Indentation Tests Research Articles

A facile method to fabricate auxetic polymer foams

This paper presents a new efficient method for manufacturing auxetic foams, a subcategory of metamaterials with intriguing mechanical properties. Unlike previous methods that require two steps involving heating or the use of a chemical solvent, the present method involves compressing the foam during the manufacturing process after cells have been formed in the die, but while the material remains soft. This one-step process is more time-efficient, energy-efficient, and flexible; it also requires fewer facilities and materials. After the manufacturing process, various mechanical properties of the auxetic foams were evaluated by compression tests (energy absorption, mean force, and maximum force) and indentation tests (stiffness, absorbed energy, and hysteresis energy). The results confirmed that the auxetic foams exhibited superior behavior compared with conventional foam at the same density. To further investigate the foam microstructures and deformation mechanisms, in situ compression tests were conducted; the macro behaviors of the foams were explained based on these observations. Overall, this paper presents a promising approach for the manufacturing of auxetic foams with improved mechanical properties that can be used in applications typically dominated by conventional foams.

Three-dimensional indentation test system for observing the distribution of internal mechanical properties in materials

This paper describes the development of a three-dimensional (3D) indentation test system capable of observing the distribution of mechanical properties in structural materials. Serial sectioning with destructive treatment has traditionally been used as a method for observing microstructure within materials in three dimensions. The serial sectioning methods using precision cutting has attracted particular attention as it enables the observation of large sample volumes. However, those methods can only observe the microstructure as image, not the mechanical properties such as hardness and elastic modulus. To measure the 3D distribution of the mechanical properties of the material, it is effective to combine repeated cutting and indentation tests on each cutting surface. Morever, combining the image observation and mechanical property tests could allow a more sophisticated analysis of the interior of material. To implement this method, we have constructed an indentation test system on a precision machine using a Berkovich indenter, micro-force sensor, and micro-movement stage.In order to achieve a 3D indentation test, it is considered necessary to unify the measurement positions in the depth direction. Furthermore, the unloading rate needs to be controlled in order to carry out stable indentation tests. Therefore, we propose a method of 3D indentation test that can precisely control the maximum depth of indentation and unloading speed.In this paper, we devise a method for driving the constructed system and a method for obtaining data and confirm the accuracy of these methods by experiment. In addition, we determine indentation depth and unloading speed which are suitable for our method by performing indentation tests on a block for ultra-microhardness. Finally, we practice 3D indentation test in which the cutting and indentation tests are repeated on specimens with different mechanical properties in the depth direction. Experimental results show that our indentation test system is appropriate to measure three-dimensional mechanical properties inside the material.

DEM modelling of surface indentations caused by granular materials: application to wheel–rail sanding

The presented surface indentation model is one step towards building a DEM model for wheel–rail sanding. In railways, so-called low-adhesion conditions can cause problems in traction and braking, and sanding is used to overcome this problem. Sand grains are blasted towards wheel–rail contact, fracture repeatedly as they enter the nip and are drawn into the contact and then increase adhesion. Research on this topic has mostly been experimental, but focussed on adhesion enhancement measurement. Thus, physical mechanisms increasing the adhesion are not well understood. Previous works involved experiments and DEM modelling of single sand grain crushing tests under realistic wheel–rail contact pressures of 900 MPa, focusing on sand fragment spread and formation of clusters of solidified fragments. In the experiments, indents in the compressing steel plates were also observed, which are also observed on wheel and rail surfaces in railway operation. These are now modelled by adapting an existing surface indentation model from literature to the case of surface indentations caused by granular materials. Two test cases are studied, and experimental spherical indentation tests for model parametrisation are presented. In a proof of concept, the mentioned single sand grain crushing tests under 900 MPa pressure are simulated including the surface indentation model. This work contributes to DEM modelling of wheel–rail sanding, which is believed to be a good approach to deepen the understanding of adhesion increasing mechanisms under sanded conditions.

Effect of artificially induced microcracks near the rock surface on granite fragmentation performance under heating treatment

Various novel assisted drilling technologies enhance rock fragmentation performance by introducing microcracks on the rock surface to weaken rock strength. However, the quantitative relationship between artificially induced microcracks and rock fragmentation characteristics is not clear. In this study, we induced artificial microcracks of varying degrees on the rock surface through one-dimensional heat conduction. With the aid of the fluorescent resin, we visualized the microcrack patterns and quantitatively assessed the artificially induced microcracks. Subsequently, we performed quasi-static indentation tests on granite samples containing microcracks to establish the quantitative relationship between microcracks and rock fragmentation performance. The results indicate that the release of crystal water within the temperature range of 200 °C–300 °C is the primary factor leading to a significant increase in microcracks. Load drop signals correlate with the propagation of microcracks, including the competitive interactions between mechanically induced microcracks and artificially induced microcracks. Artificially induced microcracks require a certain initial length to continue propagating under mechanical stress, and excessively short microcracks are detrimental to subsequent propagation. A higher density of microcracks implies a more complex microcrack network, facilitating the merging of cracks to form rock chips under smaller mechanical loads. The consistency between the length density and number density of microcracks in influencing the crater parameters reflects their equal importance in affecting rock fragmentation performance. These findings could help determine the extent of rock weakening by artificially induced microcracks and reveal the mechanisms of rock fracture behavior influenced by microcrack, holding significant implications for the optimization of the process parameters of various assisted rock drilling techniques.

Effect of zirconium addition on microstructural characteristics and nano-mechanical properties of P9 steel

Micro-alloying in steels has significant effects on microstructure and its properties. The main objective of the work is to understand the influence of zirconium (Zr) addition to P9 ferritic/martensitic (F/M) steel on phase stability, microstructure, and nanomechanical properties. The alloy compositions in this study were designed using thermodynamic calculations, based on which steels with Zr concentration in the range of 0.05–2 wt.% were synthesized using vacuum arc melting. The cast alloy was subjected to thermo-mechanical treatments followed by austenitization and tempering treatments. Zr concentration of the steel was found to influence the nature of secondary phases formed, which were quantified through detailed synchrotron X-ray diffraction (XRD) analysis and also characterised extensively using electron microscopy techniques. Detailed structural analysis of the Fe23Zr6 phase using aberration corrected transmission electron microscopy is reported for the first time. The nano-mechanical properties of the heat-treated steels were evaluated using instrumented indentation tests at room temperature with a sphero-conical indenter. A systematic variation in hardness and yield strength with Zr content of P9 steel was observed, which is correlated to the microstructural changes. The P9 F/M steel with optimum concentration of Zr, with better mechanical properties is proposed through this structure-property correlation study.

Surface Layer Performance of Low-Cost 3D-Printed Sliding Components in Metal-Polymer Friction

Abstract The paper presents the results of contact strength and tribological property tests of spare parts made of a popular resin using a 3D DLP printing technology. Two printer models by the same manufacturer were used in the study. The post-processing technique, which shapes the final functional properties, was diversified. Surface performance properties were compared, i.e. Shore hardness, indentation hardness, Martens hardness, elastic modulus, and parameters related to surface creep and relaxation. Tribo-logical durability in rotary motion and tribological wear in reciprocating linear motion were also evaluated using micro- and nanotribometers. This was followed by surface analyses of the friction track of the analysed materials using microscopic methods: a scanning electron microscope, a WLI interferometric microscope, and an optical microscope. The results were statistically processed and the relationship between the parameters determined in the indentation test was determined.

Deformation Behavior of Alloys Based on Iron and Manganese in Scratch, Tensile, and Indentation Tests

Deformation Behavior of Alloys Based on Iron and Manganese in Scratch, Tensile, and Indentation Tests

Development of a Method for Estimating Stress-strain Relationships Based on the Results of Indentation Tests that Eliminated the Size Effect Attributed to Ultra-small Loads

Development of a Method for Estimating Stress-strain Relationships Based on the Results of Indentation Tests that Eliminated the Size Effect Attributed to Ultra-small Loads

Application of instrument indentation test for residual stress characterization of 5083 aluminium alloy

Abstract An abnormal cracking phenomenon occurred at the corner of a ventilation window on the 5083 aluminum alloy wallboard used in certain transportation equipment. The residual stresses of the wallboard were measured using an instrumented indentation test. Initially, stress loading was applied to the 5083 specimens using a residual stress loading device to verify the effectiveness of the instrument indentation test (IIT) for testing the residual stresses of 5083 aluminum alloy. Subsequently, IIT was conducted under static conditions at the serving site of the equipment, and the working stresses under dynamic conditions were detected using a strain monitor. The results indicate that the total tensile stress at the uncracked corner of the ventilation window has exceeded the 5083 yield strength, so excessive tensile stress is the main cause of the abnormal cracking of the wallboard.

Experimental investigations on characterizing the uniaxial mechanical property variations along the thickness of hydrogenation reactor welded joints by spherical indentation tests

To meet the demands for non-destructive testing of uniaxial mechanical properties of welded joints of thick-wall hydrogenation reactors, this study provides an experimental investigation on whether the spherical indentation tests (SITs) can accurately characterize the uniaxial mechanical property variations along the thickness of welded joints. The phenomenologically summarized empirical method (i.e., the Kwon method) and the semi-analytical method (i.e., the simplified-IIEM) were selected as representatives, and their reliability was judged from the viewpoints of stress-strain prediction, the inversion accuracy and repeatability of strength, and the ability to characterize the variation of uniaxial mechanical properties along the thickness of welded joints. Characteristics of the inverse predictions were analyzed, and the source of errors in each method were extensively investigated. This study provides a theoretical and technical guidance for the engineering application and promotion of SITs.

Relationship between depth-wise refractive index and biomechanical properties of human articular cartilage.

Optical properties of biological tissues, such as refractive index (RI), are fundamental properties, intrinsically linked to the tissue's composition and structure. We hypothesize that, as the RI and the functional properties of articular cartilage (AC) are dependent on the tissue's structure and composition, the RI of AC is related to its biomechanical properties. This study aims to investigate the relationship between RI of human AC and its biomechanical properties. Human cartilage samples ( ) were extracted from the right knee joint of three cadaver donors (one female, aged 47 years, and two males, aged 64 and 68 years) obtained from a commercial biobank (Science Care, Phoenix, Arizona, United States). The samples were initially subjected to mechanical indentation testing to determine elastic [equilibrium modulus (EM) and instantaneous modulus (IM)] and dynamic [dynamic modulus (DM)] viscoelastic properties. An Abbemat 3200 automatic one-wavelength refractometer operating at 600 nm was used to measure the RI of the extracted sections. Similarly, Spearman's and Pearson's correlation coefficients were employed for non-normal and normal datasets, respectively, to determine the correlation between the depth-wise RI and biomechanical properties of the cartilage samples as a function of the collagen fibril orientation. A positive correlation with statistically significant relations ( ) was observed between the RI and the biomechanical properties (EM, IM, and DM) along the tissue depth for each zone, e.g., superficial, middle, and deep zones. Likewise, a lower positive correlation with statistically significant relations ( ) was also observed for collagen fibril orientation of all zones with the biomechanical properties. The results indicate that, although the RI exhibits different levels of correlation with different biomechanical properties, the relationship varies as a function of the tissue depth. This knowledge paves the way for optically monitoring changes in AC biomechanical properties nondestructively via changes in the RI. Thus, the RI could be a potential biomarker for assessing the mechanical competency of AC, particularly in degenerative diseases, such as osteoarthritis.

Stress and Strain Characterization for Evaluating Mechanical Safety of Lithium-Ion Pouch Batteries under Static and Dynamic Loadings

The crashworthiness of electric vehicles depends on the response of lithium-ion cells to significant deformation and high strain rates. This study thoroughly explores the mechanical behavior due to damage of lithium-ion battery (LIB) cells, focusing on Lithium Nickel Manganese Cobalt Oxide (NMC) and Lithium Iron Phosphate (LFP) types during both quasi-static indentation and dynamic high-velocity penetration tests. Employing a novel approach, a hemispherical indenter addresses gaps in stress–strain data for pouch cells, considering crucial factors like strain rate/load rate and battery cell type. In the finite element method (FEM) analysis, the mechanical response is investigated in two stages. First, a viscoplastic model is developed in Abaqus/Standard to predict the indentation test. Subsequently, a thermomechanical model is formulated to predict the high-speed-impact penetration test. Considering the high plastic strain rate of the LIB cell, adiabatic heating effects are incorporated into this model, eliminating heat conduction between elements. Addressing a notable discrepancy from prior research, this work explores the substantial reduction in force observed when transitioning from a single cell to a stack of two cells. The study aims to unveil the underlying reasons and provide insights into the mechanical behavior of stacked cells.

A New Method for the Dynamics Analysis of Super-Elastic-Plastic Foams under Inhomogeneous Loading and Unloading Conditions.

In this research, a new computational method was proposed for describing the mechanical behavior of super-elastic-plastic foams under inhomogeneous compressive impacts. The method regarded the foam material as composed of two typical mechanical properties superimposed multiple times: one was the hyper-elastic layer, and the other was the elastoplastic layer. The hyper-elastic layer and the elastoplastic layer were interwoven and overlapped, divided into double-layer, four-layer, and six-layer configurations to characterize the foam material. After the equivalent layering of the foam, by comparing the results of the four-layer and six-layer divisions, it was found that when the layering reached four layers, the foam performance curve had already converged. The study utilized the HYPERFOAM model and Mullins effect in the ABAQUS software to establish the constitutive relationship of the hyper-elastic layer. It adopted the Crushable foam model to develop the constitutive relationship of the elastoplastic layer. Under uniaxial compression conditions, quasi-static and intermediate strain rate compression tests were performed on polyethylene (PE) foam materials with three different densities. Based on the experimental results, the parameter values of the hyper-elastic-plastic foam model in the ABAQUS code were determined. By comparing the computational results and the experimental results, the established finite element (FE) model was validated using the mechanical behavior of indentation and compression tests. The results showed that this method could effectively describe the complex mechanical behavior and residual deformation of hyper-elastic-plastic foam packaging materials under non-uniform compression, and the experimental and simulation results agreed well, proving the reliability of this method.

Effect of elastic gradients on the fracture resistance of tri-layer restorative systems

ObjectivesTo assess the impact of elastic gradients formed among restorative material, cement, and substrate on the fracture resistance of tri-layer restorative systems. MethodsFour CAD/CAM materials were utilized, two glass-ceramics (IPS e.max CAD, Vita Suprinity) and two resin-ceramic hybrids (Vita Enamic, Lava Ultimate). Their fracture resistance was examined by biaxial flexure (n = 8) and Hertzian indentation (n = 10) tests. Statistical analysis was conducted using ANOVA and Tukey tests (p = 5 %). Finite element analysis (FEA) was employed to simulate the Hertzian indentation test and elucidate the stress-fields formed on the intaglio surface below the loading area. ResultsThe biaxial flexural strength (MPa) of glass-ceramics exceeded the hybrid materials (e.max 417a, Suprinity 230b, Enamic 138c, and Lava Ultimate 183bc). Conversely, the load-bearing capacity (N) of the materials bonded to dentin analog demonstrated the opposite trend, with the hybrid materials achieving superior results (e.max 830 C, Suprinity 660D, Enamic 1822B, and Lava Ultimate 2593 A). The stress-fields observed by FEA were coherent with the experimental results for Hertzian flexural stresses (MPa): e.max 501 A, Suprinity 342 C, Enamic 406B, whereas no tensile stress was observed at the intaglio surface of Lava Ultimate. SignificanceDetailed analysis of the fracture resistance of the tri-layer restorative systems showed that the elastic gradients play a more significant role than the flexural strength of the restorative materials. The coherence of the elastic moduli between the restorative material and supporting structures results in reduced tensile stress concentration at the intaglio surface beneath the loading area and enhances the ability to withstand load.

Deep Indentation Tests of Soft Materials Using Mobile and Stationary Devices.

Measurements of the properties of soft materials are important from the point of view of medical diagnostics of soft tissues as well as testing the quality of food products and many technical materials. One of the frequently used techniques for testing such materials, attractive due to its non-invasive nature, is the indentation technique, which does not puncture the material. The difficulty of testing soft materials, which affects the objectivity of the results, is related to the problems of stable positioning of the studied material in relation to the indentation apparatus, especially with a device held by the operator. This work concerns the comparison of test results using an indentation apparatus mounted on mobile and stationary handles. The tested materials are cylindrical samples of polyurethane foams with three different stiffnesses and the same samples with a 0.5 or 1 mm thick silicone layer. The study presented uses an apparatus with a flat cylindrical indenter, with a surface area of 1 cm2, pressed to a depth of 10 mm (so-called deep tests). Based on the recorded force changes over time, five descriptors of the indentation test were determined and compared for both types of handles. The tests performed showed that the elastic properties of foam materials alone and with a silicone layer can be effectively characterized by the maximum forces during recessing and retraction and the slopes of the recessing and retraction curves. In the case of two-layer materials, these descriptors reflect both the characteristics of the foams and the silicone layer. The results show that the above property of the deep indentation method distinguishes it from the shallow indentation method. The repeatability of the tests performed in the mobile and stationary holders were determined to be comparable.

Thermal runaway of Li-ion batteries caused by hemispherical indentation under different temperatures: Battery deformation and fracture

Thermal runaway (TR) of Li-ion batteries (LIBs) presents a disastrous safety hazard and a significant barrier to the wider adoption of electric vehicles (EVs). Internal short circuit (ISC) induced by mechanical abuse is one of the causes of battery TR. This paper uses hemispherical indentation tests to trigger ISC in the battery at different temperatures and studies the battery deformation and fracture mode. Results show as the initial temperature increases, the battery hardness and strength decrease, and the fracture mode of the laminar structure changes from shear fracture to localized rupture. In the shear fracture mode, the ISC homogeneously heats the battery, and it does not directly trigger TR. In the localized rupture mode, the ISC is only induced at the layers close to the indenter and generates a hot spot exceeding 200 °C, leading to the initiation of TR. Therefore, the mechanical properties of batteries under different conditions need to be studied in more detail to develop batteries that are safer under mechanical abuse.

A mechanical TiAl/TiAlN multinanolayer coating model based on microstructural analysis and nanoindentation

A finite element model reproducing the mechanical behaviour during nanoindentation tests on Ti0.67Al0.33/Ti0.54Al0.46N multilayer coatings was developed. Coatings with two different nanoperiods (10 and 50 nm) were deposited by radio-frequency magnetron sputtering from a single sintered titanium/aluminium target using the reactive gas pulsing process. X-ray diffraction and transmission electron microscopy confirmed the multilayer stacking of the coatings. The finite element models of coatings with these two stacking periods were built considering successive hypotheses: equal thicknesses for metal and nitride nanolayers stacked without transition layer, equal thicknesses stacking with a transition layer between each metal and nitride nanolayer and finally imbalanced thicknesses stacking with a transition layer. The elastic and plastic properties of the stacked nanolayers were determined on thick monolithic coatings of metal and nitride using indentation testing and the finite element model updating method respectively. The elastic-plastic properties of the interface were introduced in the multilayer model as a rule of mixtures of the metal and nitride properties using two hypotheses: parallel or serial. For 50 nm-period film, the interface has a negligible effect on the overall indentation response. On the other hand, for the 10 nm period, the imbalanced stacking model with precise knowledge of the transition layer thickness obtained by N K-edge electron energy loss spectroscopy is required to reproduce the experimental indentation curve. Compared to classical analytical models accounting for hardness, not only the hardnesses but also the indentation moduli appear to be well predicted and evaluated in this work.

Characterisation and Application of Bio-Inspired Hybrid Composite Sensors for Detecting Barely Visible Damage under Out-of-Plane Loadings.

Traditional inspection methods often fall short in detecting defects or damage in fibre-reinforced polymer (FRP) composite structures, which can compromise their performance and safety over time. A prime example is barely visible impact damage (BVID) caused by out-of-plane loadings such as indentation and low-velocity impact that can considerably reduce the residual strength. Therefore, developing advanced visual inspection techniques is essential for early detection of defects, enabling proactive maintenance and extending the lifespan of composite structures. This study explores the viability of using novel bio-inspired hybrid composite sensors for detecting BVID in laminated FRP composite structures. Drawing inspiration from the colour-changing mechanisms found in nature, hybrid composite sensors composed of thin-ply glass and carbon layers are designed and attached to the surface of laminated FRP composites exposed to transverse loading. A comprehensive experimental characterisation, including quasi-static indentation and low-velocity impact tests alongside non-destructive evaluations such as ultrasonic C-scan and visual inspection, is conducted to assess the sensors' efficacy in detecting BVID. Moreover, a comparison between the two transverse loading types, static indentation and low-velocity impact, is presented. The results suggest that integrating sensors into composite structures has a minimal effect on mechanical properties such as structural stiffness and energy absorption, while substantially improving damage visibility. Additionally, the influence of fibre orientation of the sensing layer on sensor performance is evaluated, and correlations between internal and surface damage are demonstrated.

Inverse Method to Determine Parameters for Time-Dependent and Cyclic Plastic Material Behavior from Instrumented Indentation Tests.

Indentation is a versatile method to assess the hardness of different materials along with their elastic properties. Recently, powerful approaches have been developed to determine further material properties, like yield strength, ultimate tensile strength, work-hardening rate, and even cyclic plastic properties, by a combination of indentation testing and computer simulations. The basic idea of these approaches is to simulate the indentation with known process parameters and to iteratively optimize the initially unknown material properties until just a minimum error between numerical and experimental results is achieved. In this work, we have developed a protocol for instrumented indentation tests and a procedure for the inverse analysis of the experimental data to obtain material parameters for time-dependent viscoplastic material behavior and kinematic and isotropic work-hardening. We assume the elastic material properties and the initial yield strength to be known because these values can be determined independently from indentation tests. Two optimization strategies were performed and compared for identification of the material parameters. The new inverse method for spherical indentation has been successfully applied to martensitic steel.

Parallel-beams magnetic actuator for in-situ transmission electron microscope observation of mechanical testing

Abstract Understanding the microscopic mechanisms behind mechanical fractures is essential for enhancing material properties and increasing reliability through fatigue suppression. Conventional mechanical testing methods, such as indentation tests that press a sharp needle into a specimen or tensile tests using hydraulic pumps, are unable to capture nanoscale deformations under applied forces. As a result, the microscopic mechanisms that influence mechanical properties are often inferred indirectly, and material design largely depends on the engineer’s intuition and occasional serendipity. To overcome these challenges, in-situ observation techniques utilizing transmission electron microscopes (TEMs) have been developed to enable the observation of sample deformations at the nanoscale. However, despite their high resolution, conventional TEMs are limited by a small available space -often just a few millimeters- that restricts the application of sufficient force to fracture specimens. Traditional actuation methods, such as thermal expansion, electrostatic force, and piezoelectric actuators, fail to generate significant forces within such confined spaces. In response to these limitations, our research involved the development of a micromachine with multiple parallel beams. This device leverages the Laplace force generated by an electric current passing through the beams and the magnetic field of the TEM. We demonstrated the capability to produce significant force using the magnetic field from the microscope’s magnetic lens. The actuator developed in our study successfully generated forces exceeding 50 µN, marking a significant advancement in the in-situ observation capabilities for mechanical testing.