Nanoscale Adhesion and Material Transfer at 2D MoS2-MoS2 Interfaces Elucidated by In Situ Transmission Electron Microscopy and Atomistic Simulations.

Low-dimensional materials, such as MoS2, hold promise for use in a host of emerging applications, including flexible, wearable sensors due to their unique electrical, thermal, optical, mechanical, and tribological properties. The implementation of such devices requires an understanding of adhesive phenomena at the interfaces between these materials. Here, we describe combined nanoscale in situ transmission electron microscopy (TEM)/atomic force microscopy (AFM) experiments and simulations measuring the work of adhesion (Wadh) between self-mated contacts of ultrathin nominally amorphous and nanocrystalline MoS2 films deposited on Si scanning probe tips. A customized TEM/AFM nanoindenter permitted high-resolution imaging and force measurements in situ. The Wadh values for nanocrystalline and nominally amorphous MoS2 were 604 ± 323 mJ/m2 and 932 ± 647 mJ/m2, respectively, significantly higher than previously reported values for mechanically exfoliated MoS2 single crystals. Closely matched molecular dynamics (MD) simulations show that these high values can be explained by bonding between the opposing surfaces at defects such as grain boundaries. Simulations show that as grain size decreases, the number of bonds formed, the Wadh and its variability all increase, further supporting that interfacial covalent bond formation causes high adhesion. In some cases, sliding between delaminated MoS2 flakes during separation is observed, which further increases the Wadh and the range of adhesive interaction. These results indicate that for low adhesion, the MoS2 grains should be large relative to the contact area to limit the opportunity for bonding, whereas small grains may be beneficial, where high adhesion is needed to prevent device delamination in flexible systems.

A methodology to evaluate different histological preparations of soft tissues: Intervertebral disc tissues study.

A tissue preparation method will inevitably alter the tissue content. This study aims to evaluate how different common sample preparation methods will affect the tissue morphology, biomechanical properties, and chemical composition of samples. The study focuses on intervertebral disc (IVD) tissue; however, it can be applied to other soft tissues. Raman spectroscopy synchronized with nanoindentation instrumentation was employed to investigate the compositional changes of IVD, specifically, nucleus pulposus (NP) and annulus fibrosus (AF), together with their biomechanical properties of IVD. These properties were examined through the following histological specimen types: fresh cryosection (control), fixed cryosection, and paraffin-embedded. The IVD tissue could be located using an optical microscope under three different preparation methods. Paraffin-embedded samples showed the most explicit details where the lamellae structure of AF could be identified. In terms of biomechanical properties, there was no significant difference between the fresh and fixed cryosection (p > 0.05). In contrast, the fresh cryosection and paraffin-embedded samples showed a significant difference (p < 0.05). It was also found that the tissue preparations affected the chemical content of the tissues and structure of the tissue, which are expected to contribute to biomechanical properties changes. Fresh cryosection and fixed cryosection samples are more promising to work with for biomechanical assessment in histological tissues. The findings fill essential gaps in the literature by providing valuable insight into the characteristics of IVD at the microscale. This study can also become a reference for a better approach to assessing the mechanical properties and chemical content of soft tissues at the microscale.

Mammalian tooth enamel functional sophistication demonstrated by combined nanotribology and synchrotron radiation FTIR analyses.

The teeth of limbed vertebrates used for capturing and processing food are composed of mineralized dentine covered by hypermineralized enamel, the hardest material organisms produce. Here, we combine scanning probe microscopy, depth sensing, and spectromicroscopy (SR-FTIR) to characterize the surface ultrastructural topography, nanotribology, and chemical compositions of mammal species with different dietary habits, including omnivorous humans. Our synergistic approach shows that enamel with greater surface hardness or thickness exhibited a more salient gradient feature from the tooth surface to the dentino-enamel junction (DEJ) one that corresponds to the in situ phosphate-to-amide ratio. This gradient feature of enamel covering softer dentine is the determining factor of the amazingly robust physical property of this unique biomaterial. It provides the ability to dissipate stress under loading and prevent mechanical failure. Evolutionary change in the biochemical composition and biomechanical properties of mammalian dentition is related to variations in the oral processing of different food materials.

Correlation of the degenerative stage of a disc with magnetic resonance imaging, chemical content, and biomechanical properties of the nucleus pulposus.

Intervertebral disc degeneration (IDD) is closely related to changes in the intervertebral disc (IVD) composition and the resulting viscoelastic properties. IDD is a severe condition because it decreases the disc's ability to resist mechanical loads. Our research aims to understand IDD at the cellular level, specifically the changes in the viscoelastic properties of the nucleus pulposus (NP), which are poorly understood. This study employed a system integrating nanoindentation with Raman spectrometry to correlate biomechanics with subtle changes in the biochemical makeup of the NP. The characterization was, in turn, correlated with the degenerative severity of IVD as assessed using magnetic resonance imaging (MRI) of different patients with spinal stenosis, degenerative spondylolisthesis, and degenerative scoliosis. It is shown that there is an increase in the crosslinking ratio in collagen, a reduction in proteoglycan, and a build-up of minerals upon the rise in the severity level of the disc damage in the NP. Assessment of mechanical characteristics reveals that the increasing disc degeneration makes the NP lose its elasticity, becoming more viscous. This shows that the tissue undergoes abnormalities in weight-bearing ability, which contributes to spinal instability. The correlation of the individual discs shows that grades III and IV have similarities in the changes of Amide I and III toward the storage modulus. In contrast, grades IV and V correlate with mineralization toward the storage modulus. Reduction of proteoglycan has the highest impact on the changes of the storage modulus in all grades of IDD. Connecting compositional alterations to IVD micromechanics at various degrees of degeneration expands our understanding of tissue behavior and provides critical insight into clinical diagnostics, treatment, and tissue engineering.

Three-Dimensional Finite Element Investigation into Effects of Implant Thread Design and Loading Rate on Stress Distribution in Dental Implants and Anisotropic Bone.

Variations in the implant thread shape and occlusal load behavior may result in significant changes in the biological and mechanical properties of dental implants and surrounding bone tissue. Most previous studies consider a single implant thread design, an isotropic bone structure, and a static occlusal load. However, the effects of different thread designs, bone material properties, and loading conditions are important concerns in clinical practice. Accordingly, the present study performs Finite Element Analysis (FEA) simulations to investigate the static, quasi-static and dynamic response of the implant and implanted bone material under various thread designs and occlusal loading directions (buccal-lingual, mesiodistal and apical). The simulations focus specifically on the von Mises stress, displacement, shear stress, compressive stress, and tensile stress within the implant and the surrounding bone. The results show that the thread design and occlusal loading rate have a significant effect on the stress distribution and deformation of the implant and bone structure during clinical applications. Overall, the results provide a useful insight into the design of enhanced dental implants for an improved load transfer efficiency and success rate.

Nanonetwork Thermosets from Templated Polymerization for Enhanced Energy Dissipation.

Herein, we aim to develop a facile method for the fabrication of mechanical metamaterials from templated polymerization of thermosets including phenolic and epoxy resins using self-assembled block copolymer, polystyrene-polydimethylsiloxane with tripod network (gyroid), and tetrapod network (diamond) structures, as templates. Nanoindentation studies on the nanonetwork thermosets fabricated reveal enhanced energy dissipation from intrinsic brittle thermosets due to the deliberate structuring; the calculated energy dissipation for gyroid phenolic resins is 0.23 nJ whereas the one with diamond structure gives a value of 0.33 nJ. Consistently, the gyroid-structured epoxy gives a high energy dissipation value of 0.57 nJ, and the one with diamond structure could reach 0.78 nJ. These enhanced properties are attributed to the isotropic periodicity of the nanonetwork texture with plastic deformation, and the higher number of struts in the tetrapod diamond network in contrast to tripod gyroid, as confirmed by the finite element analysis.

Tribological Properties of Oil-in-Water Emulsion with Carbon Nanocapsule Additives.

An experimental investigation was performed on the coefficients of friction (COFs) and wear properties of pure water and oil-in-water (O/W) working fluids containing carbon nanocapsules (CNCs) with concentrations ranging from 0 to 1.0 wt.%. For the O/W working fluid, the ratio of oil to water was set as 6%. It was shown that for the water working fluid, the COF decreased by around 20% as the CNC content increased from 0 to 1.0 wt.%. In contrast, the wear volume increased by 50% as the CNC addition increased from 0 to 0.5 wt.%, but it fell to a value slightly lower than that achieved using only pure water (i.e., no CNCs) as the CNC content was further increased to 1.0 wt.%. For the O/W emulsion, the addition of 0.8 wt.% CNCs reduced the COF by around 30% compared to that of the emulsion with no CNCs. Overall, the results showed that while the addition of a small quantity (6%) of oil to the water working fluid had a relatively small effect on the wear performance, the addition of an appropriate quantity of CNCs (i.e., 0.8 wt.%) resulted in a significantly lower COF and an improved wear surface.

Description of Residual Stresses in Autofrettaged Open-Ended Cylinders Made of High-Strength Steel.

The elastic range in loading-unloading processes is often reduced with a Bauschinger effect. This material property may have a high impact on residual stresses and, as a result, on the performance of autofrettaged cylinders under service conditions. The objective of the present paper is to demonstrate this impact using a material model that accounts for the response of typical high-strength steel. The solution is semi-analytic and, therefore, can be used for fast and accurate analysis of the process of autofrettage. A numerical example illustrates the general solution. This example shows that the Bauschinger effect has a significant impact on the residual circumferential stress in the vicinity of the inner radius of the cylinder. This stress is the most significant quantity of autofrettaged cylinders. Therefore, the main result obtained suggests that even a moderate Bauschinger effect should be taken into account in analyses of the process of autofrettage.

Mass Detection in Viscous Fluid Utilizing Vibrating Micro- and Nanomechanical Mass Sensors under Applied Axial Tensile Force.

Vibrating micro- and nanomechanical mass sensors are capable of quantitatively determining attached mass from only the first three (two) measured cantilever (suspended) resonant frequencies. However, in aqueous solutions that are relevant to most biological systems, the mass determination is challenging because the quality factor (Q-factor) due to fluid damping decreases and, as a result, usually just the fundamental resonant frequencies can be correctly identified. Moreover, for higher modes the resonance coupling, noise, and internal damping have been proven to strongly affect the measured resonances and, correspondingly, the accuracy of estimated masses. In this work, a technique capable of determining the mass for the cantilever and also the position of nanobeads attached on the vibrating micro-/nanomechanical beam under intentionally applied axial tensile force from the measured fundamental flexural resonant frequencies is proposed. The axial force can be created and controlled through an external electrostatic or magnetostatic field. Practicality of the proposed technique is confirmed on the suspended multi-walled carbon nanotube and the rectangular silicon cantilever-based mass sensors. We show that typically achievable force resolution has a negligibly small impact on the accuracy of mass measurement.

Tribological Properties of Carbon Nanocapsule Particles as Lubricant Additive.

An experimental investigation is performed into the tribological properties of mineral oil lubricants containing carbon nanocapsules (CNCs) additives with various concentrations (wt.%). Friction characteristics and wear behaviors at contact interfaces are examined by the block-on-ring tests, high-resolution transmission electron microscopy (HRTEM), and mapping (MAP) analysis. The results suggest that the addition of CNCs to the mineral oil yields an effective reduction in the friction coefficient at the contact interface. Molecular dynamics (MD) simulations clarify the lubrication mechanism of CNCs at the sliding system, indicating the tribological properties are essentially sensitive to the structural evolutions of CNCs.

Human enamel rod presents anisotropic nanotribological properties.

The AFM combined nanoindentation was performed to observe the ultrastructure of enamel rod from various section plans and positions while probing their mechanical and tribological properties of the area. The nanohardness and the elastic modulus of the head region of the enamel rods are significantly higher than that of the tail region and the axial-sectional plane. Both nanohardness and elastic modulus gradually decrease from enamel surface toward dentino-enamel junction. Such a variation correlates well with the decreasing trend of calcium composition from our element analysis. The friction coefficient and nanowear of the enamel showed an inversed trend to the hardness with respect to their relative topological position in the long axis of enamel rod toward DEJ. The relationship between the nanowear depth and the distance from the outer enamel surface to DEJ presented exponential function. The results presented clarify the basic nanomechanical and nanotribological properties of human enamel rods and provide a useful reference for the future development of dental restorative materials.

Nanoscratch Characterization of GaN Epilayers on c- and a-Axis Sapphire Substrates.

In this study, we used metal organic chemical vapor deposition to form gallium nitride (GaN) epilayers on c- and a-axis sapphire substrates and then used the nanoscratch technique and atomic force microscopy (AFM) to determine the nanotribological behavior and deformation characteristics of the GaN epilayers, respectively. The AFM morphological studies revealed that pile-up phenomena occurred on both sides of the scratches formed on the GaN epilayers. It is suggested that cracking dominates in the case of GaN epilayers while ploughing during the process of scratching; the appearances of the scratched surfaces were significantly different for the GaN epilayers on the c- and a-axis sapphire substrates. In addition, compared to the c-axis substrate, we obtained higher values of the coefficient of friction (µ) and deeper penetration of the scratches on the GaN a-axis sapphire sample when we set the ramped force at 4,000 µN. This discrepancy suggests that GaN epilayers grown on c-axis sapphire have higher shear resistances than those formed on a-axis sapphire. The occurrence of pile-up events indicates that the generation and motion of individual dislocation, which we measured under the sites of critical brittle transitions of the scratch track, resulted in ductile and/or brittle properties as a result of the deformed and strain-hardened lattice structure.

The effect of contaminants on the adhesion of the spatulae of a gecko.

Many researchers have reported that the robust adhesion that enables geckos to move quickly and securely across a range of vertical and horizontal surfaces is provided by the hierarchical structure of their feet (i.e. lamellae, setae, spatulae, etc.). Maintaining this robust adhesion requires an intimate contact between the terminal tips of the spatulae and the surface. The aim of this study was to investigate the effect on the adhesive properties of the spatulae when a particle becomes trapped at the contact surface. Using the Johnson, Kendall and Roberts (JKR) theory, a model was constructed to assist in the analysis of the interactions between the spatula tip, the particle and the surface. The results showed that the keratin (the natural material of the spatula) provides a robust system for adhesion even when there is a particle in the contact area, and the effective contact area of spatulae will be 80%. When the particle is significantly harder than the surface, the adhesion properties of the contact surface influenced by the particle will be more obvious. The results also reveal that the generated adhesion is considerably higher when the spatula is in contact with a softer surface, such as wood or concrete, rather than a hard surface, such as glass or SiO2.

Nanotribological characterization of tooth enamel rod affected by surface treatment.

Tooth enamel is a hybrid organic-inorganic bionanocomposite comprised predominantly of enamel rods. Understanding the effects of anti-caries treatment on the biomechanical properties of these rods is essential in developing effective caries prevention strategies. Calcium fluoride-like deposits play an important role in caries prevention and their nanotribological properties have a direct effect upon their long-term effectiveness. Accordingly, this study utilizes a variety of techniques, namely nanoindentation, nanoscratch tests, nanowear tests and atomic force microscopy (AFM), to characterize the mechanical and tribological properties of single enamel rods before and after topical fluoride application. The results show that the CaF(2)-like deposits formed on the enamel surface following fluoride application increase the coefficient of friction of the enamel rods, but decrease their critical load and nanohardness. As a result, the nanowear depth of the treated enamel surface is around six times higher than that of the native enamel surface under an applied load of 300 microN. Following the removal of the surface deposits, however, the modulus of elasticity and wear depth of the underlying enamel surface are found to be similar to those of the original enamel surface. However, a notable increase in the surface roughness is observed.

Molecular-dynamics studies of bending mechanical properties of empty and C60-filled carbon nanotubes under nanoindentation.

This paper utilizes molecular-dynamics simulations to investigate the mechanical characteristics of a suspended (10, 10) single-walled carbon nanotube (SWCNT) during atomic force microscopy (AFM) nanoindentation at different temperatures. Spontaneous topological transition of the Stone-Wales (SW) defects is clearly observed in the indentation process. The present results indicate that under AFM-bending deformation, the mechanical properties of the SWCNT, e.g., the bending strength, are dependent on the wrapping angle. In addition, it is also found that the radial dependence of the reduced formation energy of the SW defects is reasonably insensitive only for the small tubes. However, for tube diameters greater than 2.4 nm [corresponding to the (18, 18) CNT], the SW defects tend to be more radius sensitive. The results indicate that the bending strength decreases significantly with increasing temperature. This study also investigates the variation in the mechanical properties of the nanotube with the density of C60 encapsulated within the nanotube at various temperatures. It is found that, at lower temperatures, the bending strength of the C60-filled nanotube increases with C60 density. However, the reverse tendency is observed at higher temperatures. Finally, the "sharpest tip" phenomena between the probe and the tube wall and the elastic recovery of the nanotube during the retraction process are also investigated.