12 Nanomechanical Characterization of Titanium Alloy Modified by Nitrogen Ion Implantation

Authors: Josef Sepitka, Petr Vlcak, Tomas Horazdovsky, Vratislav Perina


An ion implantation technique was used for designing the surface area of a titanium alloy and for irradiation-enhanced hardening of the surface. The Ti6Al4V alloy was treated by nitrogen ion implantation at fluences of 2·1017 and 4·1017 cm-2 and at ion energy 90 keV. The depth distribution of the nitrogen was investigated by Rutherford Backscattering Spectroscopy. The gradient of mechanical properties was investigated by nanoindentation. The continuous measurement mode was used to obtain depth profiles of the indentation hardness and the reduced storage modulus of the modified surface area. The reduced storage modulus and the hardness increase with increasing fluence. Increased fluence shifts the peak of the mechanical properties as well as the peak of nitrogen concentration towards to the surface. This effect suggests a direct relationship between mechanical properties and nitrogen distribution.

Keywords: nitrogen ion implantation, titanium-based nanolayer, storage modulus, hardness, microstructure

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11 Characterization of a Pure Diamond-Like Carbon Film Deposited by Nanosecond Pulsed Laser Deposition

Authors: Camilla G. Goncalves, Benedito Christ, Walter Miyakawa, Antonio J. Abdalla


This work aims to investigate the properties and microstructure of diamond-like carbon film deposited by pulsed laser deposition by ablation of a graphite target in a vacuum chamber on a steel substrate. The equipment was mounted to provide one laser beam. The target of high purity graphite and the steel substrate were polished. The mechanical and tribological properties of the film were characterized using Raman spectroscopy, nanoindentation test, scratch test, roughness profile, tribometer, optical microscopy and SEM images. It was concluded that the pulsed laser deposition (PLD) technique associated with the low-pressure chamber and a graphite target provides a good fraction of sp3 bonding, that the process variable as surface polishing and laser parameter have great influence in tribological properties and in adherence tests performance. The optical microscopy images are efficient to identify the metallurgical bond.

Keywords: characterization, DLC, mechanical properties, pulsed laser deposition

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10 Nanocharacterization of PIII Treated 7075 Aluminum Alloy

Authors: Bruno Bacci Fernandes, Stephan Mändl, Ataíde Ribeiro da Silva Junior, José Osvaldo Rossi, Mário Ueda


Nitrogen implantation in aluminum and its alloys is acquainted for the difficulties in obtaining modified layers deeper than 200 nm. The present work addresses a new method to overcome such a problem; although, the coating with nitrogen and oxygen obtained by plasma immersion ion implantation (PIII) into a 7075 aluminum alloy surface was too shallow. This alloy is commonly used for structural parts in aerospace applications. Such a layer was characterized by secondary ion mass spectroscopy, electron microscopy, and nanoindentation experiments reciprocating wear tests. From the results, one can assume that the wear of this aluminum alloy starts presenting severe abrasive wear followed by an additional adhesive mechanism. PIII produced a slight difference, as shown in all characterizations carried out in this work. The results shown here can be used as the scientific basis for further nitrogen PIII experiments in aluminum alloys which have the goal to produce thicker modified layers or to improve their surface properties.

Keywords: aluminum alloys, plasma immersion ion implantation, tribological properties, hardness, nanofatigue

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9 The Effect of Interfacial Chemistry on Mechanical Properties of Epoxy Composites Containing Poly (Ether Ether Ketone) Grafted Multiwall Carbon Nanotubes

Authors: Prajakta Katti, Suryasarathi Bose, S. Kumar


In this work, carboxyl functionalized multiwall carbon nanotubes (a-MWNTs) covalently grafted with hydroxylated functionalized poly (ether ether ketone), HPEEK, which is miscible with the pre-polymer (epoxy) through the esterification reaction. The functionalized MWNTs were systematically characterized using spectroscopic techniques. The epoxy composites containing a-MWNTs and HPEEK grafted multiwall carbon nanotubes (HPEEK-g-MWNTs) were formulated using mechanical stirring coupled with a bath sonicator to improve the dispersion property of the nanoparticles and were subsequently cured at 80 ̊C and post cured at 180 ̊C. With the addition of 0.5 wt% of HPEEK-g-MWNTs, an impressive 44% enhancement in the storage modulus, 22% increase in tensile strength and 38% increase in fracture toughness was observed with respect to neat epoxy. In addition to these mechanical properties, the epoxy composites displayed significant enhancement in the hardness without reducing thermal stability. These improved properties were attributed to the tailored interface between HPEEK-MWNTs and epoxy matrix.

Keywords: epoxy, MWNTs, HPEEK-g-MWNTs, tensile properties, nanoindentation, fracture toughness

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8 Mechanical Investigation Approach to Optimize the High-Velocity Oxygen Fuel Fe-Based Amorphous Coatings Reinforced by B4C Nanoparticles

Authors: Behrooz Movahedi


Fe-based amorphous feedstock powders are used as the matrix into which various ratios of hard B4C nanoparticles (0, 5, 10, 15, 20 vol.%) as reinforcing agents were prepared using a planetary high-energy mechanical milling. The ball-milled nanocomposite feedstock powders were also sprayed by means of high-velocity oxygen fuel (HVOF) technique. The characteristics of the powder particles and the prepared coating depending on their microstructures and nanohardness were examined in detail using nanoindentation tester. The results showed that the formation of the Fe-based amorphous phase was noticed over the course of high-energy ball milling. It is interesting to note that the nanocomposite coating is divided into two regions, namely, a full amorphous phase region and homogeneous dispersion of B4C nanoparticles with a scale of 10–50 nm in a residual amorphous matrix. As the B4C content increases, the nanohardness of the composite coatings increases, but the fracture toughness begins to decrease at the B4C content higher than 20 vol.%. The optimal mechanical properties are obtained with 15 vol.% B4C due to the suitable content and uniform distribution of nanoparticles. Consequently, the changes in mechanical properties of the coatings were attributed to the changes in the brittle to ductile transition by adding B4C nanoparticles.

Keywords: Fe-based amorphous, B₄C nanoparticles, nanocomposite coating, HVOF

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7 Investigation of the Self-Healing Sliding Wear Characteristics of Niti-Based PVD Coatings on Tool Steel

Authors: Soroush Momeni


Excellent damping capacity and superelasticity of the bulk NiTi shape memory alloy (SMA) makes it a suitable material of choice for tools in machining process as well as tribological systems. Although thin film of NiTi SMA has a same damping capacity as NiTi bulk alloys, it has a poor mechanical properties and undesirable tribological performance. This study aims at eliminating these application limitations for NiTi SMA thin films. In order to achieve this goal, NiTi thin films were magnetron sputtered as an interlayer between reactively sputtered hard TiCN coatings and hard work tool steel substrates. The microstructure, composition, crystallographic phases, mechanical and tribological properties of the deposited thin films were analyzed by using field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), nanoindentation, ball–on-disc, scratch test, and three dimensional (3D) optical microscopy. It was found that under a specific coating architecture, the superelasticity of NiTi inter-layer can be combined with high hardness and wear resistance of TiCN protective layers. The obtained results revealed that the thickness of NiTi interlayers is an important factor controlling mechanical and tribological performance of bi-layer composite coating systems.

Keywords: PVD coatings, sliding wear, hardness, tool steel

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6 Effect of Pretreatment on Quality Parameters of Natural Convection Mixed-Mode Solar Dried Potato

Authors: Kshanaprava Dhalsamant, Punyadarshini P. Tripathy, Shanker L. Shrivastava


With present high global population, the need for rising food usage by minimizing food wastage and investment is highly necessary to achieve food security. The purpose of this study is to enlighten the effect of pre-drying treatment on rehydration, color, texture, nanohardness, microstructure and surface morphology of solar dried potato samples dried in the mixed-mode solar dryer. Locally bought potatoes were cleaned and cut into cylindrical pieces and pretreated with sodium metabisulfite (0.5%) for 10 min before placing them in natural convection solar dryer designed and developed in Indian Institute of Technology Kharagpur, India. Advanced quality characteristics were studied using Atomic Force Microscope (AFM), Scanning Electron Microscopy (SEM) and nanoindentation method, along with color, texture and water activity. The rehydration indices of solar dried potatoes were significantly biased by pretreatment followed by rehydration temperature. A lower redness index (a*) with a higher value of yellowness index (b*), chroma (C*) and hue angle (h*) were obtained for pretreated samples. Also, the average nanohardness (H) of untreated samples exhibited substantial lower value (18.46%) compared to pretreated samples. Additionally, a creep displacement of 43.27 nm during 20 s dwell time under constant load of 200

Keywords: pretreatment, nanohardness, microstructure, surface morphology

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5 Novel Hybrid Ceramic Nanocomposites Fabricated by Rapid Sintering Technology

Authors: Iftikhar Ahmad, Abulhakim Almajid


Alumina (Al2O3) is an attractive structural ceramic however; brittleness turns Al2O3 down for advanced applications. Development of multi-phase phase ceramics systems is promising to curtail the brittleness and the incorporation of strong/elastic graphene, as third phase, into dual phase (Al2O3-SiC) is striking for mechanical upgrading purpose. Thin graphene nanosheets (GNS) were prepared by thermal exfoliation process and reinforced into dual phase ceramic system. The hybrid nanocomposite was consolidated by novel HF-IH (high-frequency induction heating) sintering furnace at 1500 °C under 50 MPa in vacuum conditions. Structural features and grain size of the resulting nanocomposite were analyzed by SEM and TEM whilst the mechanical properties were assessed by microhardness and nanoindentation techniques. The fracture toughness of the hybrid nanocomposites was appraised by direct crack measurement method. Electron microscopic investigations confirmed the preparation of thin (< 10 nm) graphene nanosheets (GNS). HF-IH sintering route condensed the three-phase (GNS-Al2O3-SiC) hybrid nanocomposite system to > 99% relative densities. SEM of the hybrid nanocomposites fractured surfaces revealed even distribution of the nanocomposite constituents and changed in fracture-mode. Structurally, 88% grain reduction into hybrid nanocomposite was also obtained. Mechanically, enhanced fracture toughness (50%) and hardness (53%) were also achieved for hybrid nanocomposites were attained against bench marked monolithic Al2O3.

Keywords: alumina, graphene, hybrid nanocomposites, rapid sintering

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