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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
31

Étude de la déflexion électrochimique de micro-leviers fonctionnalisés d'une monocouche auto-assemblée électroactive

Castonguay, Catherine 06 1900 (has links)
No description available.
32

Simulation of the Molecular Interactions for the Microcantilever Sensors

Khosathit, Padet 11 1900 (has links)
Microcantilever sensor has gained much popularity because of its high sensitivity and selectivity. It consists of a micro-sized cantilever that is usually coated on one side with chemical/biological probe agents to generate strong attraction to target molecules. The interactions between the probe and target molecules induce surface stress that bends the microcantilever. This current work applied the molecular dynamics simulation to study the microcantilever system. Lennard-Jones potentials were used to model the target-target and target-probe interactions and bond bending potentials to model the solid cantilever beam. In addition, this work studied the effect of probe locations on the microcantilever deflection. The simulation results suggest that both target-target and target-probe interactions as well as the probe locations affect the arrangement of the bonds; in term of the bonding number, the area containing the bonded molecules, and the distances between them. All these factors influence the microcantilever deflection.
33

Adhesion and dissipation at nanoscale

Li, Tianjun 10 October 2013 (has links) (PDF)
In this thesis, we test some interactions involving surfaces processes at the nanometer scale. The experiments are conducted with a highly sensitive interferometric Atomic Force Microscope (AFM), achieving a resolution down to E-28m2/Hz for the measurement of deflection. Combined with original thermal noise analysis, this tool allows quantitative characterization of the mechanical response of micrometer and nanometer sized systems, such as microcantilevers or carbon nanotubes, on a large frequency range.The first part of my work deals with the viscoelasticity of the coating of AFM cantilevers. Evidenced by a 1/f thermal noise at low frequency, this phenomenon is present when a cantilever is coated with a metallic layer (gold, aluminium, platinium, etc...). Using the fluctuation dissipation theorem and Kramers Kronig relations, we extract the frequency dependance of this viscoelastic damping on a wide range of frequency (1Hz to 20kHz). We find a generic power law dependence in frequency for this dissipation process, with a small negative coefficient that depends on materials. The amplitude of this phenomenon is shown to be linear in the coating thickness, demonstrating that the damping mechanism takes its roots in the bulk of the metallic layer.The second part of my work tackles new experiments on the interaction of carbon nanotubes with flat surfaces. Using our AFM, we perform a true mechanical response measurement of the rigidity and dissipation of the contact between the nanotube and the surface, in a peeling configuration (the nanotube is partially absorbed to the substrate). The results of this protocol are in line with the dynamic stiffness deduced from the thermal noise analysis, showing an unexpected power law dependence in frequency for the contact stiffness. We suggest some possible physical origins to explain this behavior, such as an amorphous carbon layer around the nanotube.
34

Simulation of the Molecular Interactions for the Microcantilever Sensors

Khosathit, Padet Unknown Date
No description available.
35

Microrhéomètre sur puce pour l'étude de l'écoulement d'un liquide proche d'une surface liquide

Darwiche, Ahmad 06 September 2012 (has links)
Ce travail porte sur l'étude du comportement rhéologique de fluide en milieu confiné. Pour cela le levier d'un microscope à force atomique (AFM) est utilisé pour sonder les propriétés rhéologiques d'un fluide confiné entre deux surfaces : la surface d'une sphère collée à l'extrémité du levier et une surface plane sur lequel le fluide est déposé. Le dispositif expérimental est constitué du système de mesure d'un AFM et d'un piézoélectrique permettant d'approcher ou d'éloigner de la sphère la surface plane. Un modèle analytique permet d'extraire les propriétés rhéologiques du fluide confiné à partir de la déflexion du levier induite par le pincement du fluide. Cette méthode a été validée pour les fluides newtoniens. Par contre pour les fluides non-newtoniens comme par exemple la solution de polyacrylami de nous avons trouvé que la viscosité dépend de la distance D et que le cisaillement n'est pas le seul paramètre pertinent pour interpréter les propriétés rhéologiques. / This thesis focuses on the study of the rheological behavior of confined fluids. For this purpose, the microcantilever of an atomic force microscope (AFM) is used to probe the rheological properties of a fluid confined between two surfaces, the surface of a sphere glued to the free-end of the AFM microcantilever and a flat solid surface on which the fluid is deposited. The set-up consists of an AFM, an electrical system for the deflection measurement and a piezoelectric device to move the solid surface (approach, oscillation, etc.). An analytical model allows to determine the rheological properties of the confined fluid from the measurement of the microcantilever deflection due to the hydrodynamic force exerted by the fluid on the sphere.This method has been validated for Newtonian fluids. For non-Newtonian fluids, such as polyacrylamide solution, we found that the viscosity depends on the distance D between the sphere and the plane surface and the shear rate is not the only relevant parameter for interpreting the rheological properties.
36

Design and Development of Microstereolithography (MSL) System and Its Applications in Microfabrication of Polymer and Ceramic Structures

Goswami, Ankur January 2013 (has links) (PDF)
In the present era where MEMS (Micro Electro-Mechanical Systems) technology is in¬evitable from the perspective of applications in non-silicon based micro-devices (such as biosensors, microfluidics, microvalves etc.), it is imperative to develop different micro¬fabrication technologies which are simple in operation, have low operational cost and high versatility in terms of incorporating different materials. The microfabrication tech¬nologies (e.g: bulk micromachining, surface micromachining, X-ray LIGA (lithoqraphie galvanoformung abformung) etc.), which exist commercially are mostly limited to sili¬con based technologies. They are either constrained in fabricating complex geometry in micro dimension or have high operational cost. Microstereolithography (MSL) is one such rapid prototyping technique, which can satisfy the above requirements to a larger extent. MSL h8B evolved in the l8Bt decade from conventional stereolithographic (SLA) technique, which involves the free-form microfabrication of a UV sensitive liquid resin layer by layer photo-polymerization process, when it is exposed to UV irradiation accord¬ing to the predefined CAD (Computer Aided Design). However, this technique is not limited to polymer microfabrication and it h8B an immense potential to fabricate com¬plex 3D structures of ceramics in micro dimension. In this thesis, the primary focus is on developing an in house built scanning b8Bed MSL system indigenously and to explore the possibility of micro fabrication of different materials (from polymer to ceramics involving different routes. In addition, polymer micro cantilever h8B been fabricated using this technique and its application to surface stress me8Burement h8B been demonstrated. The thesis comprises of eight chapters. The following section describes the summary of the individual chapters. Chapter 1 describes the introduction and background literature of this technol¬ogy. A brief review on MSL technology developed by various research groups and their achievements h8B been listed. Since photopolymerizable resin is the primary material to fabricate micro dimensional structures, the rate of photopolymerization is an impor¬tant phenomena which requires an attention before choosing the photopolymerizable resin. Further, this chapter also describes the photoinitiation principles and the type of photo initiators (PI) which help to photopolymerize the resin in order to fabricate micro dimensional polymer structures. In addition, this chapter also gives a glimpse of applications of this technology in fabrication of micro cantilever b8Bed sensors. The later part of the chapter focused on the microfabrication of ceramic from colloidal and met¬alorganic routes in brief. In Chapter 2, the design of the in house built MSL system and its working princi¬ples including various optical issues have been addressed. Several research groups have attempted to optimize photopolymerization parameters to incre8Be the throughput of the scanning b8Bed MSL systems through modified beam scanning techniques. Efforts in reducing the curing line width in order to get low feature size have been implemented through high numerical aperture (NA) optical setups. However, the intensity contour symmetry and the depth of field of focus have led to grossly non-vertical and non-uniform curing profiles. The focus of the work h8B been to exploit the rich potential of photoreactor scanning system in achieving desired fabrication modalities (minimum curing width, uniform depth profile, and vertical curing profile) even with a reduced NA optical setup and a single movable stage. The present study tries to manipulate to its advantage the effect of optimized lower photoinitiator (PI) concentration ([c]) in reduc¬ing the minimum curing width to 10-15 jJm, even with the higher spot size (21.4 jJm) rv through a judiciously chosen gmonomer UPIi' system. In this chapter, two different cl8BS of multifunctional acrylates (1,6 Hexane diol diacrylate (HDDA) and Trimethylol propanetriacrylate (TMPTA)) and one monofunctional methacrylate (methyl mathacry¬late (MMA)) have been chosen to explore their fabricability in micro dimensions using this MSL technology, by varying the various operational parameters including the type and the concentration of the PI. Chapter 3 deals with the application of this technology in micro cantilever based sensors. Microcantilever based sensors have been explored for several decades for their application in bio-molecular or explosive detection, chemical sensing etc. Due to the adsorption of molecular species on the cantilever surface, differential surface stress gen¬erates between the top and bottom surface of the cantilever. Depending on the type of stress (tensile or compressive) generated, the cantilever bends accordingly. The, novel diffraction based deflection method has been proposed in order to measure the deflection profile accurately for low dimensional structures. To prove this method, a dual mi¬crocantilever structure with sufficiently low gap (100 f.lm) has been fabricated using the developed MSL set up, such that diffraction occurs during transillumination by spherical wavefronts. Among the two micro cantilevers one was fabricated bent with a specific di¬mension with respect to the other. The cantilever material was chosen as poly HDDA for its low elastic modulus in order to achieve high sensitivity. From the obtained diffraction pattern, the bent profile of the each cross section of one cantilever corresponding to the other has been measured. This proposition will enable to measure surface stress at each cross section of the cantilever depending on the adsorbed analyte molecule adsorption. In Chapter 4, an effort has been made to improve the thermal, thermo mechanical and mechanical properties of the cantilever material (poly HDDA). The sensitivity of a micro cantilever depends precisely on fabrication and material aspects. The former de¬pends on the aspect ratio of the structure and can be controlled by fabrication parameters whereas the latter is inherently limited by the choice of the material. The properties of the material which impact the applicability are elastic modulus, Poisson's ratio, thermal expansion and thermal stability. Hence, these properties are studied for poly HDDA. However, the properties are not completely satisfactory for only poly HDDA (PHDDA) since, PHDDA will fail for high surface stress measurement (>275 mN/m). Hence, it h8B been copolymerized with MMA with an intention to improve the above mentioned properties and to determine the best composition for the micro cantilever application. It is observed by Finite Element Analysis (FEM) that Phpm5050 (HDDA:MMA(50:50)) composition shows optimum sensitivity when reliability is concerned for me8Buring high surface stress (275 mN/m). Chapter 5 bridges Chapter 2 and Chapter 6. Chapter 2 highlights the polymer mi¬crofabrication where8B, Chapter 6 deals with the microfabrication of ceramics. In order to fabricate ceramic micro objects by MSL, ceramic particles need to be blended with a photopolymerizable monomer followed by l8Ber induced photopolymerization . Under l8Ber irradiation, the monomer gets cured and traps the ceramic particles. Thus near net shape of green ceramic structures are 0 btained. After achieving the near net shape, it is important to remove the polymer, which acts 8B the binder for the green ceramic body. This debinding should be diffusion controlled so 8B to achieve defect free micro ceramics. Here two multifunctional monomers (HDDA and TMPTA) have been chosen 8B a b8Be monomer for fabricating ceramics. Therefore it is essential to understand the debinding mechanism of these polymers. However, (HDDA) h8B high shrinkage upon polymeriza¬tion with low rate of polymerization kinetics and low viscosity where8B the properties of (TMPTA) are exactly opposite. Hence, in order to optimize these properties, copoly¬merization of HDDA and TMPTA h8B been carried out for different compositions and their thermal properties have been investigated to understand the degradation mech¬anism. This chapter deals with the mechanism of thermal degradation by model free kinetic methods with an intention to determine the optimum composition of HDDA and TMPTA copolymer, to used 8B the b8Be monomer material for ceramic microfabrication. Besides, the debinding strategy is also discussed b8Bed on the degradation profile of the optimum composition. TH20S0(TMPTA: HDDA(20:S0)) is found to be the ideal com¬position to fabricate ceramic micro-component by MSL since its degradation is diffusion controlled in N 2 atmosphere. Chapter 6 describes the methodology of microfabrication of ceramics by the de-veloped MSL technique. A colloidal approach has been adopted to fabricate ceramics in micro-dimensions. Two different ceramics have been chosen, which have potential applications in structural (alumina) and functional (Lead Iron Niobate (PFN))aspects. Before fabricating ceramic micro-objects, ceramic particles need to be blended in the monomer suspension in the presence of dispersant at an optimum solids loading. Opti¬mization of solids loading is important in view of low dimensional shrinkage after sin¬tering. However, lower loading leads to higher shrinkage whereas higher loading would increase the viscosity of the suspension and make the suspension inconvenient to deal with. Hence, rheological studies have been carried out to optimize the solids loading and dispersant concentration. 40 vol% alumina and 35 vol% PFN are found to be the highest achievable solids loading for the chosen monomer (TH2080) composition. This chapter also describes the limitation involved in ceramic microfabrication depending on their scattering factors during laser irradiation. The chapter demonstrates the fabrica¬tion methodology of several complex ceramic(alumina and PFN) micro-objects by the in house built MSL instrument. Chapter 7 investigates the possibility of microfabrication of ceramics from metalor¬ganic precursor. In this route, titanium metal-organic (Ti-n butoxide) precursor has been chosen which is stabilized by the addition of chelating monomer (2-( methacryloyloxy) ethyl acetoacetate). Following this, the crosslinker and photoinitiators have been added to form Ti photoresist which is coated on top of the bare silicon substrate by spin coating to achieve specific thickness. The coated silicon wafer by the above photoresist has been patterned by selectively exposure in the MSL setup. The cured patterns are washed and heat treated at high temperature in order to 0 btain the net shape of the Ti02 pattern of polycrystalline rutile phase. It is observed this route is advantageous in terms of reduc¬ing curing dimension (curing width 14 f.lm) than the colloidal route (curing width more than 80 f.lm ) of fabrication of ceramics where the scattering factor greatly influences the dimensions of the feature size. The key findings and future aspects are summarized in the Chapter 8. The work reported in this thesis has been carried out by the candidate as part of the Ph.D. programme. He hopes that this would constitute a worthwhile contribution towards developing an MSL technique and its aspects in micro fabrication of polymer and ceramic structures of any complex shape and its possible applications in microdevices.
37

Study Of The Effect Of Elasticity Of The Added Mass In Mass Sensing Using Resonant Peak Shift Technique

Polapragada, Hara Krishna 08 1900 (has links) (PDF)
Micromachined biosensors are used in chemical and biological applications. A biosensor which uses mass based transduction is called a mass sensor. Mass sensors are used to detect extremely small mass of biomolecules such as proteins, viruses or even parts of DNA in the range of femtograms (10-15 gm) to zeptograms (10−21 gm). Highly effective and reliable microcantilevers are used for detecting the mass of biomolecules using either static deflection or dynamic resonant peak shifts. The main objective of our work is to investigate the effect of elasticity of the attached mass on the shift in the resonant frequency and examine the validity of the rigid mass assumption used in the literature. The natural frequencies of a resonator are either found by solving the governing differential equation or approximately using Rayleigh-Ritz method. The mass of a body, attached to a resonator beam is determined using resonant frequency shift method. In our study, we derive an analytical expression for ‘δm’ based on the shift in frequency ‘δf’ that accounts for the elasticity of the added mass and the location of the mass on the beam. We study the simplest model to incorporate these effects where the added mass is itself modeled as a single degree of freedom spring-mass system. The entire system is represented as a 2-DOF lumped model of cantilever and the attached elastic mass. The natural frequencies are obtained using eigenvalue analysis. We study the mass estimation of Escherichia Coli (E. Coli), a food borne pathogen, using experimental results reported in the literature. We treat E.Coli as an elastic mass and model it as a single degree of freedom system to account for its elasticity. We use the elastic model as well as the rigid mass model to check the results available in the literature and point out the difference that results in mass estimation using the two models. To demonstrate the effect of elasticity on mass sensing using the resonant peak shift technique, we conduct mesoscale experiments. Since the fundamental principle does not depend on any phenomenon exclusively dependent on micro scales, the mesoscale experiments are justified. For this purpose, an experimental set-up with metallic cantilevers and flexible rubber strands as attached masses are used. We also use our experimental set-up to study the effect of positional inaccuracy of the added mass (rigid) in the computation of its mass from the shift in the resonance frequency. The results obtained show that elasticity of the added mass as well as its position on the resonator affect the computed mass but this effect is dependent on the relative stiffness and mass of the resonator and the added mass. We also observe the limitations of the experiments in carrying out studies over the desired range of parameters. We also create a computational model of the system and carry out simulations to explore a larger range of parameter values. In particular, we create an FEM model of our system in ANSYS, and carry out modal analysis for the cantilever beam resonator with and without the added mass, varying the relative stiffness and mass of the two components (the cantilever beam and the added mass). We compare the results of shift in the resonant frequency with those obtained from the rigid mass model. The results show the effect of elasticity clearly in certain ranges of relative stiffness and mass.
38

A micromechanical investigation of proton irradiated oxide dispersion strengthened steels

Jones, Christopher A. January 2016 (has links)
This thesis was most concerned with the mechanical response to irradiation of two in-house produced oxide dispersion strengthened (ODS) steels and two non-ODS coun- terparts. The steels, manufactured by Dr. M. J. Gorley (University of Oxford), were me- chanically alloyed from gas-atomised Fe-14Cr-3W-0.2Ti, with the addition of 0.25Y<sub>2</sub>O<sub>3</sub> powder in the case of the ODS variants. The powders were hot isostatic pressed at consolidation temperatures of 950 &deg;C and 1150 &deg;C. The four steels were designated 14WT 950 (non-ODS), 14YWT 950 (ODS), 14WT 1150 (non-ODS) and 14YWT 1150 (ODS), and were used in the as-produced condition. Initially, the macroscale elastic modulus and yield stress were determined using a four-point flexure test, employing digital image correlation (DIC) as a strain gauge. The microcantilever size eects were then characterised, and it was determined that the yield stress signicantly diverged from macroscale values at microcantilever beam depths of &LT; 4.5 &mu;m. Using knowledge of this, the in-house produced alloys were irradiated with 2 MeV protons at the Surrey Ion Beam Centre (University of Surrey, UK) to a displacement damage of &Tilde; 0.02 dpa and 0.2 dpa (Bragg peak). This was to produce a deep irradiated layer for the fabrication of large microcantilevers with reduced size effects. The cross-sectional surface of the irradiated layer was then exposed and inclined linear arrays of 250 nm deep indents were placed across the damage prole. 14WT 1150 (non-ODS) revealed a clear proton damage prole in plots of hardness against irradiation depth, 14WT 950 (non-ODS) also showed modest hardening in the region of the Bragg peak. No appreciable hardening was observed in either 14YWT specimens, attributed to the fine dispersion of nanoscale oxides providing a high number density of defect sink sites. However, a large bimodal variation in hardness was measured in both ODS variants. This was investigated using EBSD and EDX, and was determined to be caused by a pronounced heterogeneity of the microstructure. While Hall-Petch strengthening and changes in the local chemistry had some effect on the measured hardness, the most likely cause of the large variation in local hardness was heterogeneity in the nanoscale oxide population. Microcantilevers were fabricated out of the irradiated layer cross-section in 14WT 1150 and 14YWT 1150. Larger microcantilevers, with &Tilde; 5 &mu;m beam depth, were placed with their beam centre at &Tilde; 0.026 dpa. Smaller microcantilevers, with &Tilde; 1.5 &mu;m beam depth, were placed with their beam centre at the Bragg peak, 0.2 dpa. Both the large and the small microcantilevers fabricated in 14WT 1150 (non-ODS) displayed significant irradiation hardening. In the ODS variant, 14YWT 1150, irradiation hardening appeared to be reduced. The work in this thesis successfully showed that it was possible to extract a close approximation of the macroscale yield stress from shallow irradiated layers, providing that the irradiation condition is carefully chosen in response to known size dependent behaviour. This thesis also investigated the size dependent behaviour of microcantilevers using a lengthscale dependent crystal plasticity UMAT, developed by Dunne et al. and implemented within ABAQUS 6.14-2 commercially available nite element software. The simulation of the GND density evolution with increasing plastic strain allowed their contribution to the microcantilever size effect, through mobile dislocation pinning, to be determined. This novel approach to modelling size effects in three dimensional finite element microcantilever models demonstrated that while it was possible to simulate a lengthscale-dependent response in finite element microcantilever models, the constitutive equation for the plastic velocity gradient needs to be more physically based in order the match the experimentally derived results; for example, a lengthscale-dependent term relating to the dislocation source density of the material. Although the apparent reduction of irradiation hardening in ODS in-house produced alloys showed great promise, these alloys also displayed a large amount of scatter in measured hardness and yield stress, attributed to the pronounced heterogeneity in the microstructure. Alloys with such signicant microstructural heterogeneity are not suitable for engineering or commercial use.
39

Towards the nanomechanical actuation and controlled assembly of nanomaterials using charge-transfer reactions in electroactive self-assembled monolayers

Norman, Lana 07 1900 (has links)
Les microcantileviers fonctionnalisés offrent une plateforme idéale pour la nano- et micro-mécanique et pour le développement de (bio-) capteurs tres sensible. Le principe d’opération consiste dans des évènements physicochimiques qui se passent du côté fonctionnalisé du microcantilevier induisant une différence de stress de surface entre les deux côtés du cantilevier qui cause une déflexion verticale du levier. Par contre, les facteurs et les phénomènes interfacials qui régissent la nature et l'intensité du stress de surface sont encore méconnus. Pour éclaircir ce phénomène, la première partie de cette thèse porte sur l'étude des réactions de microcantileviers qui sont recouverts d'or et fonctionnalisés par une monocouche auto-assemblée (MAA) électroactive. La formation d'une MAA de ferrocènylundécanethiol (FcC11SH) à la surface d'or d'un microcantilevier est le modèle utilisé pour mieux comprendre le stress de surface induit par l’électrochimie. Les résultats obtenus démontrent qu'une transformation rédox de la MAA de FcC11SH crée un stress de surface qui résulte dans une déflexion verticale du microcantilevier. Dépendamment de la flexibilité du microcantilevier, cette déflexion peut varier de quelques nanomètres à quelques micromètres. L’oxydation de cette MAA de FcC11SH dans un environnement d'ions perchlorate génère un changement de stress de surface compressive. Les résultats indiquent que la déflexion du microcantilevier est due à une tension latérale provenant d'une réorientation et d'une expansion moléculaire lors du transfért de charge et de pairage d’anions. Pour vérifier cette hypothèse, les mêmes expériences ont été répéteés avec des microcantileviers qui ont été couverts d'une MAA mixte, où les groupements électroactifs de ferrocène sont isolés par des alkylthiols inactifs. Lorsqu’un potentiel est appliqué, un courant est détecté mais le microcantilevier ne signale aucune déflexion. Ces résultats confirment que la déflexion du microcantilevier est due à une pression latérale provenant du ferrocènium qui se réorganise et qui crée une pression sur ses pairs avoisinants plutôt que du couplage d’anions. L’amplitude de la déflexion verticale du microcantilevier dépend de la structure moléculaire de la MAA et du le type d’anion utilisés lors de la réaction électrochimique. Dans la prochaine partie de la thèse, l’électrochimie et la spectroscopie de résonance de plasmon en surface ont été combinées pour arriver à une description de l’adsorption et de l’agrégation des n-alkyl sulfates à l’interface FcC11SAu/électrolyte. À toutes les concentrations de solution, les molécules d'agent tensio-actif sont empilées perpendiculairement à la surface d'électrode sous forme de monocouche condensé entrecroisé. Cependant, la densité du film spécifiquement adsorbé s'est avérée être affectée par l'état d'organisation des agents tensio-actifs en solution. À faible concentration, où les molécules d'agent tensio-actif sont présentes en tant que monomères solvatés, les monomères peuvent facilement s'adapter à l’évolution de la concentration en surface du ferrocènium lors du balayage du potential. Cependant, lorsque les molécules sont présentes en solution en tant que micelles une densité plus faible d'agent tensio-actif a été trouvée en raison de l'incapacité de répondre effectivement à la surface de ferrocenium générée dynamiquement. / Surface-functionalized microcantilevers provide an ideal platform for nano- and micro-mechanical actuation and highly sensitive sensing technologies. The basic principle of operation is that a chemical or physical event occurring at the functionalized surface of one side of the cantilever generates a surface stress difference (between the active functionalized and passive non-functionalized sides) that causes the cantilever to bend away from its resting position. However, the factors and phenomena contributing to both the nature and magnitude of the surface stress are not well understood. To this end, the first part of this thesis focused on investigating the potential-controlled actuation and surface stress properties of free-standing gold-coated microcantilevers functionalized with a redox-active self-assembled monolayer (SAM). A ferrocenylundecanethiolate (FcC11SAu) SAM on a gold-coated cantilever was used as a model system to investigate the surface stress generated by faradaic chemistry. The data obtained clearly demonstrates that the electrochemical transformation of a ferrocene moiety in a monomolecular organic film can generate a surface stress change of sufficient magnitude to deflect a microcantilever. In fact, depending on the flexibility of the microcantilever, the mechanical deflection resulting from the redox transformation of the surface-tethered ferrocene can range on the order of nanometers to micrometers. The oxidation of the FcC11SAu SAM in perchlorate electrolyte generates a compressive surface stress change. The microcantilever deflection is driven by the lateral tension resulting from molecular reorientation/volume expansion accompanying the charge-transfer and ion-pairing events. To verify this hypothesis, mixed SAM-modified microcantilevers, in which the electroactive ferrocenes are isolated from one another by an inert n-alkylthiolate matrix, were investigated. Under an applied potential, a Faradaic current was measured, but no microcantilever beam deflection was observed. This finding confirms that the cantilever responds to the lateral pressure exerted by an ensemble of re-orienting ferrocenium-bearing alkylthiolates upon each other rather than to individual anion pairing events. Changes in molecular structure and anion type can also be used to modulate the extent of micromechanical motion. In the next part of the dissertation, electrochemical measurements and surface plasmon resonance spectroscopy were combined to present a description of the adsorption and aggregation of n-alkyl sulfates at the FcC11SAu/electrolyte interface. At all bulk solution concentrations, the surfactant moieties packed perpendicular to the electrode surface in the form of an interdigitated condensed film. However, the density of the specifically adsorbed film was found to be affected by the organizational state of the surfactants in solution. At low concentrations, where the surfactant molecules are present as solvated monomers, the monomers can readily adapt to the changing ferrocenium concentration with the potential potential scan. However, when the molecules are present as micellar structures in solution, a lower surfactant packing density was found because of the inability to respond effectively to the dynamically generated surface ferroceniums. This research demonstrates the potential utility of charge-transfer interactions for organizing materials at solid interfaces and effecting micromechanical actuation using an electrifical stimulus.
40

Adhesion and dissipation at nanoscale / Adhésion et dissipation à l'échelle nanométrique

Li, Tianjun 10 October 2013 (has links)
Ce travail de thèse est dédié à l'étude de quelques phénomènes de surface impliquant des processus d'interactions à l'échelle nanométrique. Les expériences sont réalisées à l'aide un microscope à force atomique (AFM) à grande sensibilité, utilisant un interféromètre différentiel permettant d'atteindre une résolution de E-28m2/Hz dans la mesure de la déflexion de la sonde de force. Combiné à une approche originale d'analyse du bruit thermique, cet outil permet une caractérisation quantitative de la réponse mécanique de systèmes de taille micrométrique et nanométrique, tel que des micro-leviers ou des nanotubes de carbone, sur une large plage de fréquence.La première partie de mon travail porte sur la viscoélasticité du revêtement de leviers AFM. Mis en évidence par un bruit thermique en 1/f à basse fréquence, ce phénomène est présent lorsque le micro-levier est recouvert d'une couche nanométrique de métal (or, aluminium, platine, etc.) À l'aide du théorème fluctuation-dissipation et des relations de Kramers-Kronig, nous mesurons la dépendance en fréquence de cet amortissement viscoélastique dans une large gamme de fréquence (1Hz à 20 kHz. Nous observons une dépendance en fréquence générique sous la forme d'une loi de puissance pour ce processus de dissipation, avec un petit coefficient négatif qui dépend du matériau considéré. L'amplitude de cet effet est linéaire avec l'épaisseur du revêtement, démontrant ainsi que le mécanisme de dissipation est une propriété du volume de la couche métallique plutôt que de ses interfaces.La deuxième partie de mon travail se concentre sur de nouvelles expériences sur l'interaction de nanotubes de carbone avec des surfaces planes. En utilisant notre AFM, nous réalisons une mesure directe de la réponse mécanique (raideur, dissipation) du contact entre le nanotube et la surface, dans une géométrie de pelage (le nanotube est partiellement adsorbé sur la surface). Les résultats de ce protocole sont en accord avec la mesure de la raideur dynamique déduite de l'analyse du bruit thermique, démontrant une dépendance inattendue en loi de puissance de la raideur du contact en fonction de la fréquence. Nous proposons quelques origines physiques possibles pour expliquer ce comportement, tel qu'une couche de carbone amorphe autour du nanotube. / In this thesis, we test some interactions involving surfaces processes at the nanometer scale. The experiments are conducted with a highly sensitive interferometric Atomic Force Microscope (AFM), achieving a resolution down to E-28m2/Hz for the measurement of deflection. Combined with original thermal noise analysis, this tool allows quantitative characterization of the mechanical response of micrometer and nanometer sized systems, such as microcantilevers or carbon nanotubes, on a large frequency range.The first part of my work deals with the viscoelasticity of the coating of AFM cantilevers. Evidenced by a 1/f thermal noise at low frequency, this phenomenon is present when a cantilever is coated with a metallic layer (gold, aluminium, platinium, etc...). Using the fluctuation dissipation theorem and Kramers Kronig relations, we extract the frequency dependance of this viscoelastic damping on a wide range of frequency (1Hz to 20kHz). We find a generic power law dependence in frequency for this dissipation process, with a small negative coefficient that depends on materials. The amplitude of this phenomenon is shown to be linear in the coating thickness, demonstrating that the damping mechanism takes its roots in the bulk of the metallic layer.The second part of my work tackles new experiments on the interaction of carbon nanotubes with flat surfaces. Using our AFM, we perform a true mechanical response measurement of the rigidity and dissipation of the contact between the nanotube and the surface, in a peeling configuration (the nanotube is partially absorbed to the substrate). The results of this protocol are in line with the dynamic stiffness deduced from the thermal noise analysis, showing an unexpected power law dependence in frequency for the contact stiffness. We suggest some possible physical origins to explain this behavior, such as an amorphous carbon layer around the nanotube.

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