Experimental and numerical investigation of pilot scale microwave assisted transesterification process for biodiesel production

The goal of this study was to design and test a pilot scale process for biodiesel production using advanced microwave technology and develop a numerical model for investigating various parameters affecting this process. Dielectric properties of materials play a major role in microwave design of a process. The dielectric properties (dielectric constant ε’ and dielectric loss ε”) of biodiesel precursors: soybean oil, alcohols and catalyst and their different mixtures were measured at four different temperatures (30°C, 45°C, 60°C and 75°C) and in the frequency range of 154 MHz to 4.5 GHz. Results indicate that the microwave dielectric properties of almost all components depend on both temperature and frequency. Addition of catalyst changed the properties of solvent due to the strong ionic nature. A scaled up version of a continuous microwave transesterification process was designed, built and tested. Experimental parameters were set based on previous laboratory scale results. Experiments were performed in a well controlled continuous pilot scale microwave reactor at temperatures of 60°C and 75°C and processing times of 5 to 15 minutes. Microwave power required to achieve the temperature of 60°C was 4000W and for 75°C was 4700W. Ethanol was used as a solvent with NaOH as a catalyst (\u3c 0.2% by weight of oil). The conversion obtained was \u3e99% for all experimental conditions. The final objective was to develop a basic numerical model of continuous electromagnetic heating of biodiesel precursors. A finite element model was built using COMSOL Multiphysics 4.2 software. High frequency electromagnetic problem was coupled with the non-isothermal flow problem. The model was tested for the two different power levels. The electric field, electromagnetic power flow and temperature profiles were studied. Resulting temperature profiles were verified by comparing to the experimental data. The presented study assists in understanding microwave heating application for biodiesel production. The dielectric property analysis gives a clear picture of interaction of biodiesel components with microwave irradiation, numerical model aids in understanding temperature distribution while experiments validate the results. This study can be applied to optimize the microwave assisted continuous biodiesel production process

MICROWAVE HEATING SIMULATION OF METALS AND DIELECTRIC CERAMICS

The research objectives proposed to study metal processing using a modular industrial microwave oven. The intent of the oven was to perform casting for metal processing purposes. The research objectives were to validate the ovens performance for melting copper and then to compare the results to modeling data. The initial intent was to test the oven for its capability to melt metals. Most researchers would argue that the industrial microwave could not be used for metal processing. However, this research proposed to answer the question as to whether the industrial microwave oven could be used for processing metals or not. The strength of the research lies in the fact that the technology had not been tested on a global scale and industry has not accepted the capabilities of the oven. Nevertheless, developmental efforts have continued and the microwave technology has not ceased to be developed. Although there would be problematic issues, the focus was not to prove the theoretical equations and derive large data sets for the experiments; but to validate that the oven could be used for processing metals and used in an industrial setting where alternative metal processing technologies exist. In order to perform the research, the unit was designed and manufactured and auxiliary components purchased. The research proposed to cast copper in the experimental modular microwave oven and compare the data to the modeling data. Data collection was basically coordinated using thermocouples along the mold and an optical pyrometer for the metal. The final casts were analyzed for both metallurgical and chemical characteristics. A model was designed based upon the dimensions and operational parameters of the experimental oven and data comparison was made. A simulator was then derived using computer code to formulate a user interface panel and simulation environment representative of a laboratory environment. In order to pursue the research goals, material properties were derived as functions of temperature. For the electromagnetic properties the dielectric permittivity was required along with suggestions for the electromagnetic boundary conditions. An experiment was developed and the properties were measured for several dielectric materials; thus the most suitable ceramic material chosen

Doctor of Philosophy

dissertationPhotonic integration circuits (PICs) have received overwhelming attention in the past few decades due to various advantages over electronic circuits including absence of Joule effect and huge bandwidth. The most significant problem obstructing their commercial application is the integration density, which is largely determined by a signal wavelength that is in the order of microns. In this dissertation, we are focused on enhancing the integration density of PICs to warrant their practical applications. In general, we believe there are three ways to boost the integration density. The first is to downscale the dimension of individual integrated optical component. As an example, we have experimentally demonstrated an integrated optical diode with footprint 3 Ã- 3 m2, an integrated polarization beamsplitter with footprint 2.4 Ã- 2.4 m2, and a waveguide bend with effective bend radius as small as 0.65 m. All these devices offer the smallest footprint when compared to their alternatives. A second option to increase integration density is to combine the function of multiple devices into a single compact device. To illustrate the point, we have experimentally shown an integrated mode-converting polarization beamsplitter, and a free-space to waveguide coupler and polarization beamsplitter. Two distinct functionalities are offered in one single device without significantly sacrificing the footprint. A third option for enhancing integration density is to decrease the spacing between the individual devices. For this case, we have experimentally demonstrated an integrated cloak for nonresonant (waveguide) and resonant (microring-resonator) devices. Neighboring devices are totally invisible to each other even if they are separated as small as /2 apart. Inverse design algorithm is employed in demonstrating all of our devices. The basic premise is that, via nanofabrication, we can locally engineer the refractive index to achieve unique functionalities that are otherwise impossible. A nonlinear optimization algorithm is used to find the best permittivity distribution and a focused ion beam is used to define the fine nanostructures. Our future work lies in demonstrating active nanophotonic devices with compact footprint and high efficiency. Broadband and efficient silicon modulators, and all-optical and high-efficiency switches are envisioned with our design algorithm

Modeling, estimation and control of ring laser gyroscopes for the accurate estimation of the earth rotation

He − Ne ring lasers gyroscopes are, at present, the most precise devices for absolute angular velocity measurements. Limitations to their performances come from the non-linear dynamics of the laser. Accordingly to the Lamb semi-classical theory of gas lasers, a model can be applied to a He–Ne ring laser gyroscope to estimate and remove the laser dynamics contribution from the rotation measurements. We find a set of critical parameters affecting the long term stability of the system. We propose a method for estimating the long term drift of the laser parameters, and for filtering out the laser dynamics effects, e.g. the light backscattering. The intensities of the counterpropagating laser beams exiting one cavity mirror are continuously measured, together with the monitor of the laser population inversion. These quantities, once properly calibrated with a dedicated procedure, allow us to estimate cold cavity and active medium parameters of the Lamb theory. Our identification procedure, based on the perturbative solutions of the laser dynamics, allow us for the application of the Kalman Filter theory for the estimation of the angular velocity. The parameter identification and backscattering subtraction procedure has been verified by means of a Monte Carlo studies of the system, and then applied to the experimental data of the ring lasers G-PISA and G-WETTZELL. After the subtraction of laser dynamics effects by Kalman filter, the relative systematic error of G-PISA reduces from 50 to 5 parts in 103, and it can be attributed to the residual uncertainties on geometrical scale factor and orientation of the ring. We also report that after the backscattering subtraction, the relative systematic errors of G-WETTZELL are reduced too. Conversely, in the last decade an increasing attention was drawn to high precision optical experiments, e.g. ring laser experiments, which combine high sensitivity, accuracy and long term stability. Due to the experimental requirements, position and orientation of optical elements and laser beams formation must be controlled in the field of nano-positioning and ultra-precision instruments. Existing methods for beam direction computing in resonators, e.g. iterative ray tracing or generalized ray transfer matrices, are either computationally expensive or rely on overparametrized models of optical elements. By exploiting the Fermat’s principle, we develop a novel method to compute the beam directions in resonant optical cavities formed by spherical mirrors, as a function of mirror positions and curvature radii. The proposed procedure is based on the geometric Newton method on matrix manifold, a tool with second order convergence rate that relies on a second order model of the cavity optical length. As we avoid coordinates to parametrize the beam position on mirror surfaces, the computation of the second order model does not involve the second derivatives of the parametrization. With the help of numerical tests, we show that the convergence properties of our procedure hold for non-planar polygonal cavities, and we assess the effectiveness of the geometric Newton method in determining their configurations with an high degree of accuracy and negligible computational effort. We also presents a method to account for the (ring laser) cavity deformations due to mirrors displacement, seen as the residual motions of the mirrors centers after the removal of rigid body motions. Having the cavity configuration and the model to account for mirrors movements, the calibration and active control of the optical cavity can be addressed as a control problem. In fact, our results are of some importance not only for the design and simulation of ring laser gyroscopes, but also for the active control of the optical cavities. In the final part of this work we detail a complete model including the simulation of the physical processes of interest in the operation of a ring laser gyroscope. Simulation results for the application of the model to the ring laser GP2 are presented and discusse

Focussed microwave heating using degenerate and non-degenerate cavity modes

Microwave ovens have long been recognised as a means of reducing heating times versus conventional convection ovens. The principle design feature is based on the procurement of uniform heating within any material placed in the interior of the microwave cavity oven. Materials within the oven are subjected to a degree of heating dependent on their electromagnetic properties. For many applications, it is desirable to maintain control over the distribution of heat deposition. This can be achieved through focussing of the electromagnetic field within the cavity. Two new mechanisms are identified where an increased level of control over the heating pattern and its location could be advantageous. The research described within this thesis aims to improve heating selectivity in microwave cavity ovens by the identification and enhanced control of modal patterns in degenerate and non-degenerate resonators. This is achieved through the analysis of two novel oven arrangements. The first of these addresses the requirement for highly selective heating in hyperthermia treatment. It is demonstrated that proper selection of a forced degenerate mode set can lead to an enhancement in field focussing within the centre of the cavity through constructive and destructive interference of the fields in each mode pattern. It is found that a highly selective peak of field can be produced within the centre of a large cylindrical waveguide cavity for the purpose of hyperthermia treatment. The peak is produced using a quasi degenerate mode set excited at approximately 1:3GHz. The second example presents an open oven design for the curing of epoxy and encapsulant materials within the micro-electronics packaging industry. It is intended that the oven be placed on the arm of a precision alignment machine such that the curing and placement stages of production be combined, suggesting an increase in production efficiency. Two excitation schemes are presented based on the coupling of quasi degenerate mode sets through a wide frequency range and the excitation of a single high order mode enabling uniform field distribution for heating of encapsulant material and increased selective heating through spatial alignment of modal field peaks, respectively. Experimental results demonstrate the viability of the open-ended microwave oven for curing. Both proposed excitation methods within the open oven design are investigated with results presented. Optimisation of the heating fields is achieved through inclusion of lowloss materials within the oven. Curing of an encapsulant material covering a commercial chip package is achieved and the overall design validated

Nanocomposite electrical insulation: multiscale characterization and local phenomena comprehension

Dans le domaine de l'isolation électrique, il a été démontré que les matériaux hybrides organiques/inorganiques nanocomposites (NC) assurent une nette amélioration de leur fonctionnement à haute température/haute tension et permettent aux systèmes d'isolation électrique de renforcer leurs propriétés diélectriques. Récemment, il a été démontré que certaines modifications des propriétés électriques telles que la permittivité, la rupture diélectrique, la résistance aux décharges partielles ou la durée de vie étaient souvent attribuées à l'interphase nanoparticule/matrice, une région où la présence des nanoparticules modifie les propriétés de la matrice. De plus, des études récentes montrent qu'une fonctionnalisation de la surface des nanoparticules permet une meilleure dispersion dans la matrice hôte. Cette meilleure dispersion affecte la zone d'interphase et joue également un rôle majeur dans l'amélioration des propriétés des nanocomposites. Cependant, le rôle de l'interphase reste théorique et peu de résultats expérimentaux existent pour décrire ce phénomène. Par conséquent, en raison de l'échelle nanométrique de l'interphase, une caractérisation de ses propriétés demeure un défi. Au cours de cette thèse, deux études principales sont menées afin de mieux comprendre la relation structure-propriété dans les polymères nanocomposites. Tout d'abord, la microscopie à force atomique (AFM) est utilisée pour effectuer simultanément des mesures qualitatives et quantitatives de ces zones d'interaction dans le nanocomposite polyimide/nitrure de silicium (PI/Si3N4). Le mode Peak Force Quantitative Nano Mechanical (PF QNM) dérivé de l'AFM révèle la présence de l'interphase en mesurant les propriétés mécaniques (module de Young, déformation ou adhérence). Le mode microscopie à force électrostatique (EFM) est utilisé pour détecter et mesurer la permittivité locale de la matrice et de l'interphases. Par ailleurs, l'objectif de ce travail est de présenter l'effet de la fonctionnalisation de surface des nanoparticules de nitrure de silicium (Si3N4) sur les régions d'interphase. Ces résultats quantitatifs, à la fois mécaniques et électriques, permettent de comparer la dimension et les propriétés des interphase autour des nanoparticules traitées et non traitées. Par conséquent, cette nouvelle approche de caractérisation de cette zone confronte les résultats expérimentaux à des modèles théoriques. Un nouveau modèle basé sur les résultats expérimentaux obtenus est proposé. De plus, la deuxième partie de cette étude présente une caractérisation macroscopique des propriétés et de la rigidité diélectrique des films de polyimide pur, du nanocomposite avec des particules traitées et non traités. Les résultats révèlent le rôle de l'interphase sur la réduction du phénomène de polarisation de l'électrode (PE) dû aux mouvements ioniques surtout à haute température. Pour les nanoparticules non traitées, ces effets sont moins importants en raison de la formation d'agrégats. En revanche, une diminution nette de la PE est obtenue en fonctionnalisant la surface des nanoparticules avec le silane comme agent de couplage. Enfin, la rigidité diélectrique de l'ensemble des échantillons est mesurée et montre une augmentation considérable de la performance diélectrique des nanocomposites à haute température par rapport au PI pur.In the electrical insulation field, it was demonstrated that nanocomposite (NC) organic/inorganic hybrid materials assure a distinct improvement of their high temperature/high voltage functioning and allow the electrical insulation to strengthen its dielectric properties. Recently, it was shown that some modifications of the electrical properties such as permittivity, dielectric breakdown, partial discharges resistance or lifetime are often awarded to the nanoparticle/matrix interphase, a region where the presence of the nanoparticle changes the matrix properties. Moreover, recent studies show that the nanoparticle surface functionalization allows a better dispersion of the particles within the host matrix. This better dispersion affects the interphase zone and plays a major role in the nanocomposite properties improvement as well. However, the role of the interphase remains theoretical and few experimental results exist to describe this phenomenon. Accordingly, because of its nanometer scale, the interphase properties characterization remains a challenge. Two main studies are carried out, during this thesis work, that can provide a better understanding of structure-properties relationships in polymer nanocomposite. First, Atomic Force Microscopy (AFM) is employed to make at the same time qualitative and quantitative measurements of these interaction zones within Polyimide/Silicon Nitride (PI/Si3N4) nanocomposite. The Peak Force Quantitative Nano Mechanical (PF QNM) AFM mode reveals the presence of the interphase by measuring mechanical properties (Young modulus, deformation or adhesion). Electrostatic force microscope (EFM) mode is used in order to detect and measure the matrix and interphase local permittivity. Moreover, the aim of this work is to present the effect of the surface functionalization of silicon nitride (Si3N4) nanoparticles on the interphase regions. Mechanical and electrical quantitative results permit comparing the interphase dimension and properties between treated and untreated Si3N4 nanoparticles. As a result, this new approach to characterize the nanocomposite interphase zone using local measurements confronts experimental results with theoretical models. A new model based on the obtained experimental results is proposed. In addition, the second part of this study presents a macroscopic investigation on the dielectric properties and breakdown strength of neat polyimide, untreated and treated nanocomposite films. Results reveal the interphase role on the reduction of the electrode polarization (EP) phenomenon due to ionic movements especially at high temperatures. For untreated nanoparticles, these effects are less important due to the aggregate formation. In contrast, an EP drastic decrease is obtained by functionalizing the nanofiller surface with a silane coupling agent. Finally, the high temperature breakdown strength for all samples is investigated and shows a considerable increase of nanocomposites dielectric performance at high temperature compared to neat PI