Indentation Size Effect Research Articles

Anisotropic Plastic Deformation Mechanism and Indentation Size Effect During Berkovich Nanoindentation Process of ZnSe Crystals in Micro-nanoscale

Anisotropic Plastic Deformation Mechanism and Indentation Size Effect During Berkovich Nanoindentation Process of ZnSe Crystals in Micro-nanoscale

A new nanoindentation approach for determining both indentation size effect and continuous apparent activation volume during loading of nanocrystalline Ni and Ni-20 wt.% Fe alloy

A new nanoindentation approach is developed in this study to determine both indentation size effect (ISE) and continuous apparent activation volume () during loading of nanocrystalline nickel (NC Ni) and nanocrystalline nickel-20 wt.% iron alloy (NC Ni-Fe alloy). This approach involves conducting nanoindentation tests under loading modes controlled by both constant strain rate (CSR) and constant loading rate (CLR). Firstly, a new empirical expression for the parameter in the modified Nix-Gao model is established to study the strain rate dependence of the ISEs created in the CSR and CLR tests. Then, continuous data of each individual sample (indentation) during loading are obtained in the CLR test through the alternative use of continuous stiffness measurement technique. The stress dependence of is analyzed based on Duhamel et al.’s model, which considers the role of vacancies generated during inhomogeneous dislocation nucleation. Finally, based on the above experimental and theoretical work as well as transmission electron microscopy observation, the influences of loading mode, loading rate, and material properties (stacking fault energy) on resulting intrinsic hardness of NC Ni and NC Ni-Fe alloy are analyzed. The nanoindentation approach developed in this study provides profound insights into the mechanical behaviors during loading and underlying mechanisms of materials.

New Insights in the Nanomechanical Study of Carbon-Containing Nanocomposite Materials Based on High-Density Polyethylene

The investigation of new composite materials possessing low weight but not at the expense of their mechanical performance is of great interest in terms of reducing energy consumption in many industrial applications. This study is focused on the nanomechanical characterization of high-density polyethylene (HDPE)-based composite specimens modified with equal loadings of graphene nanoplatelets (GNPs) and/or multiwall carbon nanotubes (MWCNTs). Quasi-static nanoindentation analysis revealed the impact of the carbon nanofillers on the receiving of nanocomposites with higher nanohardness and reduced modulus of elasticity, reaching values of 0.146 GPa and 3.57 GPa, respectively. The role of the indentation size effect in elastic polymer matrix was assessed by applying three distinct peak forces. Nanoscratch experiments depicted the tribological behavior of the composite samples and inferred the influence of the carbon nanofillers on the values of the coefficient of friction (COF). It seems that the incorporation of 4 wt% GNPs in the polymer structure improves the scratch resistance of the material, resulting in a higher value of the exerted lateral force and therefore leading to the detection of a higher coefficient of friction at scratch of 0.401. A considerable pile-up response of the scratched polymer specimens was observed by means of in-situ SPM imaging of the tested surface sample area. The sway of the carbon nanoparticles on the composite pile-up behavior and the effect of the pile-up on the measured friction coefficients have been explored.

The Influence of the Degree of Tension and Compression of Copper on the Indentation Size Effect (ISE)

The present work deals with the relationship between the degree of cold plastic deformation (up to 55.3% in the neck area in the tensile test and up to 66.6% in the compression test) and the parameters of the Indentation Size Effect (ISE). The tested material consists of 97% wrought copper. The Hanemann tester (Carl Zeiss, Jena, Germany) was used to measure micro-hardness. The loads applied during the micro-hardness test were between 0.09807 N and 0.9807 N. The influence of the load on the degree of the micro-hardness and simultaneously on the ISE, expressed by the Meyer’s index n, was significant. The influence of load on the ISE parameters was also evaluated using the Meyer’s index n, the PSR method, and the Hays–Kendall approach. For the undeformed sample, the Meyer’s index was close to 2, with the increase in the degree of tensile and compressive deformation increasing its “reverse” character (n > 2).

Comparison of the mechanical properties of Mo films by different nanoindentation techniques

Nanocrystalline Mo films were prepared by magnetron sputtering. Indentation size effect (ISE) on hardness (H) was both studied by constant strain rate method (CSR) and continuous stiffness method (CSM). Inverse ISE appears and H from CSR is higher than that from CSM. Significant dislocation motion barrier effect of increased grain boundary (GB) induces strengthening. Each step of CSM promotes the generation of heterogeneous GBs and enhances GB-emitting dislocations ability, leading to softening.

Synthesis, growth and nonlinear optical properties of imidazolium hydrogen adipate monohydrate single crystal

A single crystal of Imidazolium Hydrogen Adipate Monohydrate (IHAM) has been obtained by the slow evaporation technique. The grown crystal belongs to the Triclinic crystal system. The spectral studies were further used to confirm the structure. The Hirshfeld analysis suggests that the major bonding in the crystal occurs through the Hydrogen atom constituting 69 % of the total bonding. The Void analysis shows a lower percentage of voids suggesting that the crystal is strongly packed. The optical constants such as optical and electrical conductivity, optical susceptibility and extinction coefficient were elucidated from the UV–Vis-NIR analysis. The refractive index of IHAM was determined to be 1.391 by the Prism Coupler. The work-hardening coefficient of the title compound was found to be 1.14 which classifies the material as hard. The hardness number shows the normal Indentation Size Effect (ISE). The electrical characteristics were studied by using the dielectric analyser. The solid-state parameters such as the Fermi gap, Penn gap and optical electronegativity were calculated based on the dielectric parameters. The electronic polarizability calculated by different methods is in mutual agreement. The TG/DTA analysis suggests that the material is suitable for applications up to 79 °C. The Z-Scan analysis confirms the Reverse Saturable Absorption behaviour. The third-order nonlinear susceptibility was calculated as 9.77×10−9 esu.

A comparative study on nanoscale mechanical properties of CrMnFeCoNi high-entropy alloys fabricated by casting and additive manufacturing

Additive manufacturing (AM) has emerged as a pioneering method for fabricating high entropy alloys (HEAs), yet a comprehensive comparison of their nanoscale mechanical properties with those produced by the conventional casting method remains unexplored. In this study, the nanoindentation was utilized to investigate the nanoscale elastic and plastic characteristics in both additive-manufactured (AM-ed) and as-casted single-phase face-centered cubic (FCC) equiatomic CrMnFeCoNi HEAs. Herein, the hardness, reduced modulus, indentation size effect (ISE), yield strength, fracture toughness, and strain rate sensitivity were comprehensively investigated. The results indicated that the hardness of AM-ed HEA was higher than the as-casted HEA, and the reduced modulus values showed no notable distinction between the two samples. The AM-ed HEA demonstrated simultaneous enhancements in yield strength and fracture toughness compared to the as-casted HEA. The as-casted HEA possessed a more distinct indentation size effect (ISE) than the AM-ed HEA. It was observed that the AM-ed HEA exhibited relatively lower strain rate sensitivity and a larger activation volume. This direct comparison of the mechanical properties and deformation mechanisms from a nanoscale view offers unique insights for optimizing and advancing AM techniques in the fabrication of HEAs.

Mechanical Properties of Silicon Nitride in Different Morphologies: In Situ Experimental Analysis of Bulk and Whisker Structures.

Silicon nitride (Si3N4) is widely used in structural ceramics and advanced manufacturing due to its excellent mechanical properties and high-temperature stability. These applications always involve deformation under mechanical loads, necessitating a thorough understanding of their mechanical behavior and performance under load. However, the mechanical properties of Si3N4, particularly at the micro- and nanoscale, are not well understood. This study systematically investigated the mechanical properties of bulk Si3N4 and Si3N4 whiskers using in situ SEM indentation and uniaxial tensile strategies. First, nanoindentation tests on bulk Si3N4 at different contact depths ranging from 125 to 450 nm showed significant indentation size effect on modulus and hardness, presumably attributed to the strain gradient plasticity theory. Subsequently, in situ uniaxial tensile tests were performed on Si3N4 whiskers synthesized with two different sintering aids, MgSiN2 and Y2O3. The results indicated that whiskers sintered with Y2O3 exhibited higher modulus and strength compared to those sintered with MgSiN2. This work provides a deeper understanding of the mechanical behavior of Si3N4 at the micro- and nanoscale and offers guidance for the design of high-performance Si3N4 ceramic whiskers.

Reveal of relationship between microscopy architecture and mechanical performance of Y/Bi substituted Bi-2212 engineering ceramics.

This study aims to find out how the crystallinity quality, surface morphology, and mechanical performances change with the substitution of yttrium (Y) for bismuth (Bi) impurity within molar ratios of 0.00 ≤ x ≤ 0.12 in the Bi2.0-xYxSr2.0Ca1.1Cu2.0Oy (Bi-2212) cuprates to reveal the dependence of micro surface topology on the substitution mechanism and achieve a strong relation between the impurity ions and crystallization mechanism. The materials are prepared by ceramic method. It is found that all the experimental findings improve remarkably with increasing yttrium impurity molar ratio of x = 0.01. Scanning electron microscopy (SEM) images indicate that the optimum Y ions strengthen the formation of flaky adjacent stacked layers due to the changes of thermal expansion, vibration amplitude of atoms, heat capacitance, reaction kinetics, activation energy, nucleation temperature, thermodynamic stability, and intermolecular forces. Besides, new engineering novel compound produced by optimum Y ions presents the best crystallinity quality, uniform surface view, greatest coupling interaction between grains, largest particle size distributions/orientations, and densest/smoothest surface morphology. Hardness measurement results totally support the surface morphology view. Moreover, mechanical design properties and durability of the tetragonal phase improve significantly with increasing replacement level of x = 0.01 due to the induction of new surface residual compressive stress areas, slip systems, and chemical bonding between the foreign and host atoms. Besides, the same sample exhibits the maximum strength and minimum sensitivity to loads depending on reduction of stored internal strain energy and degree of granularity. Consequently, cracks tend to propagate predominantly within the transcrystalline regions. Furthermore, each material investigated exhibits the characteristic behavior of the indentation size effect. In summary, the optimum Y-doped Bi-2212 sample paves the way for the expanded use of engineering ceramics across various applications based on the enhanced service life. RESEARCH HIGHLIGHTS: The presence of the optimum yttrium impurity significantly decreases the Ea value. As the Y/Bi replacement increases up to the molar substitution level of x = 0.01, the mechanical design properties and durability of the tetragonal phase enhance significantly.

A comparative study of indentation size effect models for different materials

The phenomenon of indentation size effect (ISE) has received great attention in aerospace, nuclear power, microelectronics and medicine. Although researchers have proposed various ISE models, these models often involve different form and number of parameters that can make our wonder which is the best in existed ISE models. Herein, three types of ISE test data, namely, normal ISE, reverse ISE and transition of normal to reverse ISE, are used to evaluate the sixteen ISE models. The comparatively study indicates that Hou-Jennet(H-J), Nix-Gao-Feng (N-G-Fs), Nix-Gao-Haušild (N-G-H), Nix–Gao-Abu Al-Rub (N-G-A) and Nix–Gao-Qius (N-G-Qs) models can accurately predict the normal ISE. The reason for this is that the friction stress that is not related to dislocation activities or the indentation size effect of plastic zone has been introduced into these models. Therefore, these two factors should be considered in future ISE models. The sixteen ISE models are originally proposed to describe the normal ISE of different materials. However, to our surprise, some of these models are able to capture the reverse ISE and the transition of normal to reverse ISE of different materials. The determination coefficients (DC) of the sixteen ISE models are also determined for different materials. For reverse ISE, the highest DC value for Ni Carbide Silicon (NiCSi), TC4 titanium alloy (TC4) and Pulsed electro-deposited Ni (PED Ni) are given by the Exponential (EXP), Nix-Gao-Feng (N-G-Fs) and Nix–Gao-Abu Al-Rub (N-G-A) models, respectively. For the transition of normal to reverse ISE, the Nix–Gao-Yuan-Chen (N-G-YC), Nix-Gao-Feng (N-G-Fs), and Nix-Gao-Haušild (N-G-H) models produce the maximum DC for ZrO2 ceramic (ZrO2), Cu single crystals (Cu) and Y2O3–ZrO2 ceramic (Y2O3–ZrO2), respectively. Moreover, the mean DC of the Nix-Gao-Feng (N-G-Fs) model is the maximum among the sixteen ISE models, followed by the Nix-Gao-Haušild (N-G-H) model, but they cannot accurately predict the reverse ISE. Therefore, the Nix-Gao-Feng (N-G-Fs) and Nix-Gao-Haušild (N-G-H) models should be further modified to accurately predict the reverse ISE.

Ultra-high hard and fracture-resistant multi-phase nanocrystalline AlCrFeMoNbNi multi-principal element alloy

Multi-phase nanocrystalline AlCrFeMoNbNi multi-principal element alloy was developed using mechanical alloying followed by spark plasma sintering. Mechanical alloying resulted in a two-phase microstructure (BCC and FCC), whereas subsequent sintering resulted in a multi-phase microstructure consisting of FCC, Rhombohedral and B2 phases. Extremely high hardness values in the range of 35.79–16.05 GPa were measured as a function of indentation load between 25 and 5000 g. A highly pronounced indentation size effect was observed. From classic Nix-Gao analysis, a load independent hardness of 13.82 GPa was estimated. The high hardness arises from a combination of finer grain size and solid solution strengthening (FCC phase) and multi-phase structure consisting of B2 and Rhombohedral phases. The major phase being FCC (83%) offers nearly 85% of the total flow stress realized for this MPEA and the remaining 15% of the flow stress must be arising from both the B2 and Rhombohedral phases. It is to be noted that the phase fractions of B2 and Rhombohedral phases are 10% and 7% respectively. Indentation fracture toughness, evaluated using the cracks developed during Vickers indentation, yielded encouraging numbers in the range 12.28–13.85 MPam. The excellent combination of ultra-high hardness and indentation fracture toughness of this AlCrFeMoNbNi MPEA surpasses the reported data on several related harder materials, including silicides, nitrides, carbides, etc.

Exploring the Effect of Aluminium Solute Atoms on Nanomechanical Properties of Copper‐Aluminium System using Nanoindentation

In this work, nanomechanical properties for Cu and Cu–Al (where Al = 2, 4, 6, and 8 wt%) alloys are determined using nanoindentation with Berkovich tip. Nanoindentation experiments are performed using trapezoidal load function where maximum load (Pm) varies from 1000 to 9000 μN at an equal interval of 1000 μN by maintaining equal loading and unloading rate. It is found that Cu8Al sample shows lower depth of penetration (h) at any load (P) in comparison to other samples due to more pinning of dislocations or hinderance of the dislocation movement by solute (Al) atoms during nanoindentation deformation. In addition, it is observed that the recovery is maximum for Cu8Al sample among all samples; however, this recovery is reducing with the increasing Pm for all samples. Thereafter, the elasticity and plasticity index are calculated from the area under the P–h curves, which shows that the elastic index is maximum for Cu8Al and minimum for Cu. Furthermore, the nanomechanical properties (reduced elastic modulus [Er] and hardness [H]) are reported for all samples and significant indentation size effect is observed for Cu8Al due to dislocation structure during deformation.

An efficient way to grow large size single crystal of imidazole by modified Czochralski technique and study of its optical and mechanical properties

Large-sized single crystal of imidazole was successfully grown for the first time by cost-effective modified Czochralski technique for lower melting point materials. Its monoclinic crystal system and cell parameters a = 7.7251 Å, b = 5.4450 Å, c = 9.2599 Å, and β = 110.556° were determined through single crystal and powder XRD analysis. Hisrshfeld surface analysis and 2D fingerprint plot of imidazole revealed that H···H, C···H/H···C and H···N/N···H has 49.7 %, 18.7 % and 28.9 % of overall intermolecular interactions present in the crystal. Direct band gap nature, high transmittance and lower absorption cutoff at 236 nm was found in UV–Vis spectroscopy. Thermal studies of the crystal were carried out using TGA and DSC analysis and sharp endothermic peak showed high crystallinity and thermal stability up to its melting point. Fundamental functional groups of the crystals were identified by FTIR technique. Mechanical strength of imidazole single crystal was analyzed by Vickers microhardness at different loads, and it was observed that after 20 g load crystals showed indentation size effect.

An improved approach to decouple the indentation size effect from nanoindentation hardness of ion-irradiated samples

An improved approach to decouple the indentation size effect from nanoindentation hardness of ion-irradiated samples

Unusual indentation depth dependent hardness and creep behaviors in NbMoTaW films at the nanoscale

Herein, nanocrystalline NbMoTaW and (NbMoTaW)N thin films were prepared via magnetron sputtering and investigated using nanoindentation creep tests at various indentation loads (P). The hardness (H) of films increases with P, exhibiting an abnormal indentation size effect (ISE). At the same time, with decreasing indentation depth (h), the creep rate and the creep rate sensitivity (m) both increase. Under a critical h (hc) for each film, m sharply increases. The diffusion between the indenter/film interface dominates the creep mechanism at h lower than hc, whereas the dislocation–grain boundary interaction dominates the creep deformation at h higher than hc. The coble creep and lattice diffusion were both excluded as the main deformation mechanism. The escape of screw dislocations to the surface leads to the softening of the film, whereas the pile-up of screw dislocations leads to hardening, explaining the abnormal ISE on H. The effect of residual stress, grain boundary structures, substrate, and impurities are also discussed.

Indentation response of multi-phase nanocrystalline NbWTi refractory multi-principal element alloy

NbWTi refractory multi-principal element alloy has been synthesized using powder metallurgy route. 40 h of mechanical alloying resulted in a single-phase alloy and subsequent spark plasma sintering transformed it into a multi-phase structure (1 BCC and 2 FCC phases). The alloy demonstrated an extremely high hardness of 12.29 ± 0.05 GPa at a load of 1000 g, along with excellent “density-normalized” hardness and indentation size effect. An indentation fracture toughness of 6.81 ± 0.16 MPa.m1/2 was measured using the cracks generated. Ultra-high absolute hardness, high “density-normalized” hardness and associated fracture toughness signifies the potential of this alloy for next generation structural engineering applications.

Densification, microstructure, mechanical, and thermionic properties of spark plasma sintered LaB6–HfB2 composite

AbstractLaB6–HfB2 composites with the different HfB2 contents (10 wt.%, 30 wt.%, 50 wt.%, 70 wt.%, and 90 wt.%) were densified by spark plasma sintering (SPS). Results showed that the densification mechanism of the composite transformed from the grain boundary diffusion into the dislocation climbing mechanism as the holding time was extended from 0 to 15 min under temperature range of 1750–1900°C. The HfB2 phase could effectively limit the grain growth of LaB6 phase, and the dynamic growth of the grain was governed by grain boundary diffusion. Both the Berkovich hardness and Vickers hardness obeyed the normal indentation size effect. LaB6–70 wt.% HfB2 composite had the highest fracture toughness of 3.98 ± .43 MPa m.5, whereas the highest current density of 18.34 A/cm2 belonged to LaB6–30 wt.% HfB2 composite. All the results demonstrated that LaB6–HfB2 composite was a promising material with the excellent structural and functional performance.

On the promotion of serrated flows and shear band behaviors in a Zr-based metallic glass during ultrasonic vibration nanoindentation

Initiation and evolution of flow units and their correlation with mechanical behaviors of metallic glasses (MGs) are well known significant for understanding the rheological behavior of glassy substances. Here, the evolution of plastic deformation behavior of a typical Zr-based MG induced by ultrasonic vibration is investigated by means of nanoindentation, especially focusing on studying structural evolution through analysis of load-displacement curves. Furthermore, the micro-morphologies of residual indentations are characterized by using the scanning electron microscope (SEM) and atomic force microscope (AFM). Compared to quasi-static nanoindentation tests, a significant reduction in the hardness and elastic modulus of the MG by about 15 % and 30 %, respectively, is observed when subjected to ultrasonic vibration nanoindentation with an amplitude of 0.4 μm, accompanied by a pronounced indentation size effect. In addition, higher ultrasonic vibration amplitude induces larger indentation depth, more pronounced serrated flows in the load-displacement curves and more remarkable shear bands around the residual indentations, indicating ultrasonic vibration-promoted plastic flows in MG. This study provides an insight into the structural origin of plastic flows in MG systems under ultrasonic vibration, which will help to facilitate their application in the fields such as ultrasonic vibration assisted forming.

Diisopropylammonium hydrogen squarate: Synthesis and comprehensive analysis of non-linear optical co-crystal using X-ray, Hirshfeld, mechanical, optical and DFT methods

This research successfully synthesized a single co-crystal of diisopropylammonium hydrogen squarate using prolonged vaporization for crystal growth. Single-crystal X-ray spectrometry confirmed its monoclinic structure, and morphological predictions were made. UV–visible spectroscopy revealed its optical transmittance with a direct optical energy band gap of 3.45 eV. Photoluminescence studies showed a strong violet emission at 402 nm when excited by a 260 nm source. Microhardness study examined the crystal's mechanical attributes portraying the normal indentation size effect followed by a qualitative overview of half-penny crack dynamics. FTIR study aided in the discernment of varied vibrational modes with NH stretching being observed at 3078 cm−1. Thermal examination further revealed the crystal's stability up till 244 °C. Proton and carbon-13 NMR spectra were analyzed to verify the presence of functional groups and the overall molecular integrity. Intermolecular interactions were analyzed using Hirshfeld surface and fingerprint mapping. The Z-scan technique demonstrated the crystal's applicative potential in its third harmonic generation capability. Theoretical calculations with Density Functional Theory (DFT) supported the experimental findings, offering insights into optimized geometries, frontier molecular orbitals, natural population and bond orbital distributions, hyperpolarizability, molecular electrostatic potentials, IR vibrational modes, and UV absorbance profiles.

Nanoindentation Test of Ion-Irradiated Materials: Issues, Modeling and Challenges.

Exposure of metals to neutron irradiation results in an increase in the yield strength and a significant loss of ductility. Irradiation hardening is also closely related to the fracture toughness temperature shift or the ductile-to-brittle transition temperature (DBTT) shift in alloys with a body-centered cubic (bcc) crystal structure. Ion irradiation is an indispensable tool in the study of the radiation effects of materials for nuclear energy systems. Due to the shallow damage depth in ion-irradiated materials, the nanoindentation test is the most commonly used method for characterizing the changes in mechanical properties after ion irradiation. Issues that affect the analysis of irradiation hardening may arise due to changes in the surface morphology and mechanical properties, as well as the inherent complexities in nanoscale indentation. These issues, including changes in surface roughness, carbon contamination, the pile-up effect, and the indentation size effect, with corresponding measures, were reviewed. Modeling using the crystal plasticity finite element method of the nanoindentation of ion-irradiated materials was also reviewed. The challenges in extending the nanoindentation test to high temperatures and to multiscale simulation were addressed.