Dissertationen zum Thema „Interface measurements“

Thesis (M.S.)--University of Missouri-Columbia, 2005.
The entire dissertation/thesis text is included in the research.pdf file; the official abstract appears in the short.pdf file (which also appears in the research.pdf); a non-technical general description, or public abstract, appears in the public.pdf file. Title from title screen of research.pdf file viewed on (December 12, 2006) Includes bibliographical references.

This dissertation describes the development of atomic force microscope cantilevers as surface stress sensors for monitoring surface processes at the solid-liquid interface. Micromechanical bending-beams are highly sensitive stress sensors; stress changes as small as 10^-4Nm^-1 can be detected using this type of bending-beam, whereas typical stress changes associated with monolayer processes are ˜0.1-1Nm^-1. As well as offering high sensitivity, micromechanical cantilevers have a fast response time (˜0.5ms in liquids) which means they are ideally suited for fast stress measurements. Textured (111) surfaces were prepared by thermal evaporation of Au onto one face of the Si₃N₄ cantilevers. These cantilevers were used as electrodes to monitor the stress changes associated with electrochemical processes, in conjunction with electrochemical measurements such as cyclic voltammetry and chronoamperometry. The potential-dependent adsorption of C1^- and I^- anions gave rise to stress changes of ˜0.5-1Nm^-1, and in both cases, adsorption of the anion was associated with an increase in compressive surface stress. Underpotential deposition (UPD) of Pb and Ag on Au(111) has been studied in detail. For Pb UPD on Au(111) a compressive stress change of ˜1Nm^-1 was measured on deposition of one monolayer. More detailed features in the surface stress-potential curve have been directly related to features in the cyclic voltammogram and known structural processes such as the potential-dependent compression of the Pb monolayer. The measured stress changes for Ag UPD on Au(111) were also ˜1Nm^-1 and did not display a strong dependence on the nature of the anion present in the electrolyte.

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An instrumented spar buoy, Met-on-a-Stick (MOAS), was designed, deployed, and validated for measuring the air sea interface processes at multiple levels. This system was deployed in June 2010 off the coast of California, and January and February 2011 in Monterey Bay. The system provides mean measurements of wind, temperature, and humidity at multiple levels within 3 m above the sea surface and measurements of sea surface temperature at three levels below ocean surface. It is small enough to be deployed and retrieved by two people. This thesis work introduces the design and the instrumentation of the system and evaluates the ability of the system for characterizing near-surface vertical variations of the marine boundary layer. The results indicate that the platform performance is as expected and is capable of providing measurements to characterize the fine variations close to the air-sea interface. We foresee a broad use of the MOAS in the future due to its low-cost and ease of deployment. Future improvements of the system include the use of better wind and GPS sensors to increase the quality of wind and wave measurements from the MOAS.

Low-frequency noise has been measured on commercial power MOSFETs. These devices, fabricated with the VDMOS structure, exhibit a 1/f type noise spectrum. The interface state density obtained from noise measurements was compared with that obtained from the subthreshold-slope method. Reasonable agreement was found between the two measurements. The radiation effects on the noise power spectral density were also investigated. The results indicated that the noise can be attributed to the generation of interface traps near the Si-SiO₂ interface. The level of interface traps generated by radiation was bias dependent. The positive gate bias gave rise to the largest interface-trap density.

The effects of high field stress on interface trap densities (Dit in MOS transistors are compared using three methods: charge-pumping, subthreshold swing and 1/f noise. The experimental MOS devices subjected to high field stress originated from two wafer lots processed with different concentrations of copper in the buffered oxide etchant. For the charge-pumping and subthreshold methods, no dependency is found on stress current polarity, wafer lot or transistor type (n- or p-channel). These two methods yield similar Dit values. For the 1/f noise method, no dependency is found on current polarity or wafer lot. However, the noise in the n-channel devices increases by several orders of magnitude as compared to the p-channel devices. A large discrepancy is found between Dit calculated from 1/f noise when compared to charge-pumping/subthreshold swing results for n-channel transistors. For p-channel transistors, the 1/f Dit results are in much better agreement with the results of the other two methods.

Robot manipulators are considered as the key element in flexible manufacturing systems. Nonetheless, for a successful accomplishment of robot integration, the robots need to be accurate. The leading source of inaccuracy is the mismatch between the prediction made by the robot controller and the actual system. This work presents techniques for identification of actual kinematic parameters and pose accuracy compensation using a laser-based 3-D measurement system. In identification stage, both direct search and gradient methods are utilized. A computer simulation of the identification is performed using virtual position measurements. Moreover, experimentation is performed on industrial robot FANUC Robot R-2000iB/210F to test full pose and relative position accuracy improvements. In addition, accuracy obtained by classical parametric methodology is improved by the implementation of artificial neural networks. Neuro-parametric method proves an enhanced improvement in simulation results. The whole proposed theory is reflected by developed simulation software throughout this work while achieving accuracy nine times better when comparing before and after implementation.

Droplet Interface Bilayers (DIBs) have a number of attributes that distinguish them from conventional artificial lipid bilayers. In particular, the ability to manipulate bilayers mechanically is explored in this thesis. Directed bilayer area changes are used to make precise measurements of the specific capacitance of DIBs and to control the two dimensional concentration of a membrane protein reconstituted in the bilayer. Chapter 1 provides a general introduction to the role of the lipid membrane en- vironment in the function of biological membranes and their integral proteins. An overview of model lipid bilayer systems is given. Chapter 2 introduces work carried out in this laboratory previously and illustrates the experimental setup of DIBs. Some important bilayer biophysical concepts are covered to provide the theoretical background to experiments in this and in later chapters. Results from the characterisation of DIBs are reported, and an account of the development of methods to manipulate the bilayer by mechanical means is given. Chapter 3 describes experiments that apply bilayer area manipulation in DIBs to achieve precise measurement of specific capacitance in a range of lipid systems. Chapter 4 reports results from experiments investigating the response of bilayer specific capacitance to an applied potential. Chapter 5 covers the background and experimental setup for total internal fluo- rescence microscopy experiments in DIBs and describes the expression, purification and characterisation of the bacterial β-barrel membrane protein pore α-Hemolysin. Chapter 6 describes experiments that apply the mechanical manipulation of bilayer area in DIBs to the corralling and control of the surface density of α-Hemolysin.

It has been desirable for years to develop non-intrusive/non-invasiveprocedures to determine the pressures and stresses at various levels andinterfaces in the railroad track structure in order to optimize track designs andimprove subsequent track performance. Recent research has developedsatisfactory procedures for measuring pressures in the track structure at theballast/subballast/subgrade levels using earth pressure cells. The researchreported in this thesis documents the development of a technique for measuringthe pressures in the track, at the rail/tie plate/tie interfaces, using a very thinpressure sensitive Tekscan sensor. The Tekscan Measurement System uses asensor composed of a matrix-based array of force sensitive cells, similar to ministrain gauges, to obtain accurate pressure distributions between two surfaces inthe track. This thesis specifically describes: 1) the optimum procedure to installthe sensors into the track, 2) the recommended practices to effectively collectdata with the software, and 3) the accepted techniques for analyzing the results.Both laboratory calibration and in-track testing have been conducted and theresults are presented. The findings attest to the usefulness and practicality of theprocedure for accurately measuring pressures in railroad tracks. The proceduremay also be applicable for a wide variety of specific track related measurementssuch as validating curve geometric criteria, assessing crossing diamond impactpressures, and evaluating the advantages/disadvantages of various types of tieplates, fastenings and tie compositions.

It has been known that a significant part of the thermal budget of an electronic package is occupied by the thermal interface material which is used to join different materials. Research in reducing this resistance through the use of vertically aligned multiwall carbon nanotube based thermal interface materials is presented. Transferred arrays anchored to substrates using thermal conductive adhesive and solder was analyzed through a steady-state infrared measurement technique. The thermal performance of the arrays as characterized through the measurement system is shown to be comparable and better than currently available interface material alternatives. Furthermore, a developed parametric model of the thermal conductive adhesive anchoring scheme demonstrates even greater potential for improved thermal resistances. Additionally, a developed transient infrared measurement system based on single point high speed temperature measurements and full temperature mappings is shown to give increased information into the thermophysical properties of a multilayer sample than other steady-state techniques.

Wear of railroad rolling stock and rails costs millions of dollars annually in all rail systems throughout the world. The rail industry has attempted to address flange wear using rail curve lubricants and presently use a variety of lubricants and lubricant applicators. The choice of lubricant and applicator is currently based on considerations that do not address the wear problem directly. This research quantified rail curve lubricant performance through laboratory simulation. The effects of lubricants in the wheel/rail contact were investigated. Rail curve lubricant performance was measured with a laboratory rail/wheel simulator for the purpose of optimising the choice of lubricant. New methods for measurement of rail curve lubricant performance have been presented. These performance measurements are total absorbed energy, the energy absorbed in the lubricant film instead of being utilised for wear processes; total distance slid, the sliding distance or accumulated strain achieved prior to development of a set tractive force limit; half life of lubricant, the time taken for a lubricant to lose half of its sliding performance; and apparent viscosity, a measure of the lubricity presented with respect to accumulated strain. The rail/wheel simulator used in this research consists of two dissimilar wheels (disks) rotating in contact with one another simulating a conformal gauge corner contact. The first wheel, a simulated rail, is driven by an electric motor which then drives the second wheel, a simulated railroad wheel, through the contact. Hydraulic braking on the railroad wheel is used to simulate the rolling/sliding conditions. The variables of the simulated contact that are controlled with this equipment are normal force, input wheel speed, slip ratio between samples, sample geometries and material properties, and lubricant types. Rail curve lubricants were laboratory tested to define their properties using the ASTM and other appropriate standards. The performance differences measured using ASTM standards based tests were susceptible to repeatability problems and did not represent the contact as accurately as the rail/wheel simulator. This laboratory simulator was used to gather data in lubricated and unlubricated conditions for the purpose of providing lubricant performance measurements. These measurements were presented and the tested lubricants were ranked conclusively using three industrially relevant performance criteria. Total sliding distance and total absorbed energy measurements of the rail curve lubricants displayed clear differences in lubricant performance for both of these criteria. Total sliding distance is equivalent to the number of axles in the field situation, while total absorbed energy is the energy unavailable for wear processes of rails and wheels. Lubricants designed using these measurements will increase lubricant performance with respect to these performance criteria which in turn will reduce wear to both rails and wheels. Measurement of the apparent viscosity of rail curve lubricants, using the rail/wheel simulator, displayed changes in rheological characteristics with respect to accumulated strain. Apparent viscosity is a measure of the shear stress transmitted from the wheels to the rails. Designing a rail curve lubricant after analysing measurements taken from the rail/wheel simulator will assist in identifying lubricant properties to reduce the wear producing shear stresses generated in a rail wheel contact. Decay of lubricant performance was measured for three different rail curve lubricants under simulated conditions. The research found appreciable and quantifiable differences between lubricants. Industrial application of the findings will improve positioning of lubrication systems, improve choice of lubricants and predict effective lubrication distance from the lubricant application point. Using the new methods of lubricant performance measurement developed in this thesis, the objective of this research, to quantify rail curve lubricant performance through laboratory simulation, has been achieved.

Wear of railroad rolling stock and rails costs millions of dollars annually in all rail systems throughout the world. The rail industry has attempted to address flange wear using rail curve lubricants and presently use a variety of lubricants and lubricant applicators. The choice of lubricant and applicator is currently based on considerations that do not address the wear problem directly. This research quantified rail curve lubricant performance through laboratory simulation. The effects of lubricants in the wheel/rail contact were investigated. Rail curve lubricant performance was measured with a laboratory rail/wheel simulator for the purpose of optimising the choice of lubricant. New methods for measurement of rail curve lubricant performance have been presented. These performance measurements are total absorbed energy, the energy absorbed in the lubricant film instead of being utilised for wear processes; total distance slid, the sliding distance or accumulated strain achieved prior to development of a set tractive force limit; half life of lubricant, the time taken for a lubricant to lose half of its sliding performance; and apparent viscosity, a measure of the lubricity presented with respect to accumulated strain. The rail/wheel simulator used in this research consists of two dissimilar wheels (disks) rotating in contact with one another simulating a conformal gauge corner contact. The first wheel, a simulated rail, is driven by an electric motor which then drives the second wheel, a simulated railroad wheel, through the contact. Hydraulic braking on the railroad wheel is used to simulate the rolling/sliding conditions. The variables of the simulated contact that are controlled with this equipment are normal force, input wheel speed, slip ratio between samples, sample geometries and material properties, and lubricant types. Rail curve lubricants were laboratory tested to define their properties using the ASTM and other appropriate standards. The performance differences measured using ASTM standards based tests were susceptible to repeatability problems and did not represent the contact as accurately as the rail/wheel simulator. This laboratory simulator was used to gather data in lubricated and unlubricated conditions for the purpose of providing lubricant performance measurements. These measurements were presented and the tested lubricants were ranked conclusively using three industrially relevant performance criteria. Total sliding distance and total absorbed energy measurements of the rail curve lubricants displayed clear differences in lubricant performance for both of these criteria. Total sliding distance is equivalent to the number of axles in the field situation, while total absorbed energy is the energy unavailable for wear processes of rails and wheels. Lubricants designed using these measurements will increase lubricant performance with respect to these performance criteria which in turn will reduce wear to both rails and wheels. Measurement of the apparent viscosity of rail curve lubricants, using the rail/wheel simulator, displayed changes in rheological characteristics with respect to accumulated strain. Apparent viscosity is a measure of the shear stress transmitted from the wheels to the rails. Designing a rail curve lubricant after analysing measurements taken from the rail/wheel simulator will assist in identifying lubricant properties to reduce the wear producing shear stresses generated in a rail wheel contact. Decay of lubricant performance was measured for three different rail curve lubricants under simulated conditions. The research found appreciable and quantifiable differences between lubricants. Industrial application of the findings will improve positioning of lubrication systems, improve choice of lubricants and predict effective lubrication distance from the lubricant application point. Using the new methods of lubricant performance measurement developed in this thesis, the objective of this research, to quantify rail curve lubricant performance through laboratory simulation, has been achieved.

The Along Track Scanning Radiometers (ATSR-1&2) on ESA's Remote Sensing Satellites (ERS-1&2) are validated using in situ radiometric data from Mutsu bay, Japan. One validation point for ATSR-1 was obtained and it was found to have an offset of -0.03K from the in situ radiometric data. Four validation points were obtained for ATSR-2 and it was fund to have an offset of 0.070.17 K in this region. The so-called 'skin effect' is investigated to improve the characterisation of the ocean-atmosphere interface. The two contrasting data sets - one from sheltered waters and one from open ocean are compared. The data presented here show that, in open oceans, at wind speeds greater than 6ms-1, T tends to a constant value of about -0.140.1K. The in situ radiometric data were taken using the SISTeR radiometer, designed and built by T.J. Nightingale. The absolute accuracy of this radiometer is assessed over a number of years and during the last campaign was found to be better than 0.025 K with an rms error (with a clean scan mirror) of less than 0.03 K. The data sets required to do this work were collected during 3 field campaigns during the summers of 1996, 1997 and 1998. MUBEX'96 and '97 took place in Mutsu Bay, Japan and CHAOS'98 was a research cruise from Tenerife to Iceland on the RRS Discovery.

The aim of the present work was to improve the predictive capabilities of current modelling methods used to assess the long-term biosphere impacts of underground repositories for radioactive wastes. A number of issues related to parameter and conceptual uncertainties associated with compartmental biosphere models that simulate transport and accumulation of radionuclides in soils were addressed. The structure of compartmental models used for radiological risk assessments has not evolved noticeably over the past few decades and most of these models rely on simple assumptions. For example, compartmental models used to predict activity concentrations of radionuclides released into soils over very long timescales (typical of the lifetime of underground disposal repositories) assume arbitrary model specifications such as soil layer thickness (the vertical discretisation of the soil column) and length of the time step. Moreover, the majority of the available models assume invariant sorption characteristics of radionuclides with soil depth and hence employ constant solid-liquid distribution coefficient (Kd) values regardless of soil characteristics known to affect radionuclide sorption (e.g. pH, redox potential, moisture content and organic matter). The empirical Kd has a profound effect on long-term predictions of radionuclide behaviour in soil since it determines the degree of radionuclide retardation due to interaction with the soil. It is associated with considerable uncertainty due to differences in experimental conditions and methods used for its measurement and the variation in soil characteristics. In this study, three soil types (arable, grassland and woodland) were incubated under anaerobic conditions and the behaviour of naturally occurring selenium, iodine, rhenium and uranium, expressed as Kd, was investigated. The results indicate that variation in soil characteristics (e.g. moisture content, pH, mineral and organic carbon content) is a significant source of K, variability. Soils relatively higher in organic matter content (e.g. top soils) have higher sorptive capacities for trace elements than mineral subsoils and hence higher Kds. Dynamic, complex behaviour of K, under flooded, anaerobic soil condtions was measured over a 3 week period in soil microcosms. This dynamic behaviour was driven by the shift in soil redox potential which was associated with solubilisation of soil organic and mineral (Fe oxide) phases. Overall, the maximum observed variation in K, over the entire incubation period did not exceed 2 orders of magnitude. Biosphere models were constructed which combined a physically-based water flow model and the compartmental approach and used to simulate the long-term vertical distribution of radionuclides in the soil as well as radionuclide dynamics under different environmental conditions. Investigating radionuclide dynamics on a short timescale could only be achieved using models with a daily time step since short-term variation was obscured by a longer (annual) time step. Simulation results give insights into some of the limitations of available biosphere modelling methods for radiological risk assessment that are often overlooked. For example, soil radionuclide activity concentrations calculated using compartmental models are sensitive to the vertical discretisation (i.e. thickness of soil layers into which the soil column is divided) and time step of the model, hence the structure of the model should not be set arbitrarily. The discretisation procedure proposed in the present study may provide a useful framework to select the appropriate structure of biosphere assessment models. With respect to the effect of uncertainty in K, on model calculations, the results show that equilibrium timescales and radionuclide activity concentrations in the soil at equilibrium increase as the K, increases. For example, the time to reach steady state radionuclide activity concentrations in the vegetated topsoil increased 14-fold and 7-fold, respectively, when K, was increased 28-fold, which is a small variation compared to the uncertainty of Kd commonly reported in the literature (e.g. a few orders of magnitude). The Kd also affects short and long-term radionuclide dynamics in soils; the activity concentration of a radionuclide with low Kd (weakly sorbing) is more responsive to seasonal fluctuations in climatic and hydrological conditions than a radionuclide with a large Kd (strongly sorbing). Radionuclide uptake by plant roots, especially those which access highly contaminated soil layers adjacent to the contaminated aquifer, could be an important mechanism that provides a direct pathway between shallow, contaminated aquifers and the soil surface where elavated contamination poses greater risks.

Thesis (Ph. D.)--Massachusetts Institute of Technology, Dept. of Materials Science and Engineering, 2009.
Cataloged from PDF version of thesis.
Includes bibliographical references.
The main goal of this thesis is to study the coupled interactions between chemically and mechanically characterized materials and cells that are relevant to microvascular physiology and pathology. In particular, the mechanical characterization of cell surface structure and force generation are realized via various atomic force microscopy (AFM) imaging techniques including AFM cell force spectroscopy and functionalized force imaging. In these approaches, the recognition of mechanical responses of cells or mapping of cell surface receptors is mediated by chemomechanically characterized AFM cantilevers. The high spatial and force resolution of AFM imaging techniques and force spectroscopy enabled investigation of mechanical interaction at the cell-cell or cell-material interfaces. This interaction was studied via the mapping of specific receptors on endothelial cell surfaces and the detection of pN-scale force transmission through ligand-receptor pairs on the plasma membrane with biophysical interpretation of cellular force generation. This thesis consists of four major chapters: the recognition of vascular endothelial growth factor receptors and of anti-angiogenic oligopeptide receptors on endothelial cell surfaces, mechanical interaction between endothelial cells and pericytes that encompass capillary blood vessels; cell-matrix contact via focal complexes; and leukemia cells rolling on endothelial cell surfaces and P-selectin-conjugated glass substrata.
(cont.) This thesis also includes appendices that detail the effect of force transducer stiffness on the measurement of unbinding force, nerve cell imaging to I observe the connection between axons and dendrites, and chemomechanical characterization of polyelectrolyte multilayers, biodegradable hydrogels, and biological glues. In Chapter 2, transmembrane receptors on endothelial cell surfaces are mapped and associated binding kinetics/thermodynamics of ligand-receptor pairs are quantified via AFM functionalized force imaging or single-molecule recognition imaging. Functionalized force imaging is then used to identify unknown receptors, receptors for an oligopeptide isolated from tissue inhibitor of metalloproteinase-2, called Loop 6. In Chapter 3, mechanical stress by pericytes that envelop capillary blood vessels is quantified, demonstrating that pericytes exert significant mechanical strain on the extracellular environment. In Chapter 4, picoNewton-scale force dynamics at fibroblasts' focal complexes, measured in real-time through cell force spectroscopy, demonstrates that cells exert mechanical force that can speed the rupture of ligand-receptor pairs in focal complexes during migration and adhesion to underlying substrata. The last part of this thesis, Chapter 5, discusses the role of actin-mediated force in leukemia cell rolling on endothelial cell surfaces. The measurement of picoNewton-scale force dynamics using cell force spectroscopy suggests that, in addition to drag force exerted by blood flow, cytoskeletal force dynamics contribute to the cell rolling process.
(cont.) Together, these studies from the single-molecule to whole-cell level detail the strong coupling between mechanical force and ligand-receptor reaction kinetics.
by Sunyoung Lee.
Ph.D.

In many experiments, surfactant adsorption and desorption at solid-liquid interfaces is found to be quite slow, considering that surfactants are small molecules. Attenuated total reflectance Fourier transform infrared spectroscopy was used to study the adsorption, desorption, and exchange of tetradecyltrimethylammonium bromide (C₁₄TABr) at the silicon oxide surface. The exchange of surfactant was monitored using protonated and perdeuterated C₁₄TABr. The data show that exchange of C₁₄TABr between the surface and the bulk solution is very fast, complete exchange occurs in less than 10 seconds. A simple exchange model suggests that the disassociation rate constant of a single monomer is no less than 1 s^-1, which is ~ 10⁴ times slower than monomer exchange in bulk solutions. The actual exchange rate may be greater than observed in the present work due to transport phenomena. The rates of exchange are similar at concentrations above and below the critical micellar concentration. Adsorption is similarly rapid, but under some circumstances there is a small residue of surfactant that is slow to desorb. Desorption experiments utilizing KBr solutions of high and low ionic strength show that two thirds of each adsorbed micelle is held by hydrophobic association, and the other third is electrostatically bound. Adsorption, desorption, and exchange experiments at temperatures of 11°C above and 8°C below the Krafft temperature (14.4°C) show similar kinetics.
Master of Science

This project aims at establishing a new method to characterize the interface between 4H-SiC and passivating dielectric layers. The investigations are made on metal-oxide-semiconductor (MOS) test structures. The oxides are made of Al2O3, deposited by atomic layer deposition (ALD), and SiO2, deposited by plasma-enhanced chemical vapour deposition (PECVD) and the semiconductor is lowly doped 4H-SiC n-type epitaxial layers. These structures have been exposed to different fluencies of Ar ion irradiation to induce damage at the interface and then measured by well-established electrical techniques, as well as the new method utilizing optical free carrier absorption (FCA) technique to assess the interface traps. We have furthermore developed an analytical tool using Matlab that can extract surface recombination velocity (SRV) from the optical data. This tool is developed for an idealized epi-layer between two surfaces, but could also be applied, for instance, to the region between the emitter and base contacts on SiC mesa etched BJT’s. First, optical free carrier absorption (FCA) measurements are carried out to measure the effective lifetimes in the structures. The data obtained from FCA is then fitted with the analytical tool and SRVs, for samples with both types of dielectrics with various Ar ion fluencies, are extracted. Standard electrical measurements using capacitance-voltage (CV) measurements are also undertaken and the density of interface traps (Dit) is extracted using the Terman method. Extracted SRV values are then compared to Ditvalues. It is observed that SiO2 samples show a large rise of SRVs, from 0.5x104 cm/s for a reference sample to 8x104 cm/s for a fluence of 1x1012 cm-2, whereas Al2O3 samples show more stable SRV, changing from 3x104 cm/s for the un-irradiated reference sample to 6x104 cm/s for a fluence of 1x1012 cm-2. A very similar trend is observed for Dit values extracted from CV measurements and it can therefore be concluded that the FCA method is very suitable for characterization of the interface, and together with CV, it should be possible to obtain quantitative values on charge carrier trapping dynamics.

To improve optical measurements, which are degraded by optical distortions, wavefront correction systems can be used. Generally, these systems evaluate a guide star in transmission. The guide star emits wellknown wavefronts, which sample the distortion by propagating through it. The system is able to directly measure the distortion and correct it. There are setups, where it is not possible to generate a guide star behind the distortion. Here, we consider a liquid jet with a radially open surface. A Mach–Zehnder interferometer is presented where both beams are stabilized through a fluctuating liquid jet surface with the Fresnel guide star (FGS) technique. The wavefront correction system estimates the beam path behind the surface by evaluating the incident beam angle and reflected beam angle of the Fresnel reflex with an observer to control the incident angle for the desired beam path. With this approach, only one optical access through the phase boundary is needed for the measurement, which can be traversed over a range of 250 μm with a significantly increased rate of valid signals. The experiment demonstrates the potential of the FGS technique for measurements through fluctuating phase boundaries, such as film flows or jets.

Thesis (PhD (Physics))--University of Stellenbosch, 2010.
ENGLISH ABSTRACT: Silicon/silicon dioxide (Si/SiO2) interface is widely used in microelectronics as the gate between the drain and source of most metal oxide semiconductor field effect transistors (MOSFETs). The functionality, reliability and electrical properties of such transistors are strongly dependent on the quality of the Si/SiO2 structure forming the gate. Characterization of the Si/SiO2 interface is important in understanding device degradation therefore the Si/SiO2 interface is a subject of intensive investigation. Research studies of Si/SiO2 interfaces using optical methods have been reported by many groups around the world but to date many open questions still exist. The physics of photoinduced trap or defect generation processes and the subsequent trapping of charge carriers, the precise role of photoinduced interfacial electric field in altering optical properties of the Si/SiO2 interface and its role in affecting the second harmonic (SH) yield measurements are not well understood. In this work a commercial near infrared femtosecond (fs) laser source [1.55 eV, 75 ± 5 fs, 10 nJ, 80 MHz] is used to study native Si/SiO2 interfaces of free standing single crystalline Si membrane and bulk Si. Optical second harmonic (SH) generated at the Si/SiO2 interfaces of a Si membrane in reflection and for the first time in transmission is demonstrated as well as stationary, single colour, pump-probe reflectivity measurements from the Si/SiO2 interface of bulk n-type Si. The experimental setups for the second harmonic generation (SHG) and pump-probe techniques were designed and implemented, and measurements were recorded by a computer controlled data acquisition system. Free standing Si membrane samples were successfully produced at the Institut f¨ur Photonische Technologien (IPHT) in Jena, Germany from bulk Si using a chemical etching process and were characterised using the z-scan technique. The penetration depth of light with a photon energy of 1.55 eV in silicon allows transmission of the fundamental fs laser pulses through the Si membrane (∼ 10 μm in thickness) and this is exploited to generate a SH signal in transmission from the Si/SiO2 interfaces of the Si membrane. In the presence of sufficiently intense fs laser light defects are created at the interfaces and populated by multiphoton transfer of charges from Si to SiO2 where they are subsequently trapped. The transfer of charge establishes interfacial electric fields across the interfaces of the Si membrane and this enhances SHG. This phenomenon is called electric field induced second harmonic (EFISH) generation. To our knowledge, EFISH measurements from interfaces of Si membrane performed in transmission are demonstrated for the first time in the present study. The demonstration of EFISH in transmission revealed new results which allowed us to provide additional perspectives on the EFISH generation process at Si/SiO2 interfaces never reported before. The temporal response of SH signals from virgin spots were recorded at different incident laser powers for both reflection and transmission geometries. The SH responses measured in transmission were observed to be time dependent and show an increase during irradiation of the sample corresponding to EFISH process. A series of SH measurements were recorded at different laser powers to compare the magnitudes of SH yield in each detection geometry for a single Si/SiO2 interface. The magnitude of the SH yield measured in transmission was higher than expected and surpassed the SH yield measured in reflection. The expectation is based on the fact that the local intensity of the fundamental beam at the second interface where the SH in transmission is generated is low compared to the local intensity at the first interface where the SH in reflection originates. A physical model is developed to consistently interpret the experimental results obtained in this study. In this model we established the origin of EFISH signals in each detection geometry, explain the unexpected high SH signals measured in transmission and provide an analysis of the time constants extracted from SH response in transmission and reflection. In addition, we also report for the first time stationary pump-probe reflectivity measurements from bulk n-type Si(111) samples with native oxide. A strong pump beam was focused on the same spot as a weak probe beam from the same fs laser source. The change in reflectivity of the Si(111)/SiO2 system was recorded by monitoring the change in intensity of the weak reflected probe beam. The temporal evolutions of the reflectivity of the material were recorded at different pump powers. The reflectivity of the material increases over several minutes of irradiation and reaches steady-state after long time irradiation. The change in reflectivity of the material is attributed to a nonlinear process called Kerr effect, and the temporal response arises from the photoinduced interfacial electric field across the Si(111)/SiO2 interface caused by multiphoton charge transfer from bulk Si(111) to the SiO2 layer. The results reported in this study contribute to the understanding of the photoinduced interfacial electric field caused by charge carrier separation across buried solid-solid interfaces. They also reveal nonlinear optical processes such as the Kerr effect caused by charge dynamics across the interface in addition to the well known SHG process.
AFRIKAANSE OPSOMMING: Die silikon/silikon dioksied (Si/SiO2) skeidingsvlak word algemeen gebruik in mikro-elektronika as die hek tussen die put en die bron van die meeste metaaloksied halfgeleier veld-effek transistors (MOSFETs). Die werkverrigting, betroubaarheid en elektriese eienskappe van sulke transistors word grootliks bepaal deur die kwaliteit van die Si/SiO2 struktuur wat die hek vorm. Karakterisering van die Si/SiO2 skeidingsvlak is belangrik om die degradering van die transistor te verstaan en daarom is die Si/SiO2 skeidingsvlak die onderwerp van intensiewe ondersoek. Ondersoek van die Si/SiO2 skeidingsvlak deur van optiese metodes gebruik te maak is geraporteer deur verskeie internasionale groepe, maar daar bestaan tot vandag toe nog n groot aantal onbeantwoorde vrae. Die fisika van die fotogenduseerde generering van defekte en van posisies waarin ladings gevang kan word, asook die daaropvolgende vasvang van ladingsdraers, die presiese rol van die fotoge¨ınduseerde elektriese veld oor die skeidingsvlak in die verandering van die optiese eienskappe van die Si/SiO2 skeidingsvlak en die grootte van die tweede harmoniek (SH) sein word nog nie goed verstaan nie. In hierdie werk word n kommersile naby-infrarooi femtosekonde (fs) laserbron [1.55 eV, 75 ± 5 fs, 10 nJ, 80 MHz] gebruik om natuurlike Si/SiO2 skeidingsvlakke van vrystaande enkelkristallyne Si membrane en soliede Si te bestudeer. Optiese tweede harmoniek (SH) wat by die Si/SiO2 skeidingsvlakke van ’n Si membraan gegenereer word - in refleksie en vir die eerste keer in transmissie - is gedemonstreer, asook stasionˆere, een-golflengte pomp-toets refleksiemetings op die Si/SiO2 skeidingsvlak van soliede n-gedoteerde Si. Die eksperimentele opstellings vir die tweede harmoniek generering (SHG) en pomp-toets tegnieke is ontwerp en uitgevoer en metings is opgeneem deur ’n rekenaarbeheerde dataversamelingstelsel. Vrystaande Si membraan monsters is suksesvol by die Institut f¨ur Photonische Technologien (IPHT) in Jena, Duitsland vervaardig uit soliede Si deur ’n chemiese etsproses en is gekarakteriseer met behulp van die z-skanderingstegniek as deel van hierdie studie. Die diepte waartoe lig met ’n fotonenergie van 1.55 eV in silikon indring laat die transmissie van die fundamentele fs laserpulse deur die Si membraan (met ∼ 10 μm dikte) toe en dit word ontgin om ’n SH sein van die Si/SiO2 skeidingsvlakke van die Si membraan in transmissie te meet. In die teenwoordigheid van fs laserlig met voldoende intensiteit word defekte by die skeidingsvlakke geskep en bevolk deur meer-foton ladingsoordrag van die Si na die SiO2 waar die ladings daaropvolgens vasgevang word. Die oordrag van ladings skep elektriese velde oor die skeidingsvlakke van die Si membraan en dit versterk die SHG. Hierdie verskynsel word elektriese veld ge¨ınduseerde tweede harmoniek (EFISH) generering genoem. Sover ons kennis strek is die meting van EFISH seine van skeidingsvlakke van Si membrane in transmissie vir die eerste keer in hierdie studie gedemonstreer. Die demonstrasie van EFISH in transmissie het nuwe resultate opgelewer wat ons toegelaat het om bykomende perspektiewe op die EFISH genereringsproses by Si/SiO2 skeidingsvlakke te verskaf waaroor nog nooit vantevore verslag gedoen is nie. Die tydafhanklike gedrag van die SH seine van voorheen onbestraalde posisies is gemeet by verskillende drywings van die inkomende laserbundel vir beide die refleksie en transmissie geometrie¨e. Die gedrag van die SH sein in transmissie is waargeneem om tydafhanklik te wees en ’n toename te toon gedurende bestraling van die monster in ooreenstemming met EFISH prosesse. ’n Reeks van SH metings is opgeneem by verskillende laserdrywings om die groottes van die SH opbrengste in elke meetgeometrie vir ’n enkele Si/SiO2 skeidingsvlak te vergelyk. Die grootte van die SH opbrengs wat in transmissie gemeet is was ho¨er as verwag is en het die grootte van die SH opbrengs in refleksie oortref. Die verwagting is gebaseer op die feit dat die lokale intensiteit by die tweede skeidingsvlak waar SH in transmisie gegenereer word relatief laag is in vergelyking met die lokale intensiteit by die eerste skeidingsvlak waar SH in refleksie ontstaan. ’n Fisiese model is ontwikkel om die eksperimentele resultate wat in hierdie studie verkry is op ’n konsekwente wyse te interpreteer. In hierdie model het ons die oorsprong van EFISH seine in elke meetgeometrie vasgestel, die onverwagte ho¨e SH seine wat in transmissie gemeet is verklaar en ’n analise van die tydkonstantes wat uit die SH gedrag in transmissie en refleksie afgelei is gedoen. Verder rapporteer ons ook vir die eerste keer stasionˆere pomp-toets reflektiwiteitsmetings van soliede n-gedoteerde Si(111) monsters met ’n natuurlike oksied. ’n Sterk pompbundel is gefokus op dieselfde posisie as ’n swak toetsbundel van dieselfde laserbron. Die verandering in reflektiwiteit van die Si(111)/SiO2 stelsel is gemeet deur die verandering in die intensiteit van die swak weerkaatste toetsbundel te monitor. Die tydevolusie van die reflektiwiteit van die mate riaal is gemeet by verskillende pompdrywings. Die reflektiwiteit van die materiaal neem toe gedurende etlike minute van bestraling en bereik ’n stasionˆere toestand na ’n lang tyd van bestraling. Die verandering in reflektiwiteit van die materiaal word toegeskryf aan ’n nielini ˆere prosess, naamlik die Kerr effek, en die tydafhanklike gedrag ontstaan as gevolg van die fotoge¨ınduseerde elektriese veld oor die Si(111)/SiO2 skeidingsvlak wat veroorsaak word deur meer-foton ladingsoordrag van die soliede Si(111) na die SiO2 laag. Die resultate wat in hierdie studie gerapporteer word dra by tot die verstaan van die fotoge ¨ınduseerde elektriese veld oor die skeidingsvlak wat veroorsaak word deur die skeiding van ladingsdraers oor die bedekte kristal-kristal skeidingsvlak. Dit lˆe ook nie-liniˆere optiese prosesse soos die Kerr effek bloot wat veroorsaak word deur die dinamika van ladings oor die skeidingsvlak, bykomend tot die bekende SHG proses.

Investigation of novel condition monitoring systems for diesel engines has received much recent attention due to the increasing demands placed upon engine components and the limitations of conventional techniques. This thesis documents experimental research conducted to assess the monitoring capabilities of Acoustic Emission (AE) analysis. In particular it focuses on the possibility of monitoring the piston ring-pack and cylinder liner interface, a critical engine sub-system for which there are currently few practical monitoring options. A series of experiments were performed on large, two-stroke and small, four-stroke diesel engines. Tests under normal operating conditions developed a detailed understanding of typical AE generation in terms of both the source mechanisms and the characteristics of the resulting activity. This was supplemented by specific tests to investigate possible AE generation at the ring-pack/liner interface. For instance, for the small engines measures were taken to remove known AE sources in order to accentuate any activity originating at the interface whilst for the large engines the interfacial conditions were purposely deteriorated through the removal of the lubricating oil supply to one cylinder. Interpretation of the results was based mainly upon comparisons with published work encompassing both the expected ring-pack behaviour and AE generation from tribological processes. This provided a strong indication that the source of the ring-pack/liner AE activity was the boundary frictional losses. The ability to monitor this process may be of significant benefit to engine operators as it enhances the diagnostic information currently available and may be incorporated into predictive maintenance strategies. A further diagnostic technique considered was the possibility of using AE parameters combined with information of crankshaft speed fluctuations to evaluate engine balance and identify underperforming cylinders.

Thesis (Ph. D.)--University of Kentucky, 2010.
Title from document title page (viewed on May 17, 2010). Document formatted into pages; contains: xii, 180 p. : ill. (some col.). Includes abstract and vita. Includes bibliographical references (p. 152-173).

Dans le cadre du retraitement des déchets nucléaires et du recyclage de métaux critiques, l'extraction par solvant est l'une des technologies les plus utilisées. L'interface liquide entre deux fluides non miscibles est considérée comme une région où de multiples phénomènes physiques et chimiques sont à prendre en compte et peuvent limiter ou favoriser le transfert d'espèces entre les deux fluides. La structure de ces interfaces doit être connue en fonction de plusieurs paramètres thermodynamiques pour pouvoir déterminer le paysage énergétique associée. La réflectivité de neutrons et de rayons est un des outils appropriés pour sonder ce genre d'interfaces enfouies et fluctuantes à l'échelle nanométrique et à l'équilibre. Pour cette étude, une nouvelle cellule a été construite et un programme spécifique d'analyse de données a été élaboré.Nous avons également porté notre étude sur deux différents systèmes bi-phasiques (eau / dodécane) contenant des sels de lanthanides et deux différents ligands non ioniques (ou extractants) : une diamide de type DMDBTDMA et de type DMDOHEMA, ces deux extractants étant connus pour avoir des comportements différents dans un processus d'extraction de cations métalliques en phase organique. Bien que la structure amphiphile des deux diamides soit bien connue, la structure de l'interface liquide / liquide semble être différente de celle que l'on pourrait s'attendre avec des tensioactifs classiques. L'organisation de ces ligands à l'interface est en effet plus complexe, varie en fonction de leurs concentrations dans la phase organique (seules des concentrations inférieures à la concentration d'agrégation critique ont été étudiées) et en fonction de la concentration d'acide et de sel dans la phase aqueuse. Une organisation de type monocouche n'est pas l'organisation principale de ces systèmes à l'équilibre mais on observe plutôt une couche épaisse de ligands.Plus précisément, dans le cas de la DMDBTDMA, cette région plus épaisse (environ trois à quatre fois la longueur du ligand) crée une région interfaciale où les molécules d'huile et d'eau peuvent se mélanger ainsi que les sels. Le système DMDOHEMA, présente une structuration différente avec également une épaisse couche de ligand (environ deux fois la longueur du ligand) mais située plus à l'intérieur de la phase huileuse et distinct de la distribution des sels à l'interface. Ces différentes structures interfaciales de DMDBTDMA et DMDOHEMA peuvent permettre d'expliquer les différents régimes de transfert ionique qualifiés soit de diffusionnel ou de cinétique
In the frame of the nuclear waste reprocessing and various kinds of critical metals recycling methods, solvent extraction is one of the most used technological processes. The liquid interface between two immiscible fluids is considered as a region where many physical and chemical phenomena take place and can limit or promote the transfer of species between both fluids. The structure of these interfaces has to be known as a function of several thermodynamical parameters to be able to determine the associated energy landscape. X-ray and neutron reflectivity are suitable techniques to probe such kind of fluctuating and buried interfaces at the nanometer scale and at equilibrium. For this study, a new cell has been built and a specific data analysis procedure was established.We have focused our study on two different biphasic systems (water/dodecane) containing lanthanides salts and two different nonionic ligands or extractant molecules: DMDBTDMA and DMDOHEMA diamides. These ligands are known to have different behaviour in the lanthanides extraction process. Although the amphiphilic chemical structure of both diamides is well known, the structure of the liquid/liquid interface appears to be different as those expected for a classical surfactant molecule. This structure looks more complex, varies as a function of the ligand concentration in the organic phase (below the critical aggregation concentration) and as a function of the proton and salt concentration of the aqueous phase. A monolayer organization does not appear as the main interfacial structuration and a thicker organic layer with an excess of salt has to be considered.In the case of the DMDBTDMA, this thicker region (approximatively three or four times the length of the ligand) creates an interfacial region where oil and water molecules as well as some salts can mix in. The DMDOHEMA system shows a different structuration where we can roughly observe also a thick layer of the ligand (approximatively two times the length of the ligand) but located more within the oil phase and forming a barrier to the salt distribution. These different interfacial structures made of DMDBTDMA and DMDOHEMA could allow to explain the diffusive or kinetic regime of ion transfer observed respectively in similar systems by others authors

In this thesis, detailed studies are presented into self-assembled, noncentrosymmetric, optically active films. Second harmonic generation (SHG) is used to measure the second order nonlinear optical susceptibility (?(2)) of ionically self-assembled monolayer (ISAM) thin films. Conventional ISAM films are fabricated by alternately immersing a substrate into oppositely-charged polyelectrolyte solutions. The polyelectrolytes bind electrostatically to the oppositely-charged substrate, and thus reverse the charge of the substrate. The charge reversal limits the amount of adsorbed material and primes the substrate for the next layer. During the deposition of the nonlinear optical (NLO) active layer, the chromophores are attracted to the oppositely-charged surface, which results in net orientation of the chromophores. Some of the net orientation is lost during the deposition of the next NLO-inactive layer as this layer orients some of the chromophores away from the substrate. A disadvantage of the polymer ISAM deposition method is that although there is a net orientation toward the substrate, a large number of chromophores are randomly or oppositely oriented. This reduces the nonlinear optical response. To overcome this problem, two alternative methods with a better net orientation are discussed: hybrid covalent / ionic deposition and multivalent monomer deposition. In both deposition methods, the NLO-active material is a monomer instead of a polymer. In hybrid covalent / ionic deposition, the NLO-inactive polymer is deposited using electrostatic attraction while the NLO-active monomer is deposited covalently. This forces alignment of the chromophores. The multivalent method uses chromophores with multiple charges on one side of the molecule and one charge (same sign) on the other. The difference in electrostatic attraction causes a preferential orientation of the chromophores during deposition. Attempts have been made to further improve the net orientation by complexation of the monomers with cyclodextrins (cone shaped organic molecules), so far with only limited success. The SHG response of NLO-active layers near the glass and air interfaces is much stronger than the SHG response of layers in the bulk of the film for all deposition methods and NLO-active materials investigated in this thesis. For larger number of bilayers (the bulk regime), the square root of the SHG signal increases linearly with the number of bilayers as expected for a uniform chromophore orientation. We isolated the interface effects through use of buffer layers of NLO-inactive polymers. The glass interface effect extends roughly one bilayer deep for all investigated materials. The air interface effect is different for polymers and monomers. For monomers, this effect extends only one bilayer deep, while it extends multiple layers deep for polymers. Using glass cells to contain the polyelectrolyte solutions, we were able to measure the SHG signal in situ, which proved to be a powerful tool to monitor the deposition rate as a function of chosen parameters. All depositions were rapid, on the order of one minute or less. Provided that a minimum concentration is met, the deposition rate and final SHG values are independent of concentration. Bulk layers deposit at the same rate as layers near the interface. For polymer NLO-active layers a secondary, slower growth of SHG is observed that is presumably due to reorganization of the adsorbed polymer layer. This secondary growth is not observed in the deposition of NLO-active monomers.
Ph. D.

Home-based rehabilitation has evolved in recent years as a cost-effective and convenient alternative to traditional clinical rehabilitation. Researchers have developed various types of sensors-based rehabilitation systems that incorporate Virtual Reality games aimed to offer the patient an entertaining and beneficial training experience from the comfort of home. This has consequently created the need to design reliable assessment and adaptation mechanisms that are able to measure and analyze the patient's performance and condition, and to accordingly make proper adjustments that conform to the abilities of the patient during the training. In this dissertation, we introduce our context-based adaptive home-based rehabilitation framework (CAHR) that offers the patients a rehabilitation environment that can adapt based on their physical, physiological, and psychological context, while taking into consideration the environmental conditions that may hinder their progress. CAHR is a generic framework that can be implemented to fit any of the upper or lower extremity rehabilitation. However, in this dissertation, we base our modeling and analysis mainly on the wrist. In CAHR, the physical condition of the patient is assessed by a fuzzy logic-based mechanism that uses the various kinematics captured during the training to provide a quantified value which reflects the Quality of Physical Performance of the patient. The rehabilitation task adaptation is achieved based on a special algorithm that defines how the physical training, psychophysiological responses, and environmental conditions must be manipulated in order to match the desired performance target parameters set by the therapist. The simulation results have shown that the proposed adaptation engine can properly adjust the rehabilitation environment based on different simulated performance behavior that might be produced by a patient. In addition, training with a special game that has been designed based on the developed framework has shown improvement in the physical capabilities of two patients suffering from upper extremity impairments.

L’ouverture du contact béton-rocher des barrages-voûtes est un phénomène fréquemment observé, qui se traduit par une piézométrie locale caractérisée par des effets non-linéaires : effet de seuil et couplage de ses facteurs explicatifs (effets hydrostatiques, thermiques, et temporels). Afin d’interpréter les mesures d’auscultation correspondantes, il est nécessaire de tenir compte de la non-additivité de ces influences, ce que ne permettent pas les modèles physico-statistiques de type régression linéaire multiple actuellement utilisés par l’ingénierie. Dans ce contexte, les objectifs de cette thèse sont d’aboutir à une meilleure compréhension des phénomènes hydrauliques ayant lieu à l’interface béton-rocher grâce à l’analyse et interprétation des mesures d’auscultation, et de caractériser l’état de dégradation du contact, en particulier son extension spatiale, à partir de ces mesures. À cet effet, deux modèles ont été développés, l’un basé sur les réseaux de neurones artificiels, l’autre sur une formulation non-linéaire du modèle HST, permettant d’expliciter l’effet des différentes charges sur l’écoulement. L’interprétation de la piézométrie en termes d’effets réversibles et irréversibles a permis de proposer une caractérisation d’ordre géométrique de l’état du contact dans un profil amont-aval, basée uniquement sur la lecture de ces effets. Puis, un modèle analytique d’écoulement a été formulé et investigué, construit à partir de cette description géométrique du contact, qui permet d’interpréter le champ de pression en plusieurs points de mesure d’un même profil
The aperture of the rock-concrete interface of arch dams is a frequently observed phenomenon that shows through the non-linear features it induces in the local piezometry: threshold effects, couplings between its explanatory factors (hydrostatic effects, thermal effects, temporal effects). In order to interpret the corresponding monitoring measurements, it is necessary to take into account the non-additivity of those influences. This is not feasible with the multi-linear regression models that are commonly used in engineering. In that context, the aim of this thesis is to come to a better understanding of the hydraulic phenomena that occur at the rock-concrete interface based on the analysis and interpretation of monitoring measurements. In parallel, the objective is to characterise the state of deterioration of the contact, and more particularly its spatial extent, thanks to those measurements. To that end, two models were developed, the first one based on artificial neural networks, the second one based on a non-linear formulation of HST, enabling to make explicit the effects of the different loads on the flow. The interpretation of the piezometry in terms of reversible and irreversible effects made it possible to propose a geometrical characterisation of the contact state in an upstream-downstream profile, based only on the analysis of those effects. Then, an analytical flow model was expressed and investigated, built on this geometrical description of the contact. It permits to interpret the pressure field in several measuring points in one profile

Le besoin croissant d'intégration de nouvelles fonctions dans les futures générations de dispositifs portables contribue au surpeuplement des circuits imprimés. Dans ce contexte, la miniaturisation des composants discrets est impérative pour compenser l'augmentation de leur nombre et pour garder la taille des cartes de circuit imprimé gérable. L'un des composants les plus courants de ce type est le condensateur, qui peut être utilisé pour découpler une partie d'un réseau électrique d'un autre. Cependant, la miniaturisation des condensateurs nécessite une augmentation de leur densité de capacité, impliquant l'intégration de condensateurs haute densité. Le succès d'une telle intégration repose sur l'utilisation à la fois de matériaux à haute constante diélectrique et d'une architecture d'empilement. Dans ce contexte, les couches de titanate-zirconate de plomb (PZT) combinées aux piles multi-MIM sont de bons candidats pour la nouvelle génération de condensateurs. La technologie multi-MIM consiste à empiler deux ou plusieurs structures MIM en parallèle afin d'augmenter la densité de la capacité sans modification effective de la surface. Avec la géométrie multi-MIM, la performance de l'appareil est fortement affectée par la qualité de l'interface Métal/PZT, il est donc important d'élaborer une chimie d'interface qui ne dégrade pas les performances des multi-MIM.Cette thèse soutenue par le projet français «Programme de l'économie numérique des investissements d'Avenir » vise deux axes de développement pour l’améliorer de la qualité des interfaces Pt/Ru/PZT: la première concerne l'optimisation du contenu de Pb en excès dans la couche de PZT, tandis que le second étudie les effets du recuit de post métallisation (PMA).La première partie de la thèse est dédiée aux analyses de densité de capacité réalisées sur les condensateurs Pt/Ru/PZT/Pt en fonction de l'excès de précurseur du Pb dans les couches de PZT déposées par voie sol-gel (10, 15, 20 et 30% de Pb respectivement pour PZT10, PZT15, PZT20 et PZT30).Nous montrons qu'une augmentation de l'excès de Pb de 10 à 20% entraîne une augmentation de la constante diélectrique maximale (environ 8,8%), ainsi qu'une diminution de la tangente de perte (de 4,36 à 3,08%) et du champ de claquage (de 1,68 à 1,26MV/cm). La PMA favorise l'augmentation du maximum de constant diélectrique (jusqu'à 7,5%) et le champ de claquage augmente de 0.5 MV/cm.Ensuite, l'influence de la chimie de surface des PZT est étudiée en fonction de l'excès de précurseur de Pb. Cet excès de Pb permet de compenser l'évaporation du plomb pendant le traitement thermique successif. En utilisant la spectroscopie de photoélectrons par rayons X (XPS), nous montrons la présence d'une phase de surface ZrOx. Les faibles niveaux d'excès de Pb conduisent à la formation de nanostructures ZrOx à la surface de la couche de PZT. Un taux plus élevé en Pb favorise la disparition totale nanostructures ZrOx en surface.Enfin, nous avons sondé l'interface Pt/Ru/PZT en fonction de l'excès de Pb et de la PMA. La microscopie électronique en transmission (TEM) montre que les nanostructures de ZrOx sont présentes à l'interface du Ru/PZT10. Les nanostructures cristallines ZrOx pourraient former une couche non ferroélectrique et ainsi affecter la densité de capacité. L'analyse en mode operando (sous polarisation in situ) par XPS haute-énergie montre une réponse électronique dépendant de la polarisation appliquée, probablement grâce à l’écrantage imparfait du champ dépolarisant à l'interface Pt/Ru/PZT10. En outre, une nouvelle phase (PbOx) est observée au niveau Pt/Ru/PZT30, probablement liée à la quantité de Pb en excès dans le PZT30. Cette phase semble induire la diminution du champ de claquage et la densité de capacité observée au niveau du Pt/Ru/PZT30/Pt. Enfin, PMA sur le Pt/Ru/PZT10 montre la création d'alliage à base de ZrRuOx et PbRuOx qui pourrait être à l'origine de l'amélioration des réponses électriques des condensateurs PZT après PMA
The growing need for the integration of an increasing number of functions into the new generation of portable devices contributes to overcrowding of printed circuit boards. In this context, the miniaturization of discrete components is imperative to maintain a manageable size of the printed circuit boards. Decoupling capacitors are one of the most important such discrete components. Miniaturization requires an increase of capacitance density, involving the integration of high-density capacitors. The success of such integration relies on the use of both high dielectric permittivity materials and a suitable stacking architecture. Lead zirconate titanate (PZT) in decoupling multiple metal-insulator-metal (multi-MIM) stacks is a good candidate for the new generation of integrated capacitors. The multi-MIM technology consists in stacking two or more PZT film-based MIM structures connected in parallel in order to increase the density of the capacitance without any effective surface area change. Device performance is heavily affected by the quality of the interface with the electrodes, so it is important to engineer interface chemistry which does not degrade the multi-MIM performance.This thesis, supported by the French “Programme de l’économie numérique des investissements d’Avenir” addresses two aspects of development aiming to improve the quality of the Pt/Ru/PZT interfaces: the first one concerns the optimization of Pb excess content in the PZT film, while the second one investigates the Post Metallization Annealing (PMA) done after deposition of electrode/PZT multilayer.The first part of the thesis presents the capacitance density analysis performed on Pt/Ru/PZT/Pt capacitors as a function of Pb excess in the sol-gel precursor solution (10, 15, 20 and 30% of excess Pb for PZT10, PZT15, PZT20 and PZT30, respectively). Pb excess compensates the lead evaporation during calcination.An increase of Pb excess from 10 to 20% leads to an increase of the maximum dielectric constant of 8.8%, a decrease of the loss tangent from 4.36 to 3.08% and breakdown field from 1.68 to 1.26MV/cm. PMA favors the enhancement of the maximum of dielectric constant by 7.5%, and the breakdown field increases to 0.5 MV/cm.The influence of the surface chemistry is studied as a function of Pb precursor excess. X-ray photoelectron spectroscopy (XPS) demonstrates that low level of Pb excess leads to the presence of a ZrOx surface phase in the form of nanostructures. Higher Pb precursor content allows the PZT synthesis to proceed to its end-point, fully consuming the ZrO2 precursor and eliminating the low dielectric constant ZrOx surface phase.We have then studied the Pt/Ru/PZT interface as a function of Pb excess and PMA. Transmission Electron Microscopy (TEM) cross-sectional analysis shows that the crystalline ZrOx nanostructures are still present at the electrode interface, constituting a dielectric layer which contributes to defining capacitor performance. Operando (under bias in situ) hard X-ray photoelectron spectroscopy (HAXPES) analysis using synchrotron radiation highlights an electronic response dependent on the applied polarization, most probably due to imperfect screening of the depolarizing field at the Pt/Ru/PZT10 interface. Furthermore, a new phase (PbOx) is observed at the Pt/Ru/PZT30 due to the high Pb excess. This new phase seems to induce a reduction in breakdown field and capacitance density. Finally, PMA on the Pt/Ru/PZT10 suggests the creation of interface ZrRuOx and PbRuOx which could be at the origin of the improvement of electrical responses of PZT capacitors after PMA.In conclusion, this thesis has provided valuable information and methodology on the correlation between surface and interface physical chemistry of PZT and Pt/Ru/PZT and electric characteristics of PZT based MIM capacitors

Orientadores: Pedro Sérgio Fadini, José Roberto Guimarães
Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Civil, Arquitetura e Urbanismo
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Resumo: Neste trabalho, o objetivo principal foi a construção e otimização de câmaras visando a quantificação dos fluxos de mercúrio dissolvido gasoso (MDG), na interface água / atmosfera em lagos da Bacia Hidrográfica do Rio Negro - AM. Foram realizados trabalhos de campo utilizando-se câmaras construídas em acrílico incolor nos quais foram determinadas as concentrações de mercúrio na atmosfera externa e interna da câmara. O ar foi bombeado através de colunas preenchidas com areia de quartzo recoberta com ouro, capazes de pré-concentrar o MDG por amalgamação. A quantificação do mercúrio foi realizada empregando-se a técnica de Espectrometria de Fluorescência Atômica do Vapor Frio (CVAFS), em um equipamento operando embarcado. Em campanha realizada no mês de Janeiro de 2003, os fluxos de MDG registrados no Lago Araca (águas brancas) foram, em pmol m-2 h-1: -20,68; + 8,16 e - 0,54 em períodos sem incidência de luz, e + 29,54 ; + 32,72 em períodos iluminados. Já no Lago Iara (águas negras), os valores encontrados para MDG em períodos sem incidência de luz foram: + 28,77; + 19,00 ; + 22,35, assim como + 5,39 e - 4,85 em períodos iluminados. Os resultados sugerem que os fluxos de MDG nos lagos da Bacia do Rio Negro seguem a tendência de serem invasivos para períodos não iluminados e evasivos para períodos iluminados em águas brancas, mas evasivos para períodos não iluminados e invasivos para períodos iluminados em águas negras
Abstract: The scope of this work was the construction and optimization of fluxes chambers for the determination of dissolved gaseous mercury (DGM) in the water atmosphere interface, in lakes belonging to the Negro River basin - AM. Field work was carried out using a plexiglass flux chambers for the determination of inner and outer atmospheric gaseous mercury. The air was pumped through quartz gold-sand columns, preconcentrating the DGM by amalgamation. The mercury quantification was carried out by Cold Vapor Atomic Fluorescence Spectrometry (CVAFS), using equipment on boat. Inthe sampling period of January 2003, the DGM fluxes measured in Araca Lake (white waters) were -20.68, + 8.16 and - 0.54 pmol m-2 h-1, during a period without light incidence, and + 29.54, + 32.72 under light incidence. In the Iara Lake (black waters), the DGM fluxes were + 28.77, 19.00 and 22.35 without light incidence, and + 5.39, - 4.85 in light periods. The results suggest that DGM fluxes in white water lakes show na invasive behaviour in no light periods, as well as an evasive behaviour in light periods. However, the behaviour of DGM fluxes is opposite in black waters
Mestrado
Saneamento e Ambiente
Mestre em Engenharia Civil

La capacité opérationnelle axiale en service de pieux battus reste une zone d'incertitude, en particulier pour les structures offshore. La recherche sur le terrain a montré que le frottement latéral peut augmenter au cours des mois ou des années après le battage. Si des tendances similaires se retrouvent dans des ouvrages offshore, les avantages en terme d'ingénierie de réalisation peuvent être très importants. D'autre part, les fondations sur pieux de plates-formes de gaz, de pétrole sont soumises à des chargements cycliques à long terme qui peuvent influencer leur capacité à l'arrachement. Les pieux battus en eau profonde connaissent un grand nombre de cycles complets de charge-décharge pouvant contribuer à la dégradation du frottement latéral lors de l'installation. Cette thèse vise à mieux comprendre les principaux résultats obtenus avec des pieux réels en sable siliceux, par le biais d'une recherche à échelle de laboratoire sous conditions environnementales contrôlées. Ce travail fait partie d'un programme de recherche commun entre le Laboratoire 3SR de Grenoble, l'Imperial College London, et le projet français de recherche ANR- SOLCYP. La réponse de l'interface sol-pieu lors de l'installation ainsi que les périodes de vieillissement et de chargements cycliques axiaux ont été étudiés au laboratoire en utilisant des pieux-modèles installés dans la chambre d'étalonnage de Grenoble. Plusieurs essais avec le pieu modèle Mini-ICP (instrumenté avec des capteurs de tension totale à la surface du pieu (SST) pour les mesures de contraintes radiales de cisaillement à 3 sections) ont permis l'analyse de chemin de contrainte locale à l'interface du pieu. Des capteurs miniatures ont en outre été installés dans le massif de sable pour une mesure de contrainte lors de l'installation du pieu et son chargement ultérieur. Les effets des méthodes d'installation, de la taille des particules de sable, ou de la saturation du sable et du chargement de l'environnement, ont été pris en compte pour le vieillissement de la capacité. Les évolutions locales de l'interface radiale et du cisaillement sont en accord avec les prédictions des méthodes de conception modernes basées sur le CPT. Des preuves d'effets d'échelle soulignent l'importance des conditions aux limites appliquées à la modélisation physique. Des séries d'essais non-alternés purement en traction, ainsi que des essais alternés ont été réalisés sous contrôle en charge ou en déplacement. Les mesures locales effectuées dans les chemins de contraintes effectives montrent une contraction radiale de la masse de sable au voisinage du pieu. Les incréments de l'amplitude de charge et du déplacement imposé accélèrent les taux de dégradation cyclique. Un nouveau diagramme de stabilité cyclique a été réalisé, en résumant les essais de chargement cycliques axiaux pour les pieux foncés et battus dans du sable siliceux moyennement dense. Des mécanismes complexes comme la rupture des grains et des changements de densité locale à l'interface du pieu peuvent affecter la réponse des pieux. La cinématique derrière leur installation et l'interaction avec le sol environnant reste encore très limitée. Comprendre comment un matériau granulaire interagit avec le pieu est important pour étudier la réponse globale du pieu. Les observations globales du comportement des pieux dans la chambre d'étalonnage ont été modélisées à une échelle micro en utilisant la tomographie aux rayons X du Laboratoire 3SR à Grenoble. Le programme expérimental comprenait des essais sur une chambre d'étalonnage modèle afin d'analyser le champ de déplacement lors de l'installation d'un pieu modèle, à l'aide des techniques de corrélation d'images (DIC) en trois dimensions. Des analyses micromécaniques d'échantillons «intacts» récupérés post mortem à l'interface du pieu ont été également effectuées pour mettre en évidence de possibles changements radiaux de densité ainsi que la rupture des grains
The operational in-service axial capacity of driven piles remains an area of uncertainty, especially for offshore structures. Field research has demonstrated that axial shaft capacities may increase over the months or years after driving. If similar trends apply offshore, the realisable engineering benefits are very significant. On the other hand, the piled foundations of oil/gas platforms and wind/water turbines are subject to long term environmental and in service cyclic loading due for example to waves, vibrations and storms that may also affect their shaft capacity. Deep driven piles experience large numbers of full load-unload cycles that contribute to shaft capacity degradation during installation. This thesis aims to improve understanding of the main results obtained with full-scale piles in silica sand through a laboratory scale investigation performed under controlled environmental conditions. This work was part of a joint research programme between the Grenoble Laboratory 3SR and Imperial College London, and the French National SOLCYP research project. The response of the soil-pile interface during installation, ageing periods and cyclic loading tests have been studied using laboratory model piles installed in the large Grenoble Calibration Chamber. Several tests with the Mini-ICP pile allow the analyses of local stress path at the pile's interface. This model pile is instrumented with surface stress transducers (SST) for local measurements of total and radial shear stresses at 3 different sections along the pile's shaft. In addition, miniature soil stress transducers were installed into the sand mass for total stress measurements during pile installation and loading. Possible ageing effects as installation methods, sand particle size, sand saturation and environmental loading were studied. Local evolution of interface radial and shear stresses agree with predictions from modern CPT based design methods. Evidence of possible scale effects remark the importance of the boundary conditions applied in physical modelling. Series of one-way purely tensile and two-way axial cyclic loading tests were performed under load and displacement control. Local measurements made of the effective stress paths shows radial contraction of the sand mass in the vicinity of the pile. Increments in loading amplitude and imposed displacements accelerate cyclic degradation rates. A new interactive shaft stability chart was produced as a summary of axial cyclic loading tests for both jacked and driven piles in medium dense silica sand. Laboratory tests confirm findings from field tests where one-way low amplitude cycles lead to beneficial increases in tensile pile capacity of up to 20%. Complex mechanisms as grain breakage and local density changes at the pile's interface. The kinematics behind the installation of piles and its interaction with the surrounding soil is still limited. Understanding how granular material interacts with the pile may reveal important to understand the global pile response. The global observations of the pile behaviour from calibration chamber tests were modelled at a micro scale using Micro Computed Tomography at the Grenoble Laboratory 3SR. The experimental campaign included tests on a model calibration chamber devoted to the displacement field analyses during the installation of a model piles using three dimensional (3D) digital image correlation (DIC). Micromechanical analysis of « intact » post-mortem samples recovered at the pille's interface were also conducted for evidences of radial density gradient and grain breakage

Cette thèse vise à approfondir notre compréhension du processus de coagulation des deux catégories de taille de particules de caoutchouc issues du latex d’Hevea brasiliensis et à établir un lien avec les propriétés mécaniques du caoutchouc final. L’originalité réside dans une approche multi-échelle et pluridisciplinaire, englobant l’analyse des particules natives et de leur auto-organisation à l’état liquide, ainsi que les propriétés mécaniques des films secs sous forme de feuilles de caoutchouc (mini ADS). L’étude a été menée sur deux tailles de particules provenant des clones, RRIM600 et PB235. La première partie aux interfaces liquide/air est une nouvelle approche utilisant une cuve de Langmuir, avec un suivi des cinétiques d’adsorption des particules à l’interface à l’aide de techniques complémentaires telles que l’ellipsométrie, la tensiométrie, la rhéologie et la microscopie à angle de Brewster. Les premières étapes de la coagulation et l’organisation des composants des particules ont été observées par microscopie à force atomique. La seconde partie a permis de relier ces organisations aux propriétés mécaniques de feuilles de caoutchouc sec à travers des essais de traction uni axiale. Ce travail ouvre de nouvelles perspectives en reliant les processus moléculaires aux propriétés macroscopiques du caoutchouc naturel, élargissant ainsi les voies de recherche dans ce domaine
The aim of this thesis is to gain a deeper understanding of the coagulation process of the two size classes of rubber particles derived from Hevea brasiliensis latex, and to establish a link with the mechanical properties of the final rubber. The originality lies in a multi-scale, multi-disciplinary approach, covering the analysis of native particles and their self-organization in the liquid state, as well as the mechanical properties of dry films in the form of rubber sheets (mini ADS). The study was carried out on two particle sizes from the RRIM600 and PB235 clones. The first part is a new liquid/air approach using a Langmuir trough, with particle adsorption kinetics at the interface monitored using complementary techniques such as ellipsometry, tensiometry, rheology and Brewster angle microscopy. The first stages of coagulation and the organization of particle components were observed by atomic force microscopy. In the second part, these organizations were linked to the mechanical properties of dry rubber sheets using uniaxial tensile tests. This work opens up new perspectives by linking molecular processes to the macroscopic properties of natural rubber, thus broadening research lines in this field

This thesis deals with design of software for control and evaluation of climatic and temperature test in accredited testing laboratory CVVOZE. It includes literar research in field of climatic and temperature tests, definition of software requirements and making of application flowchart diagram. The thesis also includes implementation description of proposed control software in terms of the program and also a documentation of the application, which focuses on explanation of all application functions to the user.

Thesis (Ph. D. in Mechanical Engineering)--Naval Postgraduate School, September 2002.
Dissertation supervisor: Indranath Dutta. Includes bibliographical references (p. 119-124). Also available online.

Thesis (S.M.)--Massachusetts Institute of Technology, Program in Media Arts & Sciences, 2000.
Includes bibliographical references (p. 131-135).
Inertial measurement components, which sense either acceleration or angular rate, are being embedded into common user interface devices more frequently as their cost continues to drop dramatically. These devices hold a number of advantages over other sensing technologies: they measure relevant parameters for human interfaces and can easily be embedded into wireless, mobile platforms. The work in this dissertation demonstrates that inertial measurement can be used to acquire rich data about human gestures, that we can derive efficient algorithms for using this data in gesture recognition, and that the concept of a parameterized atomic gesture recognition has merit. Further we show that a framework combining these three levels of description can be easily used by designers to create robust applications. A wireless six degree-of-freedom inertial measurement unit (IMU), with a cubical form factor (1.25 inches on a side) was constructed to collect the data, providing updates at 15 ms intervals. This data is analyzed for periods of activity using a windowed variance algorithm, whose thresholds can be set analytically. These segments are then examined by the gesture recognition algorithms, which are applied on an axis-by-axis basis to the data. The recognized gestures are considered atomic (i.e. cannot be decomposed) and are parameterized in terms of magnitude and duration. Given these atomic gestures, a simple scripting language is developed to allow designers to combine them into full gestures of interest. It allows matching of recognized atomic gestures to prototypes based on their type, parameters and time of occurrence. Because our goal is to eventually create stand-alone devices,the algorithms designed for this framework have both low algorithmic complexity and low latency, at the price of a small loss in generality. To demonstrate this system, the gesture recognition portion of (void*): A Cast of Characters, an installation which used a pair of hand-held IMUs to capture gestural inputs, was implemented using this framework. This version ran much faster than the original version (based on Hidden Markov Models), used less processing power, and performed at least as well.
by Ari Yosef Benbasat.
S.M.

Att kunna simulera en AOD-process (Argon, OxygenandDecarburization) är i dagsläget möjligt med hjälp av en programvara. En sådan programvara används till utbildning och forskning för utveckling av rostfritt stål.   Kobolde & Partners AB är ett företag som äger en sådan programvara. I detta projekt byggs programmet ut för att ge användare möjlighet att simulera en AOD-process med osäkerhet i mätdata. Genom detta kan forskare få ökad förståelse hur processens mätresultat skiljer sig med osäkerhet i mätdata.
: Being able to simulate an AOD process (Argon, Oxygen andDecarburization) is possible nowadays with help of software. This kind ofsoftware is used for education andresearch for development of stainless steel.   Kobolde & Partners AB is a company that owns this kind of software. This project will further develop this software to enable users to simulate an AOD process with uncertainty in measurement. This allows scientist to get more knowledge how a process measurement results

This work focuses on the interface circuitry design for MEMS resonator-based vacuum sensors. Two new measurement system topologies are proposed. The required specifications and the design of the comprising blocks for each topology are studied in detail. Next, the correct functionality and performance specifications of both architectures – designed in an IBM 0.13 μm CMOS technology – are presented through a combination of post-layout simulations and measurement results. Furthermore, the advantages and disadvantages of each design are examined in detail, followed by a comparison to similar commercial systems currently available on the market.Finally, setting the ultimate goal of building a low-power, monolithic, integrated MEMS-based temperature-compensated vacuum measurement system, areas with potential for future improvement, and expansion are discussed.
Ce travail présente la conception de circuits d'interface, pour la mesure de pression sous vide à l'aide de résonateurs MEMS. Deux nouvelles structures de systèmes de mesure sont proposées. Les spécifications requises, ainsi que la conception des blocs composants pour chaque structure, sont étudiées en détail. Par la suite, l'opération adéquate et les spécifications de performance pour les deux architectures - conçues par la technologie CMOS de IBM à 0.13 μm - sont présentées par une combinaison de simulations post-layout et de résultats mesurés. De plus, les avantages et inconvénients de chaque structure sont évalués en détail, suivis d'une comparaison avec des systèmes commerciaux similaires présentement disponibles sur le marché. Finalement, pour s'approcher du but ultime de construire le meilleur système intégré et monolithique de mesure de pression sous vide, à faible consommation de puissance et avec compensation pour les variations thermiques, les possibilités d'améliorations futures et d'extension sont discutées.

Dans le domaine photovoltaïque, les performances des cellules solaires sont impactées par deux problématiques majeures : les pertes par réflexion et les pertes par recombinaisons. Le premier objectif de ce travail est de diminuer la réflexion de la lumière à la surface du silicium en utilisant une couche antireflet de nitrure de silicium. Cette dernière est réalisée par pulvérisation cathodique magnétron en utilisant des gaz non toxiques (Ar, N2). Le deuxième objectif de cette étude est la passivation des centres de recombinaison au niveau de l'interface couche antireflet/silicium. Pour cela, une approche est proposée, consistant à modifier la surface du silicium par nitruration plasma N2 générée par deux types de sources plasma : une source ECR (Electron Cyclotron Résonance) et une source GDS (Glow Discharge Source). Une couche tampon SiNx d'une épaisseur inférieure à 10 nm est alors réalisée.Une première étude de la nitruration par plasma N2, reposant sur la modélisation des signaux AR-XPS, a permis de déterminer la composition chimique en profondeur, l’épaisseur de la couche nitrurée et d’identifier les différents phénomènes physiques se déroulant lors du processus de nitruration. Ces résultats nous a permis de comprendre et maîtriser le processus de nitruration sur deux orientations de substrats Si (100) et (111). Une deuxième étude a été menée pour déterminer la composition chimique ainsi que les propriétés optiques de couches antireflets de nitrure de silicium élaborées par pulvérisation RF sur les surfaces de silicium nitrurées et non nitrurées. Cette étude a révélé que ces films pourraient être employés comme couches antireflets pour les cellules photovoltaïques à base de silicium. La dernière partie de ce travail a porté sur l’étude de l’interface couche antireflet/silicium. Les résultats de mesures électriques n’ont pas montré une amélioration conséquente des propriétés électriques lors de l’ajout d’une couche tampon SiNx. Néanmoins, nous avons suggéré des paramètres optimaux pour diminuer les perturbations engendrées par les différents processus de dépôt
In the photovoltaic field, efficiency of solar cells is impacted by two major issues: reflection losses and recombination losses. The first objective of this work is to reduce light reflection at the silicon surface by using a silicon nitride anti-reflective coating. This layer is deposited by magnetron sputtering using non-toxic gases (Ar, N2). The second objective of this study is the passivation of recombination centers at the interface between the anti-reflective coating and silicon substrate. The approach developed here to achieve this consisting in modifying the silicon surface by nitridation using a N2 Glow Discharge Source (GDS) and Electron Cyclotron Resonance (ECR) source). A SiNx buffer layer with a thickness of less than 10 nm is then deposited.A first study of nitridation using N2 plasma, based on the modeling of AR-XPS intensity, allowed us to determine the chemical composition in depth, the thickness of the nitrided layer, and to identify the various physical phenomena occurring during the nitridation process. These results enabled us to understand and to master the nitridation process on two orientations of the Si substrate (100) and (111). A second study was carried out to determine the chemical composition and the optical properties of the silicon nitride anti-reflective coating elaborated by RF sputtering on both nitrided and unnitrided silicon surfaces. This study revealed that these films could be used as an anti-reflective coating for silicon photovoltaic cells. The last part of this work focused on studying the interface between anti-reflective coating and silicon. The results of electrical measurements did not show a significant improvement in electrical properties with the addition of a SiNx buffer layer. Nevertheless, we suggested optimal parameters to reduce defects induced by the various deposition processes

Air voids are known to be sites for the initiation of corrosion in reinforcing steel bar in concrete structures. The development of suitable non-destructive methods for measuring the void content at the reinforcing steel/concrete interface would therefore provide a predictive measure of the susceptibility of a structure to future reinforcing steel corrosion, and also allow the concrete composition to be adjusted during subsequent pouring. Of particular interest here are air voids from 1 to 10 mm in size. Normal hardened concrete contains from 1 - 2 % air voids by volume. A literature survey of existing NDT methods showed that they did not possess sufficient resolution to detect small voids less than 10 mm in size in concrete. A drawback to existing methods is excessive signal attenuation by the concrete, mainly because they are applied from outside the concrete. It was considered that the only approach to overcome signal attenuation was to develop methods to measure voids from inside the concrete. This is the approach is adopted in the thesis. New methods and approaches to measuring small voids in concrete were proposed. A new sensor was developed, referred to as a voidmeter, and optical fibre and tactile pressure mapping techniques applied in unique ways for measuring small voids. The principle of the voidmeter is simple: a rubber sleeve is stretched over a perforated steel tube, cast in concrete and inflated using water. The volume of water in excess of that needed to fill the sensor itself equals the volume of voids at the sensor/concrete interface. Testing in concrete showed that the voidmeter could measure total void volume with good accuracy in the range covered of 0.2 - 1.2 ml, equivalent to a measured void volume content of 1 - 5%. Resolution was estimated at 0.1 ml. Void sizes at the concrete interface surface ranged from less than one to over 15 mm. The fibre optic sensor consists of a plastic fibre from which the cladding has been removed. A fibre embedded in concrete measures void content by sensing the different refractive index of air compared to other concrete materials at the fibre surface. The light response of a fibre embedded in mortar, using plastic sleeves on the fibre and aluminium powder to generate voids, was found to be proportional to air void contact over the range 0-100%. The tactile pressure sensor consists of a pressure sensitive pad, and would appear to have potential for measuring void contect by attachment to rebar in concrete. Three types of pressure sensor were tested and found to measure air voids as small as 2mm in size on concrete surfaces. Experimental work was also carried out to understand air void morphology at the steel/mortar surface and the effect of air voids on water transport in mortar. Air voids were found to collect preferentially next to solid objects such as mould surfaces. It was speculated that this increased porosity may result in rebar being conduits for increased water migration in concrete.

The origin of this project was the problem of foot ulceration in the diabetic patient. Whilst the principal cause of the susceptibility to foot ulceration in patients with this pathology, and others such as leprosy, is abnormal physiology, there is no doubt the mechanical forces that are applied to the foot surface are a major factor. Currently several devices are available to measure the perpendicular forces at the foot-shoe interface (ie. the "pressure" distribution). However the full assessment of tri-axial forces at this interface has largely eluded quantification despite the fact that it has been demonstrated that shear forces may be of equal significance to those of direct pressure. The purpose of this study was to develop a transducer for the assessment of the three dimensional forces experienced, over a very localised area, at the foot-shoe interface during normal functional locomotor activity. The application of such a device in the clinical setting will provide valuable information for the medical and orthotic professions and thereby assist them in the treatment of many patients who are at risk of foot ulceration. The principle for a transducer to be embedded in an insole and utilising electromagnetic induction between air-cored coils was proposed. Coil winding techniques were developed to enable manufacture of coils within constrained sizes. Examination of the inductive coupling possible between the coils and its variation with displacement in space was carried out using a purpose built testing rig. Transducer electronics were designed and manufactured and a data logging system implemented. Various approaches to the derivation of 3D interpretation from the system were implemented in software. An examination of the accuracy of the approach was made. A prototype design and manufacturing method was suggested utilising a specific grade of silicone rubber. The results indicated that the design proposed could be implemented effectively in a size suited to in-shoe application. The design offers a relatively low cost method which could be adapted for use in many applications requiring three dimensional displacement or force measurements.

Interconnects in power module result in thermal interfaces. The thermal interfaces degrade under thermal cycling, or chemical loading. Moreover, the reliability of thermal interfaces can be especially problematic when the interconnecting area is large, which increases its predisposition to generate defects (voids, delamination, or nonuniform quality) during processing. In order to improve the quality of the bonding process, as well as to be able to accurately assess interface reliability, it would be desirable to have a simple, reliable, and nondestructive measurement technique that would produce a 2-d map of the interface thermal resistance across a large bonded area. Based on the transient thermal method of JEDEC standard 51-14, we developed a measurement technique that involves moving a thermal sensor discretely across a large-area bonded substrate and acquiring the interface thermal resistance at each location. As detailed herein, the sensor was fabricated by packaging an IGBT bare die. An analytical thermal model was built to investigate the effects of thermal sensor packaging materials and structural parameters on the sensitivity of the measurement technique. Based on this model, we increased the detection sensitivity of the sensor by modifying the size of the sensor substrate, the material of the sensor substrate, the size of the IGBT bare die, the size of the heat sink, and the thermal resistance between sample and the heat sink. The prototype of the thermal sensor was fabricated by mounting Si IGBT on copper substrate, after which the Al wires were ultrasonic bonded to connect the terminals to the electrodes. The sensor was also well protected with a 3-d printed fixture. Then the edge effect was investigated, indicating the application of the thermal sensor is suitable for samples thinner than the value in TABLE 2 3. The working principle of the movable thermal sensor – Zth measurement and its structure function analysis – was then evaluated by sequence. The Zth measurement was evaluated by measuring the Zth change of devices induced by degradation in sintered silver die-attach layer during temperature cycling. At the end of the temperature cycling, failure modes of the sintered silver layer were investigated by scanning electron microscope (SEM) and X-ray scanning, to construct a thermal model for FEA simulation. The simulation results showed good agreement with the measured Zth result, which verified the accuracy of the test setup. The sensitivity of structure function analysis was then evaluated by measuring thermal resistance (Rth) of interface layers with different thermal properties. The structure function analysis approach successfully detected the Rth change in the thermal interface layer. The movable thermal sensor was then applied for 2d-mapping of the interface Rth of a large-area bonded substrate. Examining the test coupons bonded by sintered silver showed good and uniform bonding quality. The standard deviation of Rth is about 0.005 K/W, indicating the 95% confidence interval is about 0.01 K/W, which is commonly chosen as the error of measurement. The sensitivity of the movable thermal sensor was evaluated by detecting defects/heat channels of differing sizes. The 2-d mapping confirmed that the thermal sensor was able to detect defect/heat channel sizes larger than 1x1 mm2. The accuracy of the sensitivity was verified by FEA simulation. Moreover, the simulated results were consistent with the measured results, which indicates that the movable sensor is accurate for assessing interface thermal resistance. In summary, based on structure function analysis of the transient thermal impedance, the concept of a movable thermal sensor was proposed for two-dimensional mapping of interface thermal resistance. (1) Preliminary evaluation of this method indicated both transient thermal impedance and structure function analysis were sensitive enough to detect the thermal resistance change of thermal interface layers. With the help of transient thermal impedance measurement, we non-destructively tested the reliability of sintered silver die-attach layer bonded on either Si3N4 AMB or AlN DBA substrates. (2) An analytical thermal model was constructed to evaluate the design parameters on the sensitivity and resolution of the movable thermal sensor. A detailed design flow chart was provided in this thesis. To avoid edge effect, requirements on thickness and materials of test coupon also existed. Test coupon with smaller thermal conductivity and larger thickness had a more severe edge effect. (3) The application of the movable sensor was demonstrated by measuring the 2-d thermal resistance map of interface layers. The results indicated for bonded copper plates (k = 400 W/mK) with thickness of 2 mm, the sensor was able to detect defect/heat channel with size larger than 1x1 mm2.
Doctor of Philosophy
Interconnects in power module result in thermal interfaces. The thermal interfaces degrade during operation and their reliability can be especially problematic when the interconnecting area is large. In order to improve the quality of the bonding process, as well as to be able to accurately assess interface reliability, it would be desirable to have a simple, reliable, and nondestructive measurement technique that would produce a 2-d map of the interface thermal resistance across a large bonded area. Based on the transient thermal method of JEDEC standard 51-14, we developed a measurement technique that involves moving a thermal sensor discretely across a large-area bonded substrate and acquiring the interface thermal resistance at each location. As detailed herein, the sensor was fabricated by packaging an IGBT bare die, which allowed us to get a 2-d map of the interface thermal resistance. A thermal model was also constructed to guide the design of the sensor, to increase its performance. Moreover, the preliminary test of the test setup was conducted to prove its feasibility for the sensor. Eventually, the sensor’s performance and application was demonstrated by measuring the 2-d thermal resistance map of the bonded interfaces.

The magnitudes and relative pressure distributions transmitted to the crosstie-ballast interface of railroad track significantly influences the subsequent behavior and performance of the overall track structure. If the track structure is not properly designed to distribute the heavy-axle loads of freight cars and locomotives, deficiencies and inherent failures of the crossties, ballast, or underlying support layers can occur, requiring substantial and frequent maintenance activities to achieve requisite track geometrical standards. Incorporating an understanding of the pressure distribution at the crosstie-ballast interface, appropriate designs can be applied to adequately provide a high performing and long-lasting railroad track. Although this can be considered a simple concept, the magnitudes and distributions of pressures at the crosstie-ballast interface have historically proven to be difficult to quantifiably measure and assess over the years. This document describes the development and application of a method to measure average railroad track crosstie-ballast interfacial pressures using timber crossties and pressure cells specifically designed for granular materials. A procedure was specifically developed for recessing the cells in the bottoms of timber crossties. The validity of the test method was initially verified with a series of laboratory tests. These tests used controlled loads applied to sections of trackbed constructed in specifically designed resilient frames. The prototype trackbed section was intended to simulate typical in-track loading conditions and ballast response. Cells were subsequently installed at a test site on an NS Railway well-maintained mainline just east of Knoxville, TN. Six successive crossties were fitted with pressure cells at the ballast interface below the rail seat. Pressure cells were also installed at the center of two crossties where the ballast is typically not tamped or consolidated. Trackbed pressures at the crosstie-ballast interface were periodically measured for numerous revenue freight trains during a period of twenty-one months. After raising and surfacing the track, the ballast was permitted to further consolidate under normal train traffic before again measuring pressures. Having the ballast tightly and uniformly compacted under crossties is important to ensuring representative and reproducible pressure measurements. Measured maximum pressures under the rail at the crosstie-ballast interface ranged from 20 to 30 psi (140 to 210 kPa) for locomotives and loaded freight cars with smooth wheels producing negligible wheel/rail impacts. Crosstie-ballast interface pressures were typically 3 psi (20 kPa) maximum for empty freight cars with smooth wheels. Heavily loaded articulated intermodal car pressures for shared trucks tended to reach nearly 40 psi (280 kPa), actually higher than locomotive-produced pressures. The recorded pressures under the center of the ties were normally negligible, less than 1 psi (7 kPa) for locomotives and loaded freight cars. Wheel-Rail force parameters measured by nearby wheel-impact load detectors (WILD) were compared to crosstie-ballast pressure data for the same trains traversing the test site. Increases in peak WILD forces, either due to heavier wheel loads or increased impacts, were determined to relate favorably to increases in recorded trackbed pressures with a power relationship. The ratios between the peak and nominal wheel forces and trackbed pressures also have strong relationships.

International Telemetering Conference Proceedings / October 22-25, 2001 / Riviera Hotel and Convention Center, Las Vegas, Nevada
This article presents a measurement system based on the RS-485 interface. The presented system is an alternative solution for distributed measurement systems, which cannot be built using IEEE-488 interface due to distance limitation between elements of the system. The RS-485 interface is a base for communication between measurement instruments and uses a Master-Slave protocol to exchange data between them. One dedicated master device, usually a PC, controls all slave devices connected to the interface. To control measurement devices SCPI language is used. This solution simplifies communication between measurement devices and allows utilizing the HP-VEE environment to control any SCPI devices connected to the RS-485 network.