Super-durable ultralong carbon nanotubes.

Fatigue resistance is a key property of the service lifetime of structural materials. Carbon nanotubes (CNTs) are one of the strongest materials ever discovered, but measuring their fatigue resistance is a challenge because of their size and the lack of effective measurement methods for such small samples. We developed a noncontact acoustic resonance test system for investigating the fatigue behavior of centimeter-long individual CNTs. We found that CNTs have excellent fatigue resistance, which is dependent on temperature, and that the time to fatigue fracture of CNTs is dominated by the time to creation of the first defect.

Continuous, Ultra-lightweight, and Multipurpose Super-aligned Carbon Nanotube Tapes Viable over a Wide Range of Temperatures.

In extreme environments, such as at ultrahigh or ultralow temperatures, the amount of tape used should be minimal so as to reduce system contamination and unwanted residues. However, tapes made from conventional materials typically lose their adhesiveness or leave residues difficult to remove under such conditions. Thus, the development of more versatile, lightweight, and easily removable tapes for applications in such extreme environments has received considerable attention. Here, we report that horizontally superaligned carbon nanotube (SACNT) tapes can be used to provide perfect van der Waals (vdW) interface contacts over a wide range of temperatures (from -196 to 1000 °C), yielding outstanding adhesiveness with specific adhesion strengths up to ∼1.1 N/µg. With a surface density of only 0.5-5 µg/cm2, hundreds of times lighter than the vertically aligned CNT adhesives, the SACNT tapes can be cost-effectively provided in hundreds of meters. They have multipurpose adhesive abilities for versatile materials and are also easily separated from samples even after exposure to extreme temperature regimes. First-principles calculations confirm the mechanism of vdW adhesion and reveal that ultraflat and nanometer-thick SACNT tapes may yield far greater adhesive abilities. These SACNT tapes show great potential for use in mechanical bonding, electrical bonding, and thermal dissipation in electronic devices.

Carbon nanotube bundles with tensile strength over 80 GPa.

Carbon nanotubes (CNTs) are one of the strongest known materials. When assembled into fibres, however, their strength becomes impaired by defects, impurities, random orientations and discontinuous lengths. Fabricating CNT fibres with strength reaching that of a single CNT has been an enduring challenge. Here, we demonstrate the fabrication of CNT bundles (CNTBs) that are centimetres long with tensile strength over 80 GPa using ultralong defect-free CNTs. The tensile strength of CNTBs is controlled by the Daniels effect owing to the non-uniformity of the initial strains in the components. We propose a synchronous tightening and relaxing strategy to release these non-uniform initial strains. The fabricated CNTBs, consisting of a large number of components with parallel alignment, defect-free structures, continuous lengths and uniform initial strains, exhibit a tensile strength of 80 GPa (corresponding to an engineering tensile strength of 43 GPa), which is far higher than that of any other strong fibre.

Sensing Performance Analysis on Quartz Tuning Fork-Probe at the High Order Vibration Mode for Multi-Frequency Scanning Probe Microscopy.

Multi-frequency scanning near-field optical microscopy, based on a quartz tuning fork-probe (QTF-p) sensor using the first two orders of in-plane bending symmetrical vibration modes, has recently been developed. This method can simultaneously achieve positional feedback (based on the 1st in-plane mode called the low mode) and detect near-field optically induced forces (based on the 2nd in-plane mode called the high mode). Particularly, the high mode sensing performance of the QTF-p is an important issue for characterizing the tip-sample interactions and achieving higher resolution microscopic imaging but the related researches are insufficient. Here, we investigate the vibration performance of QTF-p at high mode based on the experiment and finite element method. The frequency spectrum characteristics are obtained by our homemade laser Doppler vibrometer system. The effects of the properties of the connecting glue layer and the probe features on the dynamic response of the QTF-p sensor at the high mode are investigated for optimization design. Finally, compared with the low mode, an obvious improvement of quality factor, of almost 50%, is obtained at the high mode. Meanwhile, the QTF-p sensor has a high force sensing sensitivity and a large sensing range at the high mode, indicating a broad application prospect for force sensing.

A Multiscale Material Testing System for In Situ Optical and Electron Microscopes and Its Application.

We report a novel material testing system (MTS) that uses hierarchical designs for in-situ mechanical characterization of multiscale materials. This MTS is adaptable for use in optical microscopes (OMs) and scanning electron microscopes (SEMs). The system consists of a microscale material testing module (m-MTM) and a nanoscale material testing module (n-MTM). The MTS can measure mechanical properties of materials with characteristic lengths ranging from millimeters to tens of nanometers, while load capacity can vary from several hundred micronewtons to several nanonewtons. The m-MTM is integrated using piezoelectric motors and piezoelectric stacks/tubes to form coarse and fine testing modules, with specimen length from millimeters to several micrometers, and displacement distances of 12 mm with 0.2 µm resolution for coarse level and 8 µm with 1 nm resolution for fine level. The n-MTM is fabricated using microelectromechanical system technology to form active and passive components and realizes material testing for specimen lengths ranging from several hundred micrometers to tens of nanometers. The system's capabilities are demonstrated by in-situ OM and SEM testing of the system's performance and mechanical properties measurements of carbon fibers and metallic microwires. In-situ multiscale deformation tests of Bacillus subtilis filaments are also presented.

Study of the tensile properties of individual multicellular fibres generated by Bacillus subtilis.

Multicellular fibres formed by Bacillus subtilis (B. subtilis) are attracting interest because of their potential application as degradable biomaterials. However, mechanical properties of individual fibres remain unknown because of their small dimensions. Herein, a new approach is developed to investigate the tensile properties of individual fibres with an average diameter of 0.7 µm and a length range of 25.7-254.3 µm. Variations in the tensile strengths of fibres are found to be the result of variable interactions among pairs of microbial cells known as septa. Using Weibull weakest-link model to study this mechanical variability, we predict the length effect of the sample. Moreover, the mechanical properties of fibres are found to depend highly on relative humidity (RH), with a brittle-ductile transition occurring around RH = 45%. The elastic modulus is 5.8 GPa in the brittle state, while decreases to 62.2 MPa in the ductile state. The properties of fibres are investigated by using a spring model (RH < 45%) for its elastic behaviour, and the Kelvin-Voigt model (RH > 45%) for the time-dependent response. Loading-unloading experiments and numerical calculations demonstrate that necking instability comes from structural changes (septa) and viscoelasticity dominates the deformation of fibres at high RH.

Research on the Sensing Performance of the Tuning Fork-Probe as a Micro Interaction Sensor.

The shear force position system has been widely used in scanning near-field optical microscopy (SNOM) and recently extended into the force sensing area. The dynamic properties of a tuning fork (TF), the core component of this system, directly determine the sensing performance of the shear positioning system. Here, we combine experimental results and finite element method (FEM) analysis to investigate the dynamic behavior of the TF probe assembled structure (TF-probe). Results from experiments under varying atmospheric pressures illustrate that the oscillation amplitude of the TF-probe is linearly related to the quality factor, suggesting that decreasing the pressure will dramatically increase the quality factor. The results from FEM analysis reveal the influences of various parameters on the resonant performance of the TF-probe. We compared numerical results of the frequency spectrum with the experimental data collected by our recently developed laser Doppler vibrometer system. Then, we investigated the parameters affecting spatial resolution of the SNOM and the dynamic response of the TF-probe under longitudinal and transverse interactions. It is found that the interactions in transverse direction is much more sensitive than that in the longitudinal direction. Finally, the TF-probe was used to measure the friction coefficient of a silica-silica interface.

Measurement of the cleavage energy of graphite.

The basal plane cleavage energy (CE) of graphite is a key material parameter for understanding many of the unusual properties of graphite, graphene and carbon nanotubes. Nonetheless, a wide range of values for the CE has been reported and no consensus has yet emerged. Here we report the first direct, accurate experimental measurement of the CE of graphite using a novel method based on the self-retraction phenomenon in graphite. The measured value, 0.37±0.01 J m(-2) for the incommensurate state of bicrystal graphite, is nearly invariant with respect to temperature (22 °C≤T≤198 °C) and bicrystal twist angle, and insensitive to impurities from the atmosphere. The CE for the ideal ABAB graphite stacking, 0.39±0.02 J m(-2), is calculated based on a combination of the measured CE and a theoretical calculation. These experimental measurements are also ideal for use in evaluating the efficacy of competing theoretical approaches.

Characterization of micro-contact resistance between a gold nanocrystalline line and a tungsten electrode probe in interconnect fatigue testing.

An electromechanically-coupled micro-contact resistance measurement system is built to mimic the contact process during fatigue testing of nanoscale-thickness interconnects using multiple probe methods. The design combines an optical microscope, high-resolution electronic balance, and micromanipulator-controlled electric probe, and is coupled with electrical measurements to investigate microscale contact physics. Experimental measurements are performed to characterize the contact resistance response of the gold nanocrystalline pad of a 35-nm-thick interconnect under mechanical force applied by a tungsten electrode probe. Location of a stable region for the contact resistance and the critical contact force provides better understanding of micro-contact behavior relative to the effects of the contact force and the nature of the contact surface. Increasing contact temperature leads to reduced contact resistance, softens the pad material, and modifies the contact surface. The stability of both contact resistance and interconnect resistance is studied under increasing contact force. Major fluctuations emerge when the contact force is less than the critical contact force, which shows that temporal contact resistance will affect interconnect resistance measurement accuracy, even when using the four-wire method. This performance is demonstrated experimentally by heating the Au line locally with a laser beam. Finally, the contact resistances are calculated using the LET (Li-Etsion-Talke) model together with combined Holm and Sharvin theory under various contact forces. Good agreement between the results is obtained. This research provides a way to measure change in interconnect line resistance directly under a stable contact resistance regime with a two-wire method that will greatly reduce the experimental costs.

Interferometric dynamic measurement: techniques based on high-speed imaging or a single photodetector.

In recent years, optical interferometry-based techniques have been widely used to perform noncontact measurement of dynamic deformation in different industrial areas. In these applications, various physical quantities need to be measured in any instant and the Nyquist sampling theorem has to be satisfied along the time axis on each measurement point. Two types of techniques were developed for such measurements: one is based on high-speed cameras and the other uses a single photodetector. The limitation of the measurement range along the time axis in camera-based technology is mainly due to the low capturing rate, while the photodetector-based technology can only do the measurement on a single point. In this paper, several aspects of these two technologies are discussed. For the camera-based interferometry, the discussion includes the introduction of the carrier, the processing of the recorded images, the phase extraction algorithms in various domains, and how to increase the temporal measurement range by using multiwavelength techniques. For the detector-based interferometry, the discussion mainly focuses on the single-point and multipoint laser Doppler vibrometers and their applications for measurement under extreme conditions. The results show the effort done by researchers for the improvement of the measurement capabilities using interferometry-based techniques to cover the requirements needed for the industrial applications.

Dynamic behavior of tuning fork shear-force structures in a SNOM system.

Piezoelectric tuning fork shear-force structures are widely used as a distance control unit in a scanning near-field optical microscopy. However, the complex dynamic behavior among the micro-tuning forks (TFs), optical fiber probes, and the probe-surface interactions is still a crucial issue to achieve high-resolution imaging or near-field interaction inspections. Based on nonlinear beam tension-bending vibration theory, vibration equations in both longitudinal and lateral directions have been established when the TF structure and the optical fiber are treated as deformable structures. The relationship of the probe-surface interaction induced by Van der Waals force has been analyzed and the corresponding numerical results used to describe the vibrational behavior of the probe approaching the sample surface are obtained. Meanwhile, the viscous resistance of the liquid film on the sample surface has also been investigated using linear beam-bending vibration theory. Experiments testing the interaction between the probe and the water film on a single crystal silicon wafer have been carried out and the viscous resistance of the water film was estimated using the established equations. Finally, to use the TF-probe structure as a force sensor, the relation between the dynamic response of the TF-probe system and an external force on the probe tip was obtained.

Therapeutic effects of Chinese osteopathy in patients with lumbar disc herniation.

A clinical study was conducted in 72 lumbar disc herniation (LDH) patients and 40 asymptomatic subjects to evaluate the efficacy of Feng's spinal manipulation (FSM). FSM was performed twice a week for less than 20 days. Changes in the symmetrical index of spinal column (SISC) and quantified symptom index (QSI) before and after FSM in both groups were collected. The QSI consisted of the visual analogue scale (VAS), score of the Japanese Orthopedic Association, and straight leg raising test, for measurement of pain perception, dysfunction of lower limb extension or flexion, and symptomatic relief. A correlation analysis was conducted to compare the difference in protruded nucleus pulposus size using computerized projection grating profilometry, SISC, and QSI before and after the therapy. The results showed that the SISC and QSI significantly decreased after treatment in the LDH group (p < 0.01). The SISC before and after treatment was closely correlated with the improvement of QSI, although there was no change in protruded nucleus pulposus following the therapy. Among the five components in SISC, the LR was found to be an ideal indicator for evaluation of the real circumstances in LDH patients. Our data suggested that FSM achieved satisfactory therapeutic effects in relieving the symptom of LDH while no effects were observed in asymptomatic subjects.

Observation of high-speed microscale superlubricity in graphite.

A sheared microscopic graphite mesa retracts spontaneously to minimize interfacial energy. Using an optical knife-edge technique, we report first measurements of the speeds of such self-retracting motion (SRM) from the mm/s range at room temperature to 25 m/s at 235°C [corrected]. This remarkably high speed is comparable with the upper theoretical limit found for sliding interfaces exhibiting structural superlubricity. We observe a strong temperature dependence of SRM speed which is consistent with a thermally activated mechanism of translational motion that involves successive pinning and depinning events at interfacial defects. The activation energy for depinning is estimated to be 0.1-1 eV.

Alternating-current induced thermal fatigue of gold interconnects with nanometer-scale thickness and width.

With dramatic reduction in sizes of microelectronic devices, the characteristic width and thickness of interconnects in large-scale integrated circuits have reached nanometer scale. Thermal fatigue damage of so small interconnects has attracted more and more attentions. In this work, thermal fatigue of Au interconnects, 35 nm thick and 0.1-5 µm wide, is investigated by applying various alternating current densities to generate cycling temperature and strain in them. A multi-probe measuring system is installed in a scanning electron microscope and a probe-type temperature sensor is for the first time introduced into the system for real-time measuring the temperatures on the pads of the tested interconnects. A one-dimensional heat conduction equation, which uses measured temperatures on the pads as boundary conditions and includes a term of heat dissipation through the interface between the interconnect and the oxidized silicon substrate, is proposed to calculate the time-resolved temperature distribution along the Au interconnects. The measured fatigue lifetimes are presented versus current density and thermal cyclic strain, and the results show that narrower Au lines are more reliable. The failure mechanism of those Au interconnects differs from what is observed in thick interconnects with relatively larger grain size. Topography change caused by localized plasticity on the less-constrained surfaces of the interconnects have not been observed. Instead, grain growing and reorienting due to local temperature varying appear, and grain boundary migration and mergence take place during high temperature fatigue in such thin and narrow interconnects. These results seem to reflect a strain-induced boundary migration mechanism, and the damage morphology also suggests that fatigue of the interconnects with decreased grain size and film thickness is controlled by diffusive mechanisms and interface properties rather than by dislocation glide. Open circuit eventually took place by melting at a region of severely damage cross-sectional area with the grain growing and reorienting.

Surface effects on the mechanical properties of nanoporous materials.

Using the theory of surface elasticity, we investigate the mechanical properties of nanoporous materials. The classical theory of porous materials is modified to account for surface effects, which become increasingly important as the characteristic sizes of microstructures shrink to nanometers. First, a refined Timoshenko beam model is presented to predict the effective elastic modulus of nanoporous materials. Then the surface effects on the elastic microstructural buckling behavior of nanoporous materials are examined. In particular, nanoporous gold is taken as an example to illustrate the application of the proposed model. The results reveal that both the elastic modulus and the critical buckling behavior of nanoporous materials exhibit a distinct dependence on the characteristic sizes of microstructures, e.g. the average ligament width.

[Correlation studies between MRI and the symptom scores of patients with LDH before and after manipulative therapy].

OBJECTIVE: To study the correlation between the MRI and some symptom scores of the patients with lumbar disc herniation (LDH), such as VAS (visual analogue scale), JOA (Japanese orthopedic association scale),and SLR (straight leg raising test) before and after manipulative therapy. METHODS: From June to December in 2007, 70 patients with LDH were selected in the study. Among the patients, 40 patients were male and 30 patients were female, ranging in age from 21 to 56 years (averaged 39 years). MRI was used to measure the size and position of the protruded nucleus pulposus (size of disc protrution, the angle between nerve root canal and disc protrution). Correlation study was conducted between the MRI and VAS, JOA, and SLR before and after therapy. The correlation between the changes of MRI and that of the quantified clinical indexes of LDH patients was also analyzed. RESULTS: There were significant differences before and after therapy in some quantified indexes for the clinical manifestation of the patients, such as VAS, JOA,and SLR. There were no significant changes in the shape and size of protrude nucleus pulposus after 20 days' therapy by CT or MR recheck. Correlation study between the quantified indexes of clinical manifestation (JOA) and MRI before and after the treatment showed that there was no significant correlation. CONCLUSION: The study proves again that the shape and size of protrude nucleus pulposus has no paralleled relation with the patient's clinical manifestation,which is demonstrated by the recheck of MRI after a successful spinal manipulative treatment in the study.

Correlation of the thermal and electrical conductivities of nanoporous gold.

We measured the thermal and electrical conductivities of nanoporous Au thin foils in the temperature range 93-300 K. Resulting from the nanoscale microstructure, the two types of conductivities are both temperature dependent and significantly lower than those of bulk Au. However, the corresponding Lorenz number is strikingly similar to that of bulk Au, indicating that the Wiedemann-Franz law holds perfectly well for nanoporous metals in this temperature range. Compared to the bulk value, the Debye temperature of nanoporous Au is decreased. We predict the theoretical Debye temperature of nanoporous Au by its relation to the elastic constants. The present results indicate that the nanoporous Au foils should be comprised of macroscopic, single-crystalline porous grains rather than nanocrystals.

A uniaxial tension system and its applications in testing of thin films and small components.

The aim of this investigation is to develop a uniaxial tension system for testing very small samples that allows observation of the gauge section by optical or atomic force microscopy. Major parts of the system consist of a pair of identical piezoelectric actuators, two symmetrical double-cantilevered force sensors, and two symmetrical universal coupling joints. It can accomplish both-end loaded uniaxial tension to produce centrosymmetric deformations of the tested objects in the field of view and can apply tensile loads in the range from 7.8 microN to 15 N to the samples. Sample extensions from submicrometers to 100 microm can be measured with displacement resolution of several tens of nanometers. The system's performance is demonstrated by tests of a polycrystalline aluminum alloy thin sheet, a mica thin sheet, and a fibril of bamboo.

Meniscus-climbing behavior and its minimum free-energy mechanism.

Some insects can climb up the top of the meniscus surface generated by a hydrophilic wall by fixing their posture without moving their appendages [Baudoin, R. Bull. Biol. Fr. Belg. 1955, 89, 16. Hu, D. L.; Bush, J. W. M. Nature 2005, 437, 733]. To better understand this interesting phenomenon, we did meniscus-climbing experiments of bent copper sheets. It was found that the sheets do not always climb up the top of the meniscus surface but may stop and stably stay at various positions on the meniscus surface, depending upon their curvatures and masses, and that bent copper sheets can self-assemble into an oriented array (or an anisotropic form) through self-rotating on the water surface. The minimum energy mechanism of meniscus-climbing and self-rotating was then numerically studied. It was further shown that the meniscus-climbing and the rotating behavior is not only a general phenomenon for floating objects with hydrophilic surfaces, even those with fairly large sizes and weights (e.g., a metal bottle cap), but is also conditionally realizable for floating objects with hydrophobic surfaces.