Cyclic Indentation Research Articles

Total body irradiation is associated with long-term deficits in femoral bone structure but not mechanical properties in male rhesus macaques.

Exposure to ionizing radiation for oncological therapy increases the risk for late-onset fractures in survivors. However, the effects of total body irradiation (TBI) on adult bone are not well-characterized. The primary aim of this study was to quantify the long-term effects of TBI on bone microstructure, material composition, and mechanical behavior in skeletally mature rhesus macaque (Macaca mulatta) non-human primates. Femora were obtained post-mortem from animals exposed to an acute dose of TBI (6.0-6.75Gy) nearly a decade earlier, age-matched non-irradiated controls, and non-irradiated young animals. The microstructure of femoral trabecular and cortical bone was assessed via micro-computed tomography. Material composition was evaluated by measuring total fluorescent advanced glycation end products (fAGEs). Cortical bone mechanical behavior was quantified via four-point bending and cyclic reference point indentation (cRPI). Animals exposed to TBI had slightly worse cortical microstructure, including lower cortical thickness (-11%, p = 0.037) and cortical area (-24%, p = 0.049), but similar fAGE content and mechanical properties as age-matched controls. Aging did not influence cortical microstructure, fAGE content, or cRPI measures but diminished femoral cortical post-yield properties, including toughness to fracture (-32%, p = 0.032). Because TBI was administered after the acquisition of peak bone mass, these results suggest that the skeletons of long-term survivors of adulthood TBI may be resilient, retaining or recovering their mechanical integrity during the post-treatment period, despite radiation-induced architectural deficits. Further investigation is necessary to better understand radiation-induced skeletal fragility in mature and immature bone to improve care for radiation patients of all ages.

Advancement of constant and progressive load multi‐cycle indentation method on surface properties characterization of polymers

AbstractIn recent years, polymers have been popular in industrial applications due to their lightweight, corrosion‐resistant, improved surface polish, ease of manufacturing, cost‐effectiveness, and so forth. Similarly, micro/nano‐indentation has gained popularity as a technique for assessing the surface mechanical characteristics of polymers. The present study conducted comprehensive experiments using cyclic micro‐indentation on engineering polymers, specifically poly‐ether‐ether‐ketone (PEEK), poly(methyl methacrylate) (PMMA), and poly(tetra‐fluoroethylene) (PTFE). An appropriate and optimal indentation method has been proposed after analyzing the behavior and significance of all the input parameters in evaluating the properties. Both constant load multi‐cycle (CLMC) and progressive load multi‐cycle (PLMC) were considered for this investigation. A comparative evaluation has been conducted to assess two multi‐cycle tests on these materials. From the analysis of the input parameters, including maximum loads, loading and unloading rates, and the number of cycles, the unloading rate and indentation cycle are crucial factors in determining hardness (H) and elastic modulus (E). Increasing the loading rates leads to an increase in H and a reduction in E for all three materials. This effect arises from the thermal effect, which is characterized by the creep modulus and a closed hysteresis loop. Employing the holding duration and multiple cycle data in constant load multi‐cycle can significantly influence the creep behavior and use of the hysteresis loop for fatigue behavior. Similarly, a progressive load multi‐cycle indentation with a force greater than 0.5 N and a minimum of five cycles is the most accurate approach for evaluating surface mechanical parameters.

Room‐temperature bulk plasticity and tunable dislocation densities in KTaO3

AbstractWe report room‐temperature bulk plasticity mediated by dislocations in single‐crystal cubic potassium tantalate oxide (KTaO3), contrasting the conventional knowledge that single‐crystal KTaO3 is susceptible to brittle fracture. A mechanics‐based combinatorial experimental approach using cyclic Brinell indentation, scratching, and uniaxial bulk compression consistently demonstrates room‐temperature dislocation plasticity in KTaO3 from the mesoscale to the macroscale. This approach also delivers tunable dislocation densities and plastic zone size. Scanning transmission electron microscopy analysis underpins the activated slip system to be <110> {10}. Given the growing significance of KTaO3 as an emerging electronic oxide and the increasing interest in dislocations for tuning the physical properties of oxides, our findings are expected to trigger synergistic research interest in KTaO3 with tunable dislocation densities.

Contact fatigue of thin hard diamond-like carbon films on M50 steels under cyclic spherical micro-indentation

Contact fatigue behaviors of thin hard diamond-like carbon (DLC) films on M50 steels during cyclic spherical micro-indentations were investigated. The stress-strain evolution of the entire system was analyzed by finite element methods. The film fracture mechanisms and interfacial bearing responses under monotonic and repeated contacts were comprehensively explored. Concentrated tensile and shear stresses were found to, respectively, govern the initiation and propagation of the surface ring cracks. Elevated tensile stresses at the initiation and epilogue of each indentation cycle enhanced bottom radial cracking. At the interfaces, the maximum tensile (σnmax) and shear (σtmax) stresses occurred at the end of unloading and loading processes, respectively. With increasing maximum indentation forces, σnmax initially increased and then gradually decreased, while σtmax increased monotonically.

Near‐surface plastic deformation in polycrystalline SrTiO3 via room‐temperature cyclic Brinell indentation

AbstractDislocations are being used to tune versatile mechanical and functional properties in oxides with most current studies focusing on single crystals. For potentially wider applications, polycrystalline ceramics are of concern, provided that dislocations can be successfully introduced. However, in addition to preexisting pores and flaws, a major barrier for bulk plastic deformation of polycrystalline ceramics lies in the grain boundaries (GBs), which can lead to dislocation pile‐up and cracking at the GBs due to the lack of sufficient independent slip systems in ceramics at room temperature. Here, we use the cyclic Brinell indentation method to circumvent the bulk deformation and focus on near‐surface regions to investigate the plastic deformation of polycrystalline SrTiO3 at room temperature. Dislocation etch‐pit analysis suggests that plastic deformation can be initiated within the grains, at the GBs, and from the GB triple junction pores. The deformability of the individual grains is found to be dependent on the number of cycles, as also independently evidenced on single‐crystal SrTiO3 with representative surface orientations (001), (011), and (111). We also identify a grain‐size‐dependent plastic deformation.

Strain softening observed during nanoindentation of equimolar-ratio Co–Mn– Fe–Cr–Ni high entropy alloy

This research article presents an atomistic study on the cyclic nanoindentation of an equimolar-ratio Co–Mn–Fe–Cr–Ni high-entropy alloy (HEA) using molecular dynamics simulation. The study investigated the effects of indentation depth on the cyclic load versus the indentation depth of the HEA. The results showed that the cyclic response exhibits a pronounced shift towards plasticity with pile-up formation instead of sinking behavior at higher indentation depths. Within the realm of molecular dynamics simulations, the simulated hardness value reached up to 16 GPa for the initial indentation cycle. A steep drop in the load–displacement curve was observed during the elastic–plastic transition, signifying substantial strain softening of the substrate. It was found that the densely clustered stacking faults undergo a reverse transition during cyclic loading, contributing to the backpropagation phase responsible for elastic recovery despite subsequent strain hardening. The study provides important insights into the underlying mechanisms governing the cyclic mechanical behavior of HEAs to guide their improved micromanufacturing.

Indentation fracture of 4H-SiC single crystal

Understanding the deformation and fracture behavior of single crystal silicon carbide (SiC) under a single particle is of scientific and practical importance for the micromachining of single crystal SiC. In this work, we investigate the indentation fracture of a 4H-SiC single crystal wafer with the indentation direction perpendicular to (0001) plane, using Berkovich, Vickers, and Knoop indenters. All the indentations create radial cracks for the normal loads used in this work. Both the Vickers and Knoop hardness tests produce lateral cracks. The fracture toughness calculated from the Vickers hardness tests is smaller than the ones calculated from the Knoop hardness tests and the Berkovich indentations under large indentation loads. The fracture toughness of 4H-SiC single crystal decreases with the increase of the indentation load under small indentation loads for the Berkovich indentations, revealing the phenomenon of surface hardening. The surface energy calculated from the radial cracks is comparable to the results reported in the literature. We establish an analytical expression of the total energy dissipation of a single indentation cycle, including the contribution of indentation-induced cracking, which offers an approach to calculate the ratio of the energy dissipation due to cracking to the energy dissipation due to plastic deformation and determine the dominant deformation process controlling the indentation deformation. The analysis of the energy dissipation for the indentations of the 4H-SiC single crystal by the Berkovich indenter reveals that the energy dissipation from the indentation-induced cracking is significantly larger than (more than eight times) that from plastic deformation for the indentation loads larger than 75 mN.

Damage and crack extension mechanism of hard and brittle materials induced by cyclic indentation

Damage and crack extension mechanism of hard and brittle materials induced by cyclic indentation

Inescapable foot shock induces a PTSD-like phenotype and negatively impacts adult murine bone.

Post-traumatic stress disorder (PTSD) is associated with osteopenia, osteoporosis and increased fracture risk in the clinical population. Yet, the development of preclinical models to study PTSD-induced bone loss remains limited. In this study, we present a previously unreported model of PTSD in adult female C57BL/6 mice, by employing inescapable foot shock and social isolation, that demonstrates high face and construct validity. A subset of mice exposed to this paradigm (i.e. PTSD mice) display long-term alterations in behavioral and inflammatory indices. Using three-dimensional morphometric calculations, cyclic reference point indentation (cRPI) testing and histological analyses, we find that PTSD mice exhibit loss of trabecular bone, altered bone material quality, and aberrant changes in bone tissue architecture and cellular activity. This adult murine model of PTSD exhibits clinically relevant changes in bone physiology and provides a valuable tool for investigating the cellular and molecular mechanisms underlying PTSD-induced bone loss.

Structural changes in a metallic glass under cyclic indentation

Using molecular dynamics simulation, a CuZr metallic glass was subjected to cyclic indentation to investigate cyclic hardening. Structural changes occurring after each indentation cycle were analyzed by examining the radial changes of the structural motifs in the vicinity of the indenter surface. The analysis revealed initial local structural modifications that corresponded to a more relaxed glass state, followed by a slow restoration of the initially destroyed structures. These findings provide new insights into the microstructural causes of cyclic hardening in metallic glasses.

Improvement of the mechanical performance of ZnAlMg coated steel brazed joints through precipitation-based strengthening

The non-fusion weld-brazing process has attracted considerable attention in the automotive industry due to its lower susceptibility to welding-related defects and high capability to join similar and dissimilar materials. However, the mechanical performance of the brazed joint is limited to the strength of the filler material, which restricts the widespread adoption of this technique in the automotive industry. The objective of the present study is to investigate a viable and effective solution for enhancing the local mechanical properties of the braze bead through the in-situ formation of precipitates during weld-brazing of ZnAlMg coated steel. The results showed that increasing heat input led to the dilution of molten filler material (i.e., CuSi3Mn alloy) by the steel substrate, resulting in the formation of a high number density of FeSi(Cu) precipitates with irregular morphologies within the braze bead. Analysis of cyclic load-depth indentation measurements within the braze bead revealed that the presence of FeSi(Cu) precipitates led to a considerable improvement of mechanical properties in the local region of the braze bead. Ultimately, this resulted in higher resistance of the braze bead to cracking as well as greater structural integrity when subjected to non-uniform deformation (such as rotation) during shear-tensile loading. The results also showed that the increased heat input led to optimized joint geometry and improved bonding of joint interfaces, further contributing to the improving mechanical properties of the joint. This study introduces a novel approach to the development of highly robust braze joints through the use of a precipitation-based strengthening mechanism. This approach offers an effective solution to extend the scope of the brazing process for joining high/ultra-high-strength materials used in the automotive industry.

Surface treatments and substrate-coating interface effects on damage accumulation kinetics in hard-coated WC-Co hardmetals under cyclic multi-axial high-temperature loading

Coated hardmetals are commonly used tool materials for metal cutting applications. For these applications, the substrate- and the coating surface qualities are improved by grinding, polishing, or blasting. The focus of the current work was to study the influence of different combinations of substrate-coating surface processing techniques on the induced damage in Al2O3/TiCN hard-coated WC-12 wt% hardmetal substrates and the depth to which the damage reaches into the substrate. The substrate and coating surfaces were prepared by grinding, polishing, dry blasting, wet blasting, or remaining in the deposited state. Investigations were performed using cyclic indentation with a novel ball-in-cone test method in a vacuum at 700 °C, under conditions that imitate the combined shear-compression loads that occur at the cutting edges of metal cutting tools. Additionally, finite element simulations were performed to characterize the stress state arising during ball-in-cone testing. The kinetics of defect formation and accumulation in the hardmetal substrate as a function of the loading situation during the ball-in-cone test will also be discussed. The defects that formed in the substrate during cyclic loading were studied using scanning electron microscopy in cross-sections prepared by focused ion beam milling. A larger increase in defect frequency was observed for rougher coating surfaces and substrate-coating interfaces than for smoother ones. Furthermore, 6 μm thick coatings exhibited a higher defect frequency after cyclic loading than 15 μm thick coatings. Most of the observed defects were in the nm-size range close to the substrate-coating interfaces and tended to have increased in size after cyclic loading. The ball-in-cone test set-up enables the study of the damage mechanisms in coated hardmetal substrates with different treatments prior to and after deposition under tunable milling-like stress and temperature conditions.

Hormonal and non-hormonal oral contraceptives given long-term to pubertal rats differently affect bone mass, quality and metabolism.

We investigated the effects of hormonal and non-hormonal oral contraceptives (OCs) on bone mass, mineralization, composition, mechanical properties, and metabolites in pubertal female SD rats. OCs were given for 3-, and 7 months at human equivalent doses. The combined hormonal contraceptive (CHC) was ethinyl estradiol and progestin, whereas the non-hormonal contraceptive (NHC) was ormeloxifene. MicroCT was used to assess bone microarchitecture and BMD. Bone formation and mineralization were assessed by static and dynamic histomorphometry. The 3-point bending test, nanoindentation, FTIR, and cyclic reference point indentation (cRPI) measured the changes in bone strength and material composition. Bone and serum metabolomes were studied to identify potential biomarkers of drug efficacy and safety and gain insight into the underlying mechanisms of action of the OCs. NHC increased bone mass in the femur metaphysis after 3 months, but the gain was lost after 7 months. After 7 months, both OCs decreased bone mass and deteriorated trabecular microarchitecture in the femur metaphysis and lumbar spine. Also, both OCs decreased the mineral: matrix ratio and increased the unmineralized matrix after 7 months. After 3 months, the OCs increased carbonate: phosphate and carbonate: amide I ratios, indicating a disordered hydroxyapatite crystal structure susceptible to resorption, but these changes mostly reversed after 7 months, indicating that the early changes contributed to demineralization at the later time. In the femur 3-point bending test, CHC reduced energy storage, resilience, and ultimate stress, indicating increased susceptibility to micro-damage and fracture, while NHC only decreased energy storage. In the cyclic loading test, both OCs decreased creep indentation distance, but CHC increased the average unloading slope, implying decreased microdamage risk and improved deformation resistance by the OCs. Thus, reduced bone mineralization by the OCs appears to affect bone mechanical properties under static loading, but not its cyclic loading ability. When compared to an age-matched control, after 7 months, CHC affected 24 metabolic pathways in bone and 9 in serum, whereas NHC altered 17 in bone and none in serum. 6 metabolites were common between the serum and bone of CHC rats, suggesting their potential as biomarkers of bone health in women taking CHC. Both OCs have adverse effects on various skeletal parameters, with CHC having a greater negative impact on bone strength.

Plasticity in cyclic indentation of a Cu-Zr-based bulk metallic glass after tensile loading: An experimental and molecular dynamics simulation study

In this study, we combined experiments and molecular dynamics simulations to investigate the deformation of metallic glasses subjected to previous tensile deformation. The experimental investigations were conducted on a Zr67Cu10.6Ni9.8Ti8.8Be3.8 (wt%) sample and the molecular dynamics simulations were performed on a Cu64.5Zr35.5 sample. Initially, plasticity was induced in the specimens by tensile deformation through the formation of shear bands, and we studied the further evolution of plasticity using cyclic indentation. We found that the macroscopic properties measured in experiments, such as hardness and hysteresis width, qualitatively agree with simulations. We use the molecular dynamics simulations to analyze the microscopic properties resulting from cyclic indentation and determine the polyhedral packing structures (‘motifs’) after tensile deformation in regions outside and around the shear bands. We then followed their evolution after each indentation cycle. Our findings indicate that areas outside the shear bands experience higher shear strain during cyclic indentation and that all motifs increased in fraction but evolved differently inside and outside the shear bands. The first indentation leads to the strongest change in microstructure, affecting both the material within and outside of shear bands. Repeated indentation mostly acts on the shear bands. These changes lead to a stabilization of the material in the sense that motifs with high coordination number and hence bond formation are established.

Wear and Subsurface Stress Evolution in a Half-Space under Cyclic Flat-Punch Indentation

Wear is a tremendously important phenomenon, which takes place on the surfaces of two solids in contact under cyclic loads and constitutes one of the most-significant ways of failure for mechanical elements. However, it is not the only source of failure in contacting solids. The subsurface stresses should also be considered, due to the fatigue and crack initiation problems. Nevertheless, these stresses (i.e., their maximum values and distributions) evolve with the solids’ surface wear (i.e., with the load cycles) and also depend on the friction intensity. Therefore, their evolution should be properly computed to predict failures in mechanical elements under wear conditions. This work focused on the study of the evolution of the surface wear and the subsurface stress distributions generated—in an elastic half-space—by a cylindrical flat-ended punch, under cyclic indentation loading (i.e., radial fretting wear conditions). Based on a numerical scheme recently presented by the authors, this is the first time that, for this contact problem, the surface wear and subsurface stress distribution (i.e., maximum value and its location)—and its evolution—were simultaneously analyzed when orthotropic friction and fretting wear conditions were considered. The studies presented in this work were developed for purely elastic contact assumptions.

A vitamin D deficient diet increases weight gain and compromises bone biomechanical properties without a reduction in BMD in adult female mice

Vitamin D contributes to the development and maintenance of bone. Evidence suggests vitamin D status can also alter energy balance and gut health. In young animals, vitamin D deficiency (VDD) negatively affects bone mineral density (BMD) and bone microarchitecture, and these effects may also occur due to chronic ethanol intake. However, evidence is limited in mature models, and addressing this was a goal of the current study. Seven-month-old female C57BL/6 mice (n = 40) were weight-matched and randomized to one of four ad libitum diets: control, alcohol (Alc), vitamin D deficient (0 IU/d), or Alc+VDD for 8 weeks. A purified (AIN-93) diet was provided with water or alcohol (10 %) ad libitum. Body weight and food intake were recorded weekly, and feces were collected at 0, 4, and 8 weeks. At the age of 9 months, intestinal permeability was assessed by oral gavage of fluorescein isothiocyanate–dextran. Thereafter, bone mineral density (BMD) was measured by dual-energy X-ray absorptiometry. The microarchitecture of the distal femur was assessed by micro-computed tomography and biomechanical properties were evaluated by cyclic reference point indentation. VDD did not affect BMD or most bone microarchitecture parameters, however, the polar moment of inertia (p < 0.05) was higher in the VDD groups compared to vitamin D sufficient groups. VDD mice also had lower whole bone water content (p < 0.05) and a greater average unloading slope (p < 0.01), and energy dissipated (p < 0.01), indicating the femur displayed a brittle phenotype. In addition, VDD caused a greater increase in energy intake (p < 0.05), weight gain (p < 0.05), and a trend for higher intestinal permeability (p = 0.08). The gut microbiota of the VDD group had a reduction in alpha diversity (p < 0.05) and a lower abundance of ASVs from Rikenellaceae, Clostridia_UCG-014, Oscillospiraceae, and Lachnospiraceae (p < 0.01). There was little to no effect of alcohol supplementation on outcomes. Overall, these findings suggest that vitamin D deficiency causes excess weight gain and reduces the biomechanical strength of the femur as indicated by the higher average unloading slope and energy dissipated without an effect on BMD in a mature murine model.

Towards understanding the mechanism of vibration-assisted cutting of monocrystalline silicon by cyclic nanoindentation

Ultrasonic vibration cutting (UVC) is a promising technology that can promote the processing of hard-brittle materials in ductile mode. The feature of intermittent cutting in UVC is considered to promote the ductile responses of brittle materials. However, the effect of cyclic loading/impact on microscopic deformation behavior of the workpiece material in UVC is not clearly understood. This study used cyclic nanoindentation to reveal the UVC mechanism in monocrystalline silicon (Si). The surface morphology and subsurface microstructure of the residual indents were characterized and compared with those of the UVC-machined grooves. This work attempted to correlate the tool-workpiece contacts for cyclic nanoindentation and vibration cutting. Cyclic nanoindentation results show that cyclic loading promotes the extent of silicon amorphization and decreases the threshold for transitioning the β–Sn phase to the bc8 and r8 phases. As the number of indentation cycles increases, the subsurface microstructure changes from the amorphous phase to the bc8 and r8 phases. In UVC, both the critical cutting depth for brittle-to-ductile transition and the degree of amorphization in cutting chips increase in comparison to conventional cutting, which matches the trend of cyclic nanoindentation results. The findings inform the chip formation and subsurface deformation mechanisms of brittle materials during UVC.

Investigation the temperature-dependent surface mechanical properties of PolyJet printed samples by cyclic indentation testing in a DMA system

Tools and products used in everyday life are regularly exposed to dynamic, cyclical stress. These stresses are particularly significant in the case of polymers, as their viscoelastic behavior means that creep can be considerable even at room temperature. Therefore, polymer components are often tested for maximum deformation rather than for maximum load-bearing capacity. Basic material testing methods are tensile, compression, and flexure tests, which are excellent for determining the material properties of the bulk material. However, in some cases, it is more appropriate to investigate surface mechanical properties. The ideal method for this is the depth-sensing indentation test. This method has been widely applied to polymers in the last ten years, but cyclic tests are rare, and creep is not considered in this type of indentation test. In the case of cyclical tests, temperature dependence is not fully examined, either. This paper presents the results of cyclic indentation tests on photopolymer specimens produced by additive manufacturing with the use of a dynamic mechanical analyzer with a unique indentation clamp. We performed the tests at three temperatures to investigate the influence of temperature on cyclic indentation tests. The test results show the variation of deformation between cycles and the significant effect of temperature.

Characterization of cyclic dynamic and creep responses of pure aluminum by instrumented indentation

<p indent="0mm">Dynamic behavior under cyclic loading conditions and creep behavior under quasi-static loading conditions were investigated by instrumented indentation of pure aluminum to reveal the influence of loading conditions (e.g., load, loading rate, and holding time) on indentation responses. The results of cyclic indentation show that, with the increase in the holding time, load, and loading rate of the pre-cyclic loading segment, the effect of creep on the subsequent cyclic indentation can be weakened, and the measured mechanical properties (e.g., contact depth, indentation hardness, and elastic modulus) can reach constant levels more rapidly with the increase in cycle number. The results of the creep tests show that the elastic modulus and indentation hardness decrease with the increase in holding time, the steady-state creep stress exponent obtained by instrumented indentation is independent of load, and a long holding time is not suggested for the creep tests. Indentation hardness and steady-state creep resistance measured within the inner grains are higher than those measured near the grain boundary regions.

Application of instrumented indentation technique in &amp;lt;italic&amp;gt;in situ&amp;lt;/italic&amp;gt; performance characterization of high-speed rail rim

<p indent="0mm">A purely experimental integrated algorithm for the industrial implementation of instrumented indentation technology has been established in the present study. This study proposes a multivariable iterative decoupling optimization algorithm to solve the best Hollomon constitutive model to estimate the indentation tensile properties by performing incremental cyclic indentation to take the measured maximum force, stiffness, and indentation depth of each unloading segment as the input. The Meyer power-law model is employed to improve the accuracy of the as-estimated yield strength. In addition, the critical indentation energy model is used to estimate the equivalent fracture toughness <italic>K</italic>_JC. Tensile fracture strain or elongation is used as a damage factor to calculate the critical effective indentation depth relative to the threshold of indentation cracking, which is required to obtain the necessary indentation energy for <italic>K</italic>_JC. Thereafter, the indentation tensile and toughness properties of typical high-speed rail rims were evaluated without sampling, consistent with relative results from regular standardized testing. Moreover, the distribution features of strength, hardness, yield strength ratio, and toughness, along with the depth from the surface to the inner substrate of rail rims, were studied quantitively based on the estimated indentation results. This gave a practical way for short-process nonsampling and <italic>in situ</italic> mechanical property evaluation with high-throughput results for such metallic materials or components as rail rims.