Nanoscale Broadband Viscoelastic Spectroscopy of Soft Materials Using Iterative Control

A novel approach to nanoscale broadband viscoelastic spectroscopy is presented. The proposed approach utilizes the recently developed modeling-free inversion-based iterative control (MIIC) technique to achieve accurate measurement of the material response to the applied excitation force over a broad frequency band. Scanning probe microscope (SPM) and nanoindenter have become enabling tools to quantitatively measure the mechanical properties of a wide variety of materials at nanoscale. Current nanomechanical measurement, however, is limited by the slow measurement speed: the nanomechanical measurement is slow and narrow-banded and thus not capable of measuring rate-dependent phenomena of materials. As a result, large measurement (temporal) errors are generated when material is undergoing dynamic evolution during the measurement. The low-speed operation of SPM is due to the inability of current approaches to (1) rapidly excite the broadband nanomechanical behavior of materials, and (2) compensate for the convolution of the hardware adverse effects with the material response during high-speed measurements. These adverse effects include the hysteresis of the piezo actuator (used to position the probe relative to the sample); the vibrational dynamics of the piezo actuator and the cantilever along with the related mechanical mounting; and the dynamics uncertainties caused by the probe variation and the operation condition. In the proposed approach, an input force signal with frequency characteristics of band-limited white-noise is utilized to rapidly excite the nanomechanical response of materials over a broad frequency range. The MIIC technique is used to compensate for the hardware adverse effects, thereby allowing the precise application of such an excitation force and measurement of the material response (to the applied force). The proposed approach is illustrated by implementing it to measure the frequency-dependent plane-strain modulus of poly(dimethylsiloxane) (PDMS) over a broad frequency range extending over 3 orders of magnitude (~1 Hz to 4.5 kHz).     

Fatigue damage evolution in silicon films for micromechanical applications

In this paper we examine the conditions for surface topography evolution and crack growth/fracture during the cyclic actuation of polysilicon microelectromechanical systems (MEMS) structures. The surface topography evolution that occurs during cyclic fatigue is shown to be stressassisted and may be predicted by linear perturbation analyses. The conditions for crack growth (due to pre-existing or nucleated cracks) are also examined within the framework of linear elastic fracture mechanics. Within this framework, we consider pre-existing cracks in the topical SiO₂ layer that forms on the Si substrate in the absence of passivation. The thickening of the SiO₂ that is normally observed during cyclic actuation of Si MEMS structures is shown to increase the possibility of stable crack growth by stress corrosion cracking prior to the onset of unstable crack growth in the SiO₂ and Si layers. Finally, the implications of the results are discussed for the prediction of fatigue damage in silicon MEMS structures.     

Onset of Surface Damage in Modular Orthopedic Implants: Influence of Normal Contact Loading and Stress-assisted Dissolution

Surface damage at interfaces of modular implants results from repeated fretting contacts between metallic surfaces in a corrosive environment. As a first step in understanding this complex process, multi-asperity contact experiments were conducted to characterize roughness evolution due to action of contact loads and exposure to a reactive environment. Cobalt–chromium specimens with surface roughness similar to modular implant were first subjected to only contact loading and subsequently, to alternating contact loads and exposure to reactive environment. During repeated normal contact loading, amplitude of surface roughness reached a steady value after decreasing during the first few cycles. However during the second phase surface roughness amplitude continuously evolved—decreasing during contact loading and increasing on exposure to corrosive environment. The increase in roughness amplitude during surface reaction depended on the magnitude of applied contact loads. A damage mechanism that incorporates contact-induced residual stress development and stress-assisted dissolution is proposed to elucidate the measured surface roughness evolution.     

Surface stress generation during formation of alkanethiol self-assembled monolayer (SAM)

A high resolution curvature interferometer [Wang, J., Shrotriya, P., Kim, K.S., 2006. Surface residual stress measurement using curvature interferometry. Experimental Mechanics 46 (1), 39–46] is utilized to measure surface stress development associated with formation of self-assembled monolayers (SAM) of octadecanethiols on macroscale domains (25 mm × 25 mm). Atomistic simulations are performed to investigate surface stress generation associated with SAM formation. The results of the molecular simulations are incorporated into the multiscale framework to understand the surface stress generation and curvature change observed during experiments at continuum scale.     

Local time—Temperature-dependent deformation of a woven composite

Moiré interferometry is utilized to investigate the time-temperature-dependent deformation of a woven composite substrate used in multilayer circuit board applications. Creep tests are performed at temperatures ranging from 27 to 70°C, and the resulting longitudinal and transverse displacement fields are measured via moiré interferometry. Measured displacement fields reveal the influence of fabric architecture on woven composite response. The deformation fields in the plane of the composite for loading along both warp and fill directions consist of a periodic arrangement of high-strain and low-strain regions in accordance to the interlacing bundle architecture. The deformation fields over the cross-section of the composite indicate that neighboring unit cells are subjected to equal and opposite bending moment even when the composite is loaded in uniaxial tension.     

Surface Residual Stress Measurement Using Curvature Interferometry

Surface roughness plays an important role in the delamination wear caused by rough surface contact. A recent dislocation model analysis predicts that nano-scale contacts of surface steps induce nucleation of dislocations leading to pro-load and anti-load dislocation segregation near the contact surface. Such dislocation segregation generates a sub-layer of tensile residual stress in a much thicker layer of compressive residual stress near the surface. The tensile sub-layer thickness is expected to be about 50 to 100 times the step height. In order to verify the predictions of the model analysis, contact experiments are carried out on polycrystalline aluminum surface to determine the existence of the tensile sub-layer. The variation of the residual stress along the thickness direction is measured using a newly developed high sensitivity curvature-measurement interferometer. The residual stress distribution measured with sub-nanometer spatial resolution indicates that contact loading leads to formation of a highly stressed sub-layer of tensile residual stress within a much thicker layer of compressive residual stress. Implications of tensile residual stress for delamination wear are discussed.     

Aptamer functionalized microcantilever sensors for cocaine detection

A cocaine-specific aptamer was used as a receptor molecule in a microcantilever-based surface stress sensor for detection of cocaine molecules. An interferometric technique that relies on measuring differential displacement between two microcantilevers (a sensing/reference pair) was utilized to measure the cocaine/aptamer binding induced surface stress changes. Sensing experiments were performed for different concentrations of cocaine from 25 to 500 μM in order to determine the sensor response as a function of cocaine concentration. In the lower concentration range from 25 to 100 μM, surface stress values increased proportionally to coverage of aptamer/cocaine complexes from 11 to 26 mN/m. However, as the cocaine concentration was increased beyond 100 μM, the surface stress values demonstrated a weaker dependence on the affinity complex surface coverage. On the basis of a sensitivity of 3 mN/m for the surface stress measurement, the lowest detectable threshold for the cocaine concentration is estimated to be 5 μM. Sensing cantilevers could be regenerated and reused because of reversible thermal denaturation of aptamer.     

Strategies for Positive Partial Transpose (PPT) States in Quantum Metrologies with Noise

Quantum metrology overcomes standard precision limits and has the potential to play a key role in quantum sensing. Quantum mechanics, through the Heisenberg uncertainty principle, imposes limits on the precision of measurements. Conventional bounds to the measurement precision such as the shot noise limit are not as fundamental as the Heisenberg limits, and can be beaten with quantum strategies that employ ‘quantum tricks’ such as squeezing and entanglement. Bipartite entangled quantum states with a positive partial transpose (PPT), i.e., PPT entangled states, are usually considered to be too weakly entangled for applications. Since no pure entanglement can be distilled from them, they are also called bound entangled states. We provide strategies, using which multipartite quantum states that have a positive partial transpose with respect to all bi-partitions of the particles can still outperform separable states in linear interferometers.     

Differential temperature sensors method for simultaneous determination of thermal conductivity and diffusivity

An attempt has been made to minimize the sources of error involved in the transient probe method for thermal conductivity determination. Two sensors (thermocouples) are mounted parallel to the needle probe at known distances. This modification makes it a device for simultaneous conductivity and diffusivity determination. Thermal conductivity and diffusivity for glycerine, dune sand and mustard seed are determined by this method. Results obtained are compared with those obtained by a calibrated transient probe for conductivity and by a parallel wire method for diffusivity. Analysis of the results prove it to be a better instrument over the traditional ones. The technique can also be used as a direct reading device for conductivity and diffusivity measurements.