Nanoindentation Tests Research Articles

Isoporous Membranes by the Symmetric Triblock Copolymer: A Strategy to Improve the Mechanical Strength without Sharply Changing the Pore Size and Permselectivity.

Isoporous membranes produced from diblock copolymers commonly display a poor mechanical property that shows many negative impacts on their separation application. It is theoretically predicted that dense films produced from symmetric triblock copolymers show much stronger mechanical properties than those of homologous diblock copolymers. However, to the best of our knowledge, symmetric triblock copolymers have rarely been fabricated into isoporous membranes before, and a full understanding of separation as well as mechanical properties of membranes prepared from triblock copolymers and homologous diblock copolymers has not been conducted, either. In this work, a cleavable symmetric triblock copolymer with polystyrene as the side block and poly(4-vinylpyridine) (P4VP) as the middle block was synthesized and designed by the RAFT polymerization using the symmetric chain transfer agent, which located at the center of polymer chains and could be removed to produce homologous diblock copolymers with half-length while having the same composition as that found in triblock copolymers. The self-assembly of these two copolymers in thin films and casting solutions was first investigated, observing that they displayed similar self-organized structures under these two conditions. When fabricated into isoporous membranes, they showed similar pore sizes (5-7% difference) and comparable rejection performance (∼10% difference). However, isoporous membranes produced from triblock copolymers showed significantly improved mechanical strength and higher toughness (2-10 times larger) as evidenced by the compacting resistance, strain-stress determination, and nanoindentation testing, suggesting the unique and novel structure-performance relationship in the isoporous membranes produced from symmetric triblock copolymers. The above finding will guide the way to fabricate mechanically robust isoporous membranes without notably changing the separation performance from rarely used symmetric triblock copolymers, which can be synthesized by the controlled polymerization as facilely as that found for diblock copolymers.

Nanomechanical and microstructural properties of experimental bilayered zirconia ceramics after hydrothermal aging

Two experimental ceramic systems, 3Y-TZP/5Y-PSZ (3Y/5Y) and 4Y-PSZ/5Y-PSZ (4Y/5Y), underwent analysis before (3Y/5Yi or 4Y/5Yi) and after hydrothermal aging (3Y/5Ya or 4Y/5Ya) to simulate low-temperature degradation (LTD). The samples were sintered and characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman spectroscopy, alongside nanoindentation tests to measure elastic modulus (Em) and hardness (H). Assessments were conducted on the external surfaces and at individual layers on cross-sectioned samples at predetermined regions of interest (ROIs). Degraded superficial regions were observed in the cross-sectional SEM images of the 3Y and 4Y zirconia layers after aging. XRD indicated a tetragonal→monoclinic phase transformation in the aged groups for both 3Y (66 % m-ZrO2) and 4Y (29 % m-ZrO2). Raman spectroscopy revealed monoclinic phase amounts of 86 % for 3Y and 62 % for 4Y in the degradation regions observed in the SEM micrographs. Monoclinic phase peaks were virtually no longer detected in either material beyond a depth of 15 μm. Hydrothermal aging significantly diminished the H and Em values for the 3Y and 4Y zirconia surfaces. For the analysis of different zirconia surfaces within the same subgroup, all pairwise comparisons showed statistically significant differences, except for the values of H of 3Y/5Yi and Em for 4Y/5Yi. Regarding the nanoindentation results of cross-sectioned samples, the aging protocol did not affect the H and Em values of the equivalent ROIs (layers), regardless of the bilayered system. However, significant differences in H values were observed among the ROIs (layers) within the same bilayered system. Despite surface changes, nanomechanical properties remained preserved below the surface and at the interfaces of bilayered materials after aging. Nanoscale H values varied among some layers and interfaces, whereas the Em values exhibited differences across certain surfaces.

Evaluating mechanical and biological responses of bipolymeric drug-chitosan-hydroxyapatite scaffold for wounds: Fabrication, characterization, and finite element analysis

This study aims to explore the potential of a scaffold composed of drug-chitosan-hydroxyapatite (HA) in improving tissue treatment. The focus of the investigation lies in analyzing the physical and biological properties of the scaffold and evaluating its mechanical characteristics through finite-element analysis. To synthesize microcapsules containing dextran-diclofenac sodium, the electrospraying method was employed. The drug-chitosan-HA scaffold with varying volume fractions (VF) of the synthesized microcapsules (10, 15, and 20) was fabricated using the freeze-drying technique. Microscopic and scanning electron microscopy (SEM) images were utilized to evaluate the morphology, shape, and size of the microcapsules, as well as the porosity of the scaffolds for wound healing purposes. The mechanical properties of the synthesized microcapsules were determined via a nanoindentation test, while the mechanical behavior of the fabricated scaffolds was assessed through compression testing. Additionally, a multiscale finite-element model was developed to predict the mechanical properties of tissue scaffolds containing pharmaceutical microcapsules. The findings indicate that the incorporation of drug-chitosan-hydroxyapatite into the tissue significantly enhances both mechanical and biological responses. The mechanical evaluations demonstrate that the drug-chitosan-hydroxyapatite tissue exhibits excellent resistance to pressure, making it a suitable protective covering for skin wounds. Moreover, biological evaluations reveal that an increase in scaffold porosity leads to higher swelling behavior. The scaffold containing 20 % pharmaceutical microcapsules demonstrated the greatest swelling and desirable antibacterial properties, thereby indicating its potential as an effective wound dressing. Furthermore, a multiscale finite-element model was developed to predict the mechanical properties of tissue containing pharmaceutical microcapsules. The results indicated that the average size of the microcapsules was in the range of 170 to 180 µm, and the porosity of the prepared tissue was between 52 % and 61 %. The experimental compressive properties revealed that an increase in the volume fraction of the embedded microcapsules led to an increase in the maximum compressive stress and compressive modulus of the scaffolds by up to 54.95 % and 53.18 %, respectively, for the scaffold containing 20 % VF of pharmaceutical microcapsules compared to the specimen containing 10 % VF. In conclusion, the developed scaffold has the potential to serve as an effective wound dressing, with the ability to provide structural support, facilitate controlled drug release, and promote wound healing.

Micromechanical variation of organic matter (kerogen type I) under controlled thermal maturity progression

Shale formations have recently gained plenty of attention owing to their large amounts of reserves. Horizontal drilling and hydraulic fracturing are the proposed approaches for the development of shale formations. The extended information of the mechanical properties of shale formation is crucial for designing a successful hydraulic fracturing operation. On the other hand, the mechanical properties of such organic-rich formations are greatly affected by the mechanical characteristics of the present kerogen (organic matter), which dramatically changes during the maturation process. In this study, a Qingshankou shale sample containing kerogen type I is mechanically investigated at different maturity levels using the grid nanoindentation approach. To this end, the original immature sample is artificially matured during hydrous (HP) and anhydrous (AHP) pyrolysis. More than 930 nanoindentation tests were performed on grids of 9 × 8 on the surface of 13 samples with different maturities. The test results showed that the presence of water during pyrolysis can significantly affect the shale sample’s mechanical characteristics. In higher temperatures and higher levels of maturity, the role of water becomes more pronounced. During hydrous pyrolysis, kerogen produces larger amounts of oil and bitumen, which become progressively porous. While the original sample showed a Young’s modulus value of more than 48 GPa, and it fluctuated between approximately 19 and 32 GPa during the HP scenario and between 17 and 34 GPa during the AHP process. In terms of hardness, the original sample exhibited an initial value of about 1.1 GPa and more mature samples reflected hardness values in the range of approximately 0.3 and 0.97 GPa in both scenarios. According to the trends of mechanical properties during maturation, mechanical properties decreased at the initial stage of maturation and remained relatively constant during the oil window. Then, another decline was detected at the wet-gas window’s closure. In the dry-gas window, HP and AHP scenarios exhibited different behaviors mainly due to the chemical structure of the kerogen residue.

Comparative evaluation on surface nanohardness, surface microhardness, surface roughness, and wettability of plant-based organic nanoparticle reinforced polyetheretherketone as an implant material - An in vitro study.

Synthetic inorganic materials are commonly used as reinforcing agents in polyetheretherketone (PEEK) composite, whereas natural organic plant-based reinforcing agents are negligible. Surface hardness, roughness, and wettability are indicative factors of osseointegration behavior to be used as an implant material. This study evaluated micro surface hardness (MSH), nano surface hardness (NSH), surface roughness (SR), and contact angle (CA) of PEEK-Azadirachta indica reinforced at 10 wt%, 20 wt%, and 30 wt%. This was an in vitro study. Neem (A. indica) leaf nanoparticles were prepared and reinforced with PEEK powder at 10%, 20%, and 30% weight ratios by injection molding. Sixty specimens underwent the microhardness and CA testing using a digital microhardness tester, and CA goniometer, respectively, and later nanoindentation test to analyze the nanohardness and SR. A one-way ANOVA test with a 95% confidence interval for MSH and NSH, SR, and CA was performed on the samples. A post hoc Bonferroni test was conducted (α = 0.05) to compare the groups. There was a significant increase in nanohardness (P = 0.000) with zero difference in microhardness (P = 0.514). The addition of 10 wt%, 20 wt%, and 30 wt% nanoparticles increased the SR value of the pure PEEK from 273.19 nm to 284.10 (3.99%), 296.91 (8.68%), and 287.54 (5.24%), respectively. In the analysis of the CA, CA 20% shows the lowest angle (63.69) with the highest for control specimens (82.39). There is an increase in the PEEK composite SR with a decrease in CA. The addition of plant-derived nanoparticles into the PEEK matrix has a significant impact on the hardness and hydrophobicity enhancing cell growth and osteoblastic differentiation during osseointegration of dental implants.

Characterization of a hydrothermally aged experimental alumina-toughened zirconia composite

ObjectivesTo assess the effects of different aging protocols on chemical, physical, and mechanical properties of an experimental ATZ composite compared to a zirconia. MethodsDisc-shaped specimens were obtained through uniaxial pressing of commercial powders (Tosoh), ATZ comprised of 80%ZrO2/20%Al2O3 (TZ-3YS20AB) and 3Y-TZP (3Y-SBE). The specimens of each material were divided into different groups according to the aging protocol: immediate, autoclave aging and hydrothermal reactor aging. The aging protocols were performed at 134 ºC for 20 h at 2.2 bar. Crystalline evaluations were performed using X-Ray Diffraction. The nanoindentation tests measured the elastic modulus (Em) and hardness (H). Biaxial flexural strength was performed, and Weibull statistics were used to determine the characteristic strength and Weibull modulus. The probability of survival was also determined. The Em and H data were analyzed by one-way ANOVA and Tukey test. ResultsDiffractograms revealed the presence of monoclinic phase in both materials after aging. The hydrothermal reactor decreased the Em for ATZ compared to its immediate condition; and the H for both ATZ and 3Y-TZP regarding their immediate and autoclave aging conditions, respectively. The aging protocols significantly increased the characteristic strength for ATZ, while decreased for 3Y-TZP. No difference regarding Weibull modulus was observed, except for 3Y-TZP aged in reactor. For missions of up to 500 MPa, both materials presented a high probability of survival (>99 %) irrespective of aging condition. SignificanceThe synthesized ATZ composite exhibited greater physical and microstructural stability compared to 3Y-TZP, supporting potential application of the experimental material for long-span reconstructive applications.

Microstructure, mechanical properties, and wettability of CrN and CrSiCN coatings with graded architectures

Protective CrN-based coatings are of interest for applications requiring a combination of corrosion resistance and toughness. Here, the processing-microstructure-properties relationships for metallic Cr, binary CrN, and quaternary CrSiCN coatings are reported. Hexamethyldisilazane (HMDS) was used as a single-source organosilicon precursor for Si and C during plasma-enhanced magnetron sputtering (PEMS). By varying the availability of reactive species during coating growth, graded coating architectures were produced. Scanning and transmission electron microscopy revealed that as Si and C content increased, the coating microstructure evolved from a coarse, columnar growth structure (0 at.% Si), to a nanocolumnar structure (3 at.% Si), and, finally, to a dense, nanoscale structure (6 at.% Si). Coating surface topography was characterized using optical microscopy and atomic force microscopy. While the CrSiCN coating deposited at the highest HMDS flow rate exhibited the lowest nanoscale surface roughness (Rq = 6.74 nm), it also had the greatest area fraction of microscopic surface defects. Evidence of the formation of secondary Cr2N phases within the graded interlayers of the coatings was acquired from selected area electron diffraction analysis. However, the practical adhesion of the coatings, as evaluated by the Rockwell C indentation test, was not adversely affected. Nanoindentation testing revealed that greater incorporation of Si and C into the CrN-based coatings increased coating hardness from 25.4 ± 1.6 GPa to 30.7 ± 1.8 GPa and decreased apparent elastic modulus from 295 ± 14 GPa to 284 ± 12 GPa. Contact angle goniometry was conducted to determine the wettability of the coatings. It was found that sessile water contact angles decreased from 86.5° ± 1.6° to 77.3° ± 2.1° as coating Si and C content increased.

Mechanical property of intermetallic compounds in Zn–Al solder interconnects by nanoindentation and first-principles calculations

Presently, interfacial intermetallic compounds play a vital role in determining the reliability of solder joints due to their intrinsic mechanical property. Especially for Zn–Al solder joints, the interfacial Cu–Zn IMCs grow significantly without diffusion barriers. This work comprehensively investigated the mechanical properties of interfacial IMCs in Zn–Al solder joints with and without the Ni–W–P diffusion barrier by nanoindentation tests and first-principles calculations. The nanoindentation results show that the elastic moduli of CuZn4, Cu5Zn8, CuZn and Al3Ni2 were 68.45 ± 1.4 GPa, 142.6 ± 2.3 GPa, 94.7 ± 1.16 GPa, and 221 ± 18.9 GPa, respectively. Their corresponding hardness were 1.03 ± 0.04 GPa, 5.98 ± 0.23 GPa, 1.38 ± 0.16 GPa, and 17.7 ± 0.16 GPa. Through first-principles calculations, the bulk modulus of CuZn and Cu5Zn8 exhibits isotropic behaviour, while CuZn4 and Al3Ni2 demonstrate anisotropy. In addition, the bulk modulus, shear modulus, Young's modulus and hardness values of Al3Ni2 are considerably higher when compared to those of Cu–Zn intermetallic compounds.

Microstructures and tribological properties of MoS2/Mo2N multilayer gradient films deposited by reactive magnetron sputtering

In order to compare the microstructures and tribological properties of films, pure Mo2N, pure MoS2, 3-layer and 13-layer MoS2/Mo2N gradient films were deposited by reactive magnetron sputtering. The crystalline structure, surface and cross-section morphologies, 3D surface topography, binding energy, hardness and tribological properties of films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), atom force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), nanoindenter, and wear tester, respectively. The results indicate that the preferred orientation of MoS2 in gradient films has changed. The surface and cross-section structures of gradient films become denser with increasing the number of gradient layers. Average surface roughness (Ra) of pure MoS2 film is the highest, and Ra of 13-layer film is the lowest. The binding energy of MoS2 in the composite layer of gradient film has changed. The hardness of gradient film is higher than that of MoS2 and lower than that of Mo2N. The wear resistance of gradient films is much better than that of pure MoS2, and this phenomenon is more obvious under high load conditions. The improvement in the wear resistance of gradient films is attributed to the increase of dense, hardness, H/E and H3/E2. In the initial stage of friction, the 3-layer gradient film can maintain low friction coefficient (≤0.15), which is attributed to the thick MoS2 surface layer. The wear resistance of 13-layer is much better than that of 3-layer gradient film, because it has higher hardness, higher H/E and H3/E2 than 3-layer gradient film.

Effects of post-deposition annealing on structure and mechanical properties of multilayer Ti/DLC films

The multilayer (Ti/DLC) × 3 films were deposited using a DC arc evaporator with a titanium cathode and a pulsed cathode-spark evaporator with a graphite cathode. Following the deposition of the films, a heat treatment process was performed in air and Ar atmosphere at temperatures of 200 °C and 400 °C. The investigation of the films involved the examination of their structure, surface morphology, and chemical composition using AFM, SEM, XPS and Raman. Additionally, the mechanical properties of the films were assessed by nanoindentation, sclerometry and wear test. Changes in the structure, RMS roughness, С-sp2/С-sp3 ratio of carbon atoms in the film and the formation of Ti-C carbide were determined in relation to the heat treatment conditions. Studies have demonstrated that subjecting materials to heat treatment at temperatures of 400 °C results in a decrease in friction coefficient and an increase in hardness. The deposition of films on the working surfaces of microdrills with subsequent heat treatment leads to a reduction in wear, an extension of their service life, and an improvement in drilling accuracy as compared to microdrills without films. Furthermore, microdrills with (Ti/DLC) × 3 films annealed in air at 400 °C exhibit negligible size reduction and better drilling accuracy.

Crystal organisation and material properties of Chama and Glycymeris myostraca and shells

Movement of bivalve hard and soft tissue requires muscular action. Despite diverse bivalve lifestyles and living environments, the myostracum, a specific hard tissue formed where muscles attach to the shell, appears similar in structure for species of many bivalve orders.We investigated myostracal and non-myostracal, valve, microstructure, texture and material properties of Chamidae and Glycymerididae species with electron-backscatter-diffraction, laser-confocal and backscatter electron imaging and nanoindentation testing. Chamidae and Glycymerididae follow different lifestyles and live in distinct environments. Chamidae are cemented to substrate and live in wave-swept, shallow, waters. Glycymerididae dwell in calm water and burrow into sandy/muddy sediment.We found that myostracal aragonite of all investigated species has a crystal assembly pattern that reflects crystal growth through growth competition. Aragonite is extensively twinned in the myostracum and non-myostracal, valve, layers, not in the calcitic ornamentation. For myostracal aragonite, we found cyclic twinning, for non-myostracal aragonite the twinning was polysynthetic or polycyclic. We show how twinning and crystallographic texture are transmitted between myostracal and non-myostracal, valve, layers. Relative to non-biological aragonite, myostracal and non-myostracal, valve, indentation elastic modulus is reduced by 10–15 % and 15–20 %, respectively; myostracal and valve hardness is increased by 15–20 % and 5–10 %, respectively. Comparing modulus and hardness between aragonitic microstructures, we found that, relative to other microstructures, myostracal modulus is increased by 5 % and myostracal hardness by 15 %. Hence, the myostracal material shows a unique and specific microstructure, texture, modulus, and hardness that might be necessary for muscle attachment to enable the lifestyle-controlled requirements posed onto the organism.

Morphological and structural analysis of Penaeus vannamei mandibles and an attempt at real-time cannibalism monitoring based on passive acoustics

Cannibalism is a significant factor contributing to individual disability, mortality, and reduced shrimp production in commercial culture. The primary challenge of controlling cannibalism is the real-time and efficient monitoring of its occurrence. Here, we simultaneously captured high-speed video and feeding acoustics to match sound signals to feeding behaviors in Penaeus vannamei. Building upon a feeding acoustics signal acquisition system, passive acoustic monitoring (PAM) was utilized to detect differences in the acoustic signals produced when shrimps fed on broken feed, pellet feed, and meat fragments of P. vannamei (cannibalism). The morphological and structural characteristics of P. vannamei mandibles were analyzed using micro-CT, nano-indentation, and Raman testing. The main findings were: (1) Feeding on meat fragments resulted in a distinct high-frequency impulse train signal that may serve as an effective indicator for monitoring cannibalistic behavior during culture. (2) Shrimps produced similar and stable acoustic signals while consuming pellet feed, broken feed, or meat fragments; however, there were significant differences in the numbers of generated pulses (P < 0.05), with broken feed < pellet feed < meat fragments. (3) The mandibles consisted of thin anterior incisors and flat thick posterior molar processes, both with stratified structures; the mandibles exhibited greater elastic modulus and hardness values in their outer layers than inner layers, and calcium phosphate deposits were present in both incisors and molar processes. The collisions between incisors showed patterns that were highly synchronized with the acoustic feeding signals. This study has expanded research on passive acoustics monitoring in crustaceans and provided crucial data for the development of precious feeding technology in crustaceans.

Unloading Model of Elastic-Plastic Half-Space Contacted by an Elastic Spherical Indenter.

A new unloading contact model of an elastic-perfectly plastic half-space indented by an elastic spherical indenter is presented analytically. The recovered deformation of the elastic indenter and the indented half-space has been found to be dependent on the elastic modulus ratio after fully unloading. The recovered deformation of the indented half-space can be calculated based on the deformation of the purely elastic indenter. The unloading process is assumed to be entirely elastic, and then the relationship of contact force and indentation can be determined based on the solved recovered deformation and conforms to Hertzian-type. The model can accurately predict the residual indentation and residual curvature radius after fully unloading. Numerical simulations are performed to demonstrate the assumptions and the unloading model. The proposed unloading model can cover a wide range of indentations and material properties and is compared with existing unloading models. The cyclic behavior including loading and unloading can be predicted by combining the proposed unloading law with the existing contact loading model. The combined model can be employed for low-velocity impact and nanoindentation tests and the comparison results are in good agreement.

Synthesis and characterization of multi-walled carbon nanotube-reinforced Ti–Mg alloy prepared by mechanical alloying and microwave sintering

Titanium-magnesium (Ti–Mg) alloy is a widely accepted bimetallic material suitable for biomedical applications. However, reduced wear and corrosion resistance, low strength and hardness, and stress shielding effect limit their widespread applications. Reinforcing multi-walled carbon nanotubes (MWCNTs) possessing low density, high modulus, and improved mechanical properties overcome the shortcomings of Ti–Mg alloy. In the present work, nanostructured Ti–Mg alloy was synthesized at room temperature and simultaneously reinforced with MWCNTs. The high energetic ball milling process (HEBM) has been successfully utilized to mechanically alloy Ti with Mg at room temperature by decreasing the grain size to the nanoscale and reinforcing the alloy with MWCNTs. The synthesized nanostructured powder size was 25 nm. Characterization results have shown the emergence of new phases like Ti4C4 and Mg2C3 as a result of mechanical alloying (MA). The reinforced alloy powder was consolidated by cold compaction and followed by microwave sintering. The consolidated sample crystallite size attained was 72 nm and then characterized by Nanoindentation, XRD, and SEM. XRD results show intermetallic compounds Mg2C3 and TiC in bulk samples. SADP TEM confirmed the retention of Nano and partial amorphous structures in the consolidated samples. The nanoindentation test revealed the hardness and elastic modulus values 0.93 GPa and 28.12 GPa, respectively, equivalent to CpTi and its associated alloys. The results are prevalent in those alloys used in biomedical applications produced by conventional melting and casting techniques and can be a potential biomaterial.

Analysis and Optimization of a Novel Compact Compliant 2-DOF Positioner for Positioning to Assess Bio-Specimen Characteristics

A novel compact 2-DOF compliant positioner is developed for the purpose of achieving good characteristics such as high natural frequency, high displacement amplification ratio, good linear motion, and compact structure based on its symmetrical structure. To be specific, the developed stage is proposed according to an advanced six-lever displacement amplifier arranged at an inclination angle of the rigid bar utilizing right circular hinges and a parallel guiding mechanism with integrated flexure leaf hinges to attain the above-mentioned characteristics and reduce the decoupling mobility error. First, to quickly assess the initial quality response, an integration method of kinetostatic analysis, the Lagrange method, and finite element analysis was applied to evaluate and verify the quality characteristic of the stage. The experimental result showed that the error between the analytical method and the FEA method was 1.3%, which was relatively small and reliable for quickly assessing the primary quality response of the proposed positioner. Next, to boost the important output characteristics of the developed positioner, the integration approach of the response surface method and NSGA-II algorithm was utilized to find the optimal design variables. Finally, a prototype was manufactured based on the CNC milling method to validate the experimental and FEA analysis results. The attained results show that the optimal results of safety factor and output displacement were 2.4025 and 248.9 µm. Moreover, the FEA verification results were 2.4989 and 242.16 µm, with errors for safety factor and output displacement between the optimal result and the FEA result of 3.86% and 2.78%, respectively. In addition, the simulation and experimental results of the first natural frequency were 371.83 Hz and 329.59 Hz, respectively, and the error between the FEA result and experimental result for the first natural frequency was 11.36%. Furthermore, the achieved results show that the relationship between input displacement and output displacement of the experimental result and the FEA result of the developed structure achieved a good linear connection. These results suggest that the proposed positioner will be a potential structure employed in precise positioning systems and nanoindentation testing positioning systems for checking bio-specimens’ behaviors.

Effect of Chain Orientation on Coupling of Optical and Mechanical Anisotropies of Polymer Films

Polymer films have broad applications in different industries with specific requirements for their optical and mechanical properties. In mass production, processing conditions during film formation that apply forces and motions in various directions to the film tend to manifest preferred molecular chain orientation in the film microstructure, which unavoidably produces optical and mechanical anisotropies. In this paper, we investigate the effect of such macromolecular orientations on the optical and mechanical anisotropies of several polymer films, including polystyrene, poly(methyl methacrylate), poly(ethylene terephthalate), poly(ethylene naphthalate), poly(ether ether ketone), poly(ether sulfones), poly(ethylene chlorotrifluoroethylene), poly(phenylsulfone), and polycarbonate, at temperatures well below their respective glass transitions (Tg). The film mechanical responses, including elasticity, yielding, and post-yield behaviors, were obtained for the in- and out-of-plane directions utilizing tensile and nanoindentation testing methods, respectively. In addition, the net chain orientation within the films was evaluated by birefringence through analyzing the film optical refractive indices, which were verified and complemented by wide-angle X-ray scattering (WAXS) measurements. The results reveal a considerable quantitative correlation between the birefringence and the degree of elastic anisotropy and a qualitative correlation between the chain orientation and the film post-yield tensile instability (necking). These observations corroborate the interrelationship between the microstructure of polymer films and their optical and mechanical properties. In addition, they emphasize that process conditions can be selected to tune the optical and mechanical anisotropies to best serve the material performance in specific devices. We also propose an empirical equation to approximate the out-of-plane film stiffness based upon the optical and in-plane mechanical properties.

Micromechanical property evolution and damage mechanism of coal subjected to ScCO2 treatment

Carbon dioxide (CO2) injection into deep coal seams holds considerable significance in both carbon mitigation and enhanced recovery of clean coalbed methane (CBM). The CO2-coal interaction leads to changes in the physicochemical properties, potentially impacting the stability of the target sequestration coal reservoir. This study applied the nanoindentation, scanning probe microscopy (SPM), X-ray diffraction (XRD), and electron probe X-ray Micro-Analyzer (EPMA) techniques to probe the micromechanical property change and damage mechanism of coal subjected to ScCO2 injection. The result shows that the load-displacement behavior of the tested coal changes with continuous ScCO2 treatment, and the mechanical strength significantly weakens after 4 days of ScCO2 treatment. The nanoindentation test indicates that the peak and creep displacements of tested coal increased by 168.79 % and 1046.32 % respectively with 4-day ScCO2 treatment, inferring that the coal deformation increases and changes from elastic to plastic after ScCO2 injection. As the ScCO2 treatment time increases, Young's modulus and hardness of coal exhibit an exponential decay trend and rapidly decrease by 77.77 %∼89.76 % and 68.37 %∼81.63 % respectively after the initial 3-day treatment, followed by a slow decrease with the ScCO2 duration prolonging. The XRD and EPMA results show that the carbonate minerals reacted preferentially with ScCO2, and silicate minerals experienced gradual dissolution, while the amorphous carbon fluctuated almost unchanged in the tested coal. Carbonate minerals in tested coal have decreased by 70.68 % within the first 1-day ScCO2 treatment, making the most significant contribution to the initial rapid weakening of coal mechanics. The mineral distribution is closely related to the mechanical anisotropy of coal, which is confirmed by the phenomenon that the coal anisotropy gradually weakens with the mineral reaction process. It is inferred that the mineral component and distribution of coal seams are important indicators for evaluating the intensity of physical and chemical reactions in ScCO2-injected reservoirs, which directly determines the mechanical damage behavior of sequestration reservoirs. This research provides basic support for site selection and safety assessment of carbon sequestration in deep coal seams.

A new approach for in situ electrochemical nanoindentation: Side charging as a promising alternative

Understanding hydrogen embrittlement in metals is an essential task for the energy transition, where hydrogen plays a key role. Besides the economic consequences of embrittlement, safety aspects are a very important factor to consider. Therefore, materials need to be screened in order to evaluate their mechanical response under hydrogen influence. Besides macroscopic mechanical testing, in situ electrochemical nanoindentation and micromechanical testing —in general— represent promising methods as they allow to characterize individual microstructural features. In the established “front-side” charging approach, hydrogen enters the sample at the same surface on which indentation tests are performed. An alternative is “back-side” charging, where hydrogen is introduced at the opposite side of the indentation location. In the present study, a novel “side” charging cell was designed and the results were compared to those obtained by “front-side” charging. For this purpose, a ferritic steel with high chromium content (X6Cr17) underwent a grain coarsening heat treatment to ensure that multiple nanoindentation experiments can be performed within a single grain. A similar grain orientation was tested with both charging approaches. The novel “side” charging cell design outperforms the stiffness of the reference front-side charging cell by 60 %. Both cell designs yielded constant Young's moduli before, during and several hours after charging. The hardness increased during charging due to hydrogen uptake, whereas the hardness settled several hours after charging to the values before charging started. The presence of hydrogen at the indentation side was confirmed by in situ X-ray diffraction using a self-reporting titanium film.

Evaluation of tribological and biological properties of Ti6Al4V coated with Si3N4/ND nanoparticles for orthopedic applications: a comprehensive analysis

In this study, the biocompatibility and tribological properties of Ti6Al4V coated with silicon nitride (Si3N4)/nanodiamond using the electrophoretic deposition method were investigated. Suspensions of various aqueous and alcoholic solutions were prepared in the presence of CTAB and SDS dispersers. The most stable suspension system for the electrophoresis process was selected (aqueous media/ SDS disperser). Four different voltages (20, 30, 40 and 50 V) were applied to study the effect of voltage on the coating property. One could find that processing with 40 V obtained the best coating. The nano-composite coating was characterized using scanning electron microscopy equipped with energy dispersive spectroscopy, mapping analysis and x-ray diffraction after the coating process. The samples were then subjected to two nanoindentation and nano-scratching tests to evaluate their tribological properties. Biocompatibility was assessed in an ex vivo environment using two cell culture tests to evaluate survival and cellular adhesion. The results showed that the hardness and modulus elasticity of the coated sample increased from 85 to 124 GPa and 1.14–3.55 GPa, respectively, compared to the non-coated sample. Additionally, the MTT test results indicated that cellular survival and proliferation of MG63 cells increased from 86% for the non-coated sample to 92% for the Ti6Al4V/Si3N4 /ND sample. These findings have implications for orthopedic implant applications.

Modeling of cracking behavior of CrAlN coatings on silicon during micro- and nanoindentation

The deformation and failure behavior of any coating governs the performance of the resulting coating system. In the present work, we numerically and experimentally examine the fundamental deformation mechanisms of CrAlN coating on Si substrate, particularly its cracking behavior under indentation processes. For this purpose, CrAlN coatings deposited on monocrystalline Si substrates by pulsed DC magnetron sputtering were subject to indentation procedures with different depths. Subsequent characterization of top surface and cross-sectional morphologies demonstrates a strong dependence of coating profile and microstructures on the initial surface condition of the substrate. Specifically, uniform CrAlN coatings with a thickness of 1.1 μm and densified columnar microstructures were prepared on a polished Si substrate. Berkovich nanoindentation test with an indentation depth of 530 nm derives the mechanical properties of the prepared CrAlN coating. The corresponding finite element simulation reveals the propensity of cracking initiation accompanied by the stress concentration at three edge corners of the dent. Subsequent microindentation test with an indentation depth of 1.09 μm demonstrates the coexistence of plastic deformation and brittle fracture of CrAlN coating. In particular, surface radial cracks within CrAlN coating are experimentally and theoretically observed, and the cracking processes are analyzed in detail by finite element simulations.