Extended Identification of Mechanical Parameters and Boundary Conditions by Digital Image Correlation

Abstract This paper represents a further contribution to the study of identification procedures for material mechanics resting on kinematic measurements provided by 2D Digital Image Correlation (DIC) at the microscale. Reference is made to non-conventional experiments on adhesively bonded assemblies industrially manufactured for aerospace applications. For calibration purposes a local approach is considered under plane stress conditions, focusing on a small sub-domain on the sample surface, in which mixed mode debonding is monitored. As a novelty, both the (cohesive) mechanical parameters of the interface and the actual boundary conditions prescribed at different time instants during the test are considered as unknowns to be estimated on the basis of full-field data. In this way, data smoothing and parameter identification procedures, so far usually performed in a sequence, are tackled simultaneously in a coupled framework. Since the inverse problem generalized as mentioned above turns out to be severely ill-posed, suitable regularizing provisions are applied, concerning the a priori regularity of (kinematic) displacement fields, from which boundary data are sampled, and the equilibrium (Neumann) conditions along the cracked part of the interface

Charge redistribution in electrochemically-actuated mechanical sensors

International audienceMany proofs of concept studies have established the mechanical sensitivity of functionalized microcantilevers to a large spectrum of target molecules. However, moving to real-life applications also requires the monitored mechanical effect to be highly specific. Moving towards more specificity in cantilever-based sensing, monitoring the mechanical response of electrochemically actuated microcantilevers is then thought to provide a fast, reliable and complementary experimental information to the long-time cantilever bending measurement for the detection of target molecules. Full-field measurements are therefore used to investigate the way the electro-elastic coupling is altered when a microcantilever undergoes decane-thiol adsorption. The proposed technique reveals that the latter results in a charge density redistribution along the cantilever in addition to the local surface passivation. Focusing on the cantilever tip displacement under electrochemical actuation, this redistribution partially compensates the electro-elastic coupling alteration due to the surface passivation, therefore possibly yielding an ambiguous detection result. This effect should be taken into account for the optimal design of specific electrochemically actuated mechanical sensors

Indirect Electrografting of Aryl Iodides

International audienceThe electrografting of 4-iodonitrobenzene that is not possible directly is demonstrated whilst that of 5-iodo-2-amino-pyridine, 4-iodoaniline and iodobenzene is performed with a decrease of overpotential > 2 V. The electrografting of aryl iodides is achieved through a iodine abstraction reaction: in the presence of a sterically hindered diazonium salt (2,6-dimethylbenzenediazonium), the aryl iodide is grafted to gold at the much less negative reduction potential of the diazonium salt

Multiple wavelengths reflectance microscopy to study the multi-physical behavior of MEMS

International audienceIn order to characterize surface chemomechanical driving micro-electro-mechanical systems (MEMS) behavior, we propose herein a method to simultaneously obtain a full kinematic field describing the surface displacement and a map of its chemical modification from optical measurements. Using a microscope, reflected intensity fields are recorded for two different illumination wavelengths. Decoupling the wavelength-independent and -dependent contributions to the measured relative intensity changes then yields the sought fields. This method is applied to the investigation of the electro-elastic coupling, providing images of both the local surface electrical charge density and the device deformation field

Optical Nanoimpacts of Dielectric and Metallic Nanoparticles on Gold Surface by Reflectance Microscopy: Adsorption or Bouncing?

International audienceOptical modeling coupled to experiments show that a microscope operating in reflection mode allows imaging, through solutions or even a microfluidic cover, various kinds of nanoparticles, NPs, over a (reflecting) sensing surface, here a gold (Au) surface. Optical modeling suggests that this configuration enables the interferometric imaging of single NPs which can be characterized individually from local change in the surface reflectivity. The interferometric detection improves the optical limit of detection compared to classical configurations exploiting only the light scattered by the NPs. The method is then tested experimentally, to monitor in situ and in real time, the collision of single Brownian NPs, or optical nanoimpacts, with an Au-sensing surface. First, mimicking a microfluidic biosensor platform, the capture of 300 nm FeOx maghemite NPs from a convective flow by a surface-functionalized Au surface is dynamically monitored. Then, the adsorption or bouncing of individual dielectric (100 nm polystyrene) or metallic (40 and 60 nm silver) NPs is observed directly through the solution. The influence of the electrolyte on the ability of NPs to repetitively bounce or irreversibly adsorb onto the Au surface is evidenced. Exploiting such visualization mode of single-NP optical nanoimpacts is insightful for comprehending single-NP electrochemical studies relying on NP collision on an electrode (electrochemical nanoimpacts)

Single Nanoparticle Growth from Nanoparticle Tracking Analysis: From Monte Carlo Simulations to Nanoparticle Electrogeneration

International audienceBy scrutinizing the trajectory of individual nanoparticles (NPs) in solution, NP tracking analysis (NTA) allows sizing individual NPs and providing meaningful complementary information to single NP electrochemistry.H erein, am odel is developed to extend NTAt oa llow dynamic NP sizing and to analyze the kinetics of growth of NPs in solution. Interpreting the NP trajectories as scaled Brownian motion, Monte Carlo simulations produce stochastic trajectories of growing NPs (under diffusion-controlled growth). These trajectories are grounds for determining as trategy to estimate the growth parameters of individual NPs from the time evolution analysis of the mean square displacement (MSD) curves. In particular,w ee valuate the accuracy and precision of the parameter estimates from MSD analysis. In addition, the strategy is illustrated to depict the homogeneous electrosynthesis of silver NPs from the oxidation of as acrificial Ag ultramicroelectrode (UME) in Fe 2 + solution

Bimodal Electrochemiluminescence Microscopy of Single Cells

Electrochemiluminescence (ECL) microscopy is an emerging technique with new applications such as imaging of single entities and cells. Herein, we have developed a bimodal and bicolor approach to record both positive ECL (PECL: light-emitting object on dark background) and shadow label-free ECL (SECL: nonemissive object shadowing the background luminescence) images of single cells. This bimodal approach is the result of the simultaneous emissions of [Ru(bpy)3]2+ used to label the cellular membrane (PECL) and [Ir(sppy)3]3- dissolved in solution (SECL). By spectrally resolving the ECL emission wavelengths, we recorded the images of the same cells in both PECL and SECL modes using the [Ru(bpy)3]2+ (?max = 620 nm) and [Ir(sppy)3]3- (?max = 515 nm) luminescence, respectively. PECL shows the distribution of the [Ru(bpy)3]2+ labels attached to the cellular membrane, whereas SECL reflects the local diffusional hindrance of the ECL reagents by each cell. The high sensitivity and surface-confined features of the reported approach are demonstrated by imaging cell-cell contacts during the mitosis process. Furthermore, the comparison of PECL and SECL images demonstrates the differential diffusion of tri-n-propylamine and [Ir(sppy)3]3- through the permeabilized cell membranes. Consequently, this dual approach enables the imaging of the morphology of the cell adhering on the surface and can significantly contribute to multimodal ECL imaging and bioassays with different luminescent systems

Couplage électro-elastique et adsorption : vers une nouvelle instrumentation en chimie analytique

On utilise des poutres de dimensions micrométriques comme capteurs de leur environnement. Toute modification de l'état électrochimique d'une face introduit alors une flexion du levier. On a montré par ailleurs qu'en utilisant un dispositif interférométrique de mesure de champ et une technique d'identification adaptée, on peut construire une modélisation du couplage électro-élastique. On montre ici comment la relation de couplage est modifiée par l'adsorption de molécules neutres à la surface, et on propose d'exploiter cet effet en chimie analytique

Electrochemical Investigation of Nitinol/Tantalum Hybrid Surfaces Modified by Alkylphosphonic Self-Assembled Monolayers

The surface characteristics of bare and modified nickel-titanium samples (NiTi) are investigated by spectroscopic, microscopic and electrochemical techniques. The successful electrodeposition of a tantalum coating on NiTi and the effective grafting of 1-dodecylphosphonic acid SAMs on both pristine and Ta-covered NiTi surfaces are evidenced and quantified by XPS and SEM. Cyclic voltammetry performed on the different NiTi-based electrodes highlights their specificities regarding electron transfer to a redox probe present in solution (here ruthenium(III) hexamine). Finally, the samples electrochemical characteristics at a local scale are investigated by scanning electrochemical microscopy (SECM). The impact of the surface modifications on mass transport of the redox probe is analyzed through approach curves in the feedback mode, while the recording of current maps in feedback as well as in substrate-generation/tip-collection modes leads to the qualitative identification of electrochemically-active areas corresponding to precursor pitting corrosion sites

Identification du couplage électro-élastique à partir de mesures de champs régularisées par les conditions d'équilibre

Les capteurs micromécaniques présentent de grands intérêts dans les domaines de la biologie et chimie. Leur stimulation électrochimique permet d'améliorer la mesure de flexion induite par l'adsorption de molécules ainsi que la reproductibilité des mesures. On modélise ici le couplage électro-élastique par une couche virtuelle d'épaisseur très petite devant celle du levier et contrainte à se déformer avec celui-ci. Afin de déterminer les paramètres mécaniques de ce système une méthode d'identification et régularisation à partir de mesures de champs est proposée