Dissertations / Theses on the topic 'Surface acoustic wave sensors (SAW)'

This research was born from NASA Kennedy Space Center's (KSC) need for passive, wireless and individually distinguishable cryogenic liquid and H2 gas sensors in various facilities. The risks of catastrophic accidents, associated with the storage and use of cryogenic fluids may be minimized by constant monitoring. Accidents involving the release of H2 gas or LH2 were responsible for 81% of total accidents in the aerospace industry. These problems may be mitigated by the implementation of a passive (or low-power), wireless, gas detection system, which continuously monitors multiple nodes and reports temperature and H2 gas presence. Passive, wireless, cryogenic liquid level and hydrogen (H2) gas sensors were developed on a platform technology called Orthogonal Frequency Coded (OFC) surface acoustic wave (SAW) radio frequency identification (RFID) tag sensors. The OFC-SAW was shown to be mechanically resistant to failure due to thermal shock from repeated cycles between room to liquid nitrogen temperature. This suggests that these tags are ideal for integration into cryogenic Dewar environments for the purposes of cryogenic liquid level detection. Three OFC-SAW H2 gas sensors were simultaneously wirelessly interrogated while being exposed to various flow rates of H2 gas. Rapid H2 detection was achieved for flow rates as low as 1ccm of a 2% H2, 98% N2 mixture. A novel method and theory to extract the electrical and mechanical properties of a semiconducting and high conductivity thin-film using SAW amplitude and velocity dispersion measurements were also developed. The SAW device was shown to be a useful tool in analysis and characterization of ultrathin and thin films and physical phenomena such as gas adsorption and desorption mechanisms.?
Ph.D.
Doctorate
Electrical Engineering and Computer Science
Engineering and Computer Science
Electrical Engineering

This thesis addresses the design and use of suitable nanomaterials and surface acoustic wave sensors for hydrogen detection and sensing. Nanotechnology is aimed at design and synthesis of novel nanoscale materials. These materials could find uses in the design of optical, biomedical and electronic devices. One such example of a nanoscale biological system is a virus. Viruses have been given a lot of attention for assembly of nanoelectronic materials. The tobacco mosaic virus (TMV) used in this research represents an inexpensive and renewable biotemplate that can be easily functionalized for the synthesis of nanomaterials. Strains of this virus have been previously coated with metals, silica or semiconductor materials with potential applications in the assembly of nanostructures and nanoelectronic circuits. Carbon nanotubes are another set of well-characterized nanoscale materials which have been widely investigated to put their physical and chemical properties to use in design of transistors, gas sensors, hydrogen storage cells, etc. Palladium is a well-known material for detection of hydrogen. The processes of absorption and desorption are known to be reversible and are known to produce changes in density, elastic properties and conductivity of the film. Despite these advantages, palladium films are known to suffer from problems of peeling and cracking in hydrogen sensor applications. They are also required to be cycled for a few times with hydrogen before they give reproducible responses. The work presented in this thesis, takes concepts from previous hydrogen sensing techniques and applies them to two nanoengineered particles (Pd coated TMV and Pd coated SWNTs) as SAW resonator sensing materials. Possible sensing enhancements to be gained by using these nanomaterial sensing layers are investigated. SAW resonators were coated with these two different nano-structured sensing layers (Pd-TMV and Pd-SWNT) which produced differently useful hydrogen sensor responses. The Pd-TMV coated resonator responded to hydrogen with nearly constant increases in frequency as compared to the Pd-SWNT coated device, which responded with concentration-dependent decreases in frequency of greater magnitude upon hydrogen exposure. The former behavior is more associated with acousto-electric phenomena in SAW devices and the later with mass loading. The 99% response times were 30-40 seconds for the Pd-TMV sensing layer and approximately 150 seconds for the Pd-SWNT layer. Both the films showed high robustness and reversibility at room temperature. When the Pd film was exposed to hydrogen it was observed that it produced decreases in frequency to hydrogen challenges, conforming to mass loading effect. It was also observed that the Pd film started degrading with repeated exposure to hydrogen, with shifts after each exposure going smaller and smaller.

In this dissertation, guided surface acoustic wave sensors were investigated theoretically and experimentally in detail for immunosensing applications. Shear horizontal polarized guided surface acoustic wave propagation for mass loading sensing applications was modeled using analytical modeling and characterized by perturbation analysis. The model verification was performed experimentally and a surface acoustic wave immunosensor case study was presented. The results of the immunosensing were also investigated using the perturbation analysis. Guided surface acoustic wave propagation problem was investigated in detail for gravimetric (or mass loading) guided wave sensors, more specifically for immunosensors. The analytical model was developed for multilayer systems taking viscoelasticity into account. The closed form algebraic solutions were obtained by applying appropriate boundary conditions. A numerical approach was used to solve dispersion equation. Detailed parametric investigation of dispersion curves was conducted using typical substrate materials and guiding layers. Substrate types of ST-cut quartz, 41° YX lithium Niobate and 36° YX lithium tantalate with guiding layers of silicon dioxide, metals (chromium and gold), and polymers (Parylene-C and SU-8) were investigated. The effects of frequency and degree of viscoelasticity were also studied. The results showed that frequency only has effect on thickness with same shaped dispersion curves. Dispersion curves were found to be unaffected by the degree of viscoelasticity. It was also observed that when there was a large shear velocity difference between substrate and guiding layer, a transition region with a gradual decrease in phase velocity was obtained. However, when shear velocities were close, a smooth transition was observed. Furthermore, it was observed that, large density differences between substrate and guiding layer resulted in sharp and with nearly constant slope transition. Smooth transition was observed for the cases of minimal density differences. Experimental verification of the model was done using multi-layer photoresists. It was shown that with modifications, the model was able to represent the cases studied. Perturbation equations were developed with first order approximations by relating the slope of the dispersion curves with sensitivity. The equations were used to investigate the sensitivity for material selection (substrate, guiding layer, and mass perturbing layer) and degree of viscoelasticity. The investigations showed that the sensitivity was increased by using guiding layers with lower shear velocities and densities. Among the guiding layers investigated, Parylene C showed the highest sensitivity followed by gold and chrome. The perturbation investigations were also extended to viscoelasticity and to protein layers for immunosensing applications. It was observed that, viscous behavior resulted in slightly higher sensitivity; and sensitivity to protein layers was very close to sensitivity for polymers. The optimum case is found to be ST-cut quartz with Parylene-C guiding layer for protein layer sensing. Finally, an immunosensing case study was presented for selective capture of protein B-cell lymphoma 2 (Bcl-2), which is elevated in many cancer types including ovarian cancer. The immunosensor was designed, fabricated, and experimentally characterized. An application-specific surface functionalization scheme with monoclonal antibodies, ODMS, Protein A/G and Pluronic F127 was developed and applied. Characterization was done using the oscillation frequency shift of with sensor used as the feedback element of an oscillator circuit. Detection of Bcl-2 with target sensitivity of 0.5 ng/ml from buffer solutions was presented. A linear relation between frequency shift and Bcl-2 concentration was observed. The selectivity was shown with experiments by introducing another protein, in addition to Bcl-2, to the buffer. It was seen that similar detection performance of Bcl-2 was obtained even with presence of control protein in very high concentrations. The results were also analyzed with perturbation equations.

The object of this research was to investigate dispersion in surface phononic crystals (PnCs) for application to a newly developed passive surface acoustic wave (SAW) ozone sensor. Frequency band gaps and slow sound already have been reported for PnC lattice structures. Such engineered structures are often advertised to reduce loss, increase sensitivity, and reduce device size. However, these advances have not yet been realized in the context of surface acoustic wave sensors. In early work, we computed SAW dispersion in patterned surface structures and we confirmed that our finite element computations of SAW dispersion in thin films and in one dimensional surface PnC structures agree with experimental results obtained by laser probe techniques. We analyzed the computations to guide device design in terms of sensitivity and joint spectral operating point. Next we conducted simulations and experiments to determine sensitivity and limit of detection for more conventional dispersive SAW devices and PnC sensors. Finally, we conducted extensive ozone detection trials on passive reflection mode SAW devices, using distinct components of the time dispersed response to compensate for the effect of temperature. The experimental work revealed that the devices may be used for dosimetry applications over periods of several days.

Planar two-dimensional (2-D) nanostructured indium oxide (InOx) and one-dimensional (1-D) tin oxide (SnO2) semiconductor metal-oxide layers have been utilised for gas sensing applications. Novel layered Surface Acoustic Wave (SAW) based sensors were developed consisting of InOx/SiOxNy/36°YXLiTaO3, InOx/SiNx/SiO2/36°YXLiTaO3 and InOx/SiNx/36°YXLiTaO3 The 1 µm intermediate layers of silicon oxynitride (SiOxNy), silicon nitride (SiNx) and SiO2/SiNx matrix were deposited on lithium tantalate (36°YXLiTaO3) substrates by r.f. magnetron sputtering, electron-beam evaporation and plasma enhanced chemical vapour deposition (PECVD) techniques, respectively. As a gas sensitive layer, a 100 nm thin layer of InOx was deposited on the intermediate layers by r.f. magnetron sputtering. The targeted gases were ozone (O3) and hydrogen (H2). An intermediate layer has multiple functions: protective role for the interdigital transducers' electrodes as well as an isolating effect from InOx sensing layer, thereby improving the sensor performance. The developed SAW sensors' exhibited high response magnitudes with repeatable, reversible and stable responses towards O3 and H2. They are capable of sensing concentrations as low as 20 parts-per-billion for O3 and 600 parts-per-million for H2. Additionally a conductometric type novel sensing structure of SnO2/36°YX LiTaO3 was also developed by depositing a thin layer of SnO2 nanorods by PECVD. The gas sensing performance exhibited repeatable, reversible, stable responses towards NO2 and CO. The surface morphology, crystalline structure and preferred orientation of the deposited layers were investigated by Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD). A polycrystalline, oxygen deficient non-stoichiometric InOx with grain sizes of 20-40 nm was revealed. The 1-D nanostructures were characterised by Transmission Electron Microscopy (TEM) showing nanorods with needle-like shape , diameters of 10-20 nm a t the top and 30-40 nm at the base as well as a preferential growth orientation of [ ] on the LiTaO3 substrate. The developed sensors are promising for O3, H2 and CO sensing.

SAW based sensors can offer wireless, passive operation in numerous environments and various device embodiments are employed for retrieval of the sensed data information. Single sensor systems can typically use a single carrier frequency and a simple device embodiment, since tagging is not required. In a multi-sensor environment, it is necessary to both identify the sensor and retrieve the sensed information. This dissertation presents the concept of orthogonal frequency coding (OFC) for applications to SAW sensor technology. OFC offers all advantages inherent to spread spectrum communications including enhanced processing gain and lower interrogation power spectral density (PSD). It is shown that the time ambiguity in the OFC compressed pulse is significantly reduced as compared with a single frequency tag having the same code length and additional coding can be added using a pseudo-noise (PN) sequence. The OFC approach is general and should be applicable to many differing SAW sensors for temperature, pressure, liquid, gases, etc. Device embodiments are shown and a potential transceiver is described. Measured device results are presented and compared with COM model predictions to demonstrate performance. Devices are then used in computer simulations of the proposed transceiver design and the results of an OFC sensor system are discussed.
Ph.D.
School of Electrical Engineering and Computer Science
Engineering and Computer Science
Electrical Engineering

Surface acoustic waves (SAWs) have a large number of applications and the majority of them are in the sensor and actuator fields targeted to satisfy market needs. Recently, researchers have focused on optimizing and improving device functions, sensitivity, power consumption, etc. However, SAW actuators and sensors still cannot replace their conventional counterparts in some mechanical and biomedical areas, such as actuators for liquid pumping under microfluidic channels and sensors for real-time cell culture monitoring. The two objectives of this dissertation are to explore the potential of piezoelectric materials and surface acoustic waves for research on actuators and sensors in the mechanical pump and biosensor areas. Manipulation of liquids in microfluidic channels is important for many mechanical, chemical and biomedical applications. In this dissertation, we first introduced a novel integrated surface acoustic wave based pump for liquid delivery and precise manipulation within a microchannel. The device employed a hydrophobic surface coating (Cytop) in the device design to decrease the friction force and increase the bonding. Contrary to previous surface acoustic wave based pumps which were mostly based on the filling and sucking process, we demonstrated long distance media delivery (up to 8mm) and a high pumping velocity, which increased the device’s application space and mass production potential. Additionally, the device design didn’t need precise layers of water and glass between substrate and channel, which simplified the design significantly. In this study, we conducted extensive parametric studies to quantify the effects of the liquid volume pumped, microchannel size, and input applied power as well as the existence of hydrophobic surface coating on the pumping velocity and pump performance. Our results indicated that the pumping velocity for a constant liquid volume with the same applied input power could be increased by over 130% (2.31 mm/min vs 0.99 mm/min) by employing a hydrophobic surface coating (Cytop) in a thinner microchannel (250 µm vs 500 µm) design. This device could be used in circulation, dosing, metering and drug delivery applications which necessitated small-scale precise liquid control and delivery. This dissertation also introduced a novel SAW-based sensor designed and employed for detecting changes in cell concentration. Before conducting cell concentration experiments, preliminary experiments were conducted on weight concentration differentiation of microfluidic particles based on a polydimethylsiloxane (PDMS) channel and surface acoustic wave resonator design. The results confirmed that our device exerted an ultra-stable status to detect liquid properties by monitoring continuous fluids. An improved design was carried out by depositing a 200 nm ZnO layer on top of the lithium tantalate substrate surface increased the sensitivity and enabled cell concentration detection in a microfluidic system. Comprehensive studies on cell viability were carried out to investigate the effect of shear horizontal (SH) SAWs on both a cancerous (A549 lung adenocarcinoma) and a non-cancerous (RAW264.7 macrophage) cell line. Two pairs of resonators consisting of interdigital transducers (IDTs) and reflecting fingers were used to quantify mass loading by the cells in suspension media as well as within a 3-dimensional cell culture model. In order to predict the characteristics and optimize the design of the SH-SAW biosensor, a 3D COMSOL model was built to simulate the mass loading response of the cell suspensions. These results were compared to experimental data generated by pipetting cell concentrations of 3.125K, 6.25K 12.5K, 25K and 50K cells per 100µL into the PDMS well and measuring to obtain the relative frequency shift from the two oscillatory circuit systems (one of which functioned as a control). Frequency shift measurements were also collected from A549 cells cultured on a 3D nanofiber scaffold produced by electrospinning to evaluate the device’s ability to detect changes in cell density as the cells proliferated in culture over the course of eight days. The device’s ability to detect changes in cell density over time in a 3D model along with its biocompatibility reveal great potential for this device to be incorporated into 3D in vitro cancer research applications.

A multifunctional strain sensor based on Surface Acoustic Wave (SAW) Orthogonal Frequency Coding (OFC) technology on a Langasite substrate has been investigated. Second order transmission matrix models have been developed and verified. A new parameterizable library of SAW components was created to automate the layout process. Using these new tools, a SAW strain sensor with OFC reflectors was designed, fabricated and tested. The Langasite coefficients of velocity for strain (γS = 1.699) and Temperature (γT = 2.562) were experimentally determined. The strain and temperature characterization of this strain sensor, along with the coefficients of velocity, have been used to demonstrate both the ability to sense strain and the capability for temperature compensation. The temperature-compensated SAW OFC strain sensor has been used to detect anomalous strain conditions that are indicators of fastener failures during structural health monitoring of aircraft panels with and without noise on a NASA fastener failure test stand. The changes in strain that are associated with single fastener failures were measured up to a distance of 80 cm between the sensor and the removed fastener. The SAW OFC strain sensor was demonstrated to act as an impact sensor with and without noise on the fastener failure test stand. The average measured signal to noise ratio (SNR) of 50, is comparable to the 29.1 SNR of an acoustic emission sensor. The simultaneous use of a high pass filter for impact detection, while a low pass filter is used for strain or fastener failure, demonstrates the multifunctional capabilities of the SAW OFC sensor to act as both as a fastener failure detector and as an impact detector.

Surface Acoustic Waves (SAW) fall under a special category of elastic waves that need a material medium to propagate. The energy of these waves is confined to a limited depth below the surface over which they propagate, and their amplitudes decay with increasing depth. As a consequence of their being a surface phenomenon, they are easily accessible for transduction. Due to this reason, a lot of research has been carried out in the area, which has resulted in two very popular applications of SAW - SAW devices and in Non-Destructive Testing and Evaluation. A major restriction of SAW devices is that the SAW need a piezoelectric medium for generation, propagation and reception. This thesis reports the attempt made to overcome this restriction and utilize the SAW on non-piezoelectric substrates for sensing capabilities. The velocity of the SAW is known to be dependent purely on the material properties, specifically the elastic constants and material density. This dependence is the motivation for the sensor system developed in the present work. Information on the survey of the methods suitable for the generation and reception of SAW on non-piezoelectric substrates has been included in the thesis. This is followed by the theoretical and practical details of the method chosen for the present work - the point source/point receiver method. Advantages of this method include a simple and inexpensive fabrication procedure, easy customizability and the absence of restrictions due to directivity of the SAW generated. The transducers consist of a conically shaped PZT element attached to a backing material. When the piezoelectric material on the transmitter side is electrically excited, they undergo mechanical oscillations. When coupled to the surface of a solid, the oscillations are transferred onto the solid, which then acts as a point source for SAW. At the receiver, placed at a distance from the source on the same side, the received mechanical oscillations are converted into an electrical signal as a consequence of the direct piezoelectric effect. The details of the fabrication and preliminary trials conducted on metallic as well as non-metallic samples are given. Various applications have been envisaged for this relatively simple sensor system. One of them is in the field of pressure sensing. Experiments have been carried out to employ the acoustoelastic property of a flexible diaphragm made of silicone rubber sheet to measure pressure. The diaphragm, when exposed to a pressure on one side, experiences a varying strain field on the surface. The velocity of SAW generated on the stressed surface varies in accordance with the applied stress, and the consequent strain field generated. To verify the acoustoelastic phenomenon in silicone rubber, SAW velocities have been measured in longitudinal and transverse directions with respect to that of the applied tensile strain. Similar measurements are carried out with a pressure variant inducing the strain. The non-invasive nature of this setup lends it to be used for in situ measurement of pressure. The second application is in the field of elastography. Traditional methods of diagnosis to detect the presence of sub-epidermal lesions, some tumors of the breast, liver and prostate, intensity of skin irritation etc have been mainly by palpation. The sensor system developed in this work enables to overcome the restrictive usage and occasional failure to detect minute abnormal symptoms. In vitro trials have been conducted on tissue phantoms made out of poly (vinyl alcohol) (PVA-C) samples of varying stiffnesses. The results obtained and a discussion on the same are presented.

In this thesis, the author proposes and develops novel multilayered Surface Acoustic Wave (SAW) devices with unique attributes for gas sensing applications. The design, simulation, fabrication and gas sensing performance of three multilayered SAW structures has been undertaken. The investigated structures are based on two substrates having high electromechanical coupling coefficient: lithium niobate (LiNbO3) and lithium tantalate (LiTaO3), with a piezoelectric zinc oxide (ZnO) intermediate layer. Sensitivity towards target gas analytes is provided by thin film indium oxide (InOx) or tungsten trioxide (WO3). The high performance of the gas sensors is achieved by adjusting the intermediate ZnO layer thickness. Sensitivity calculations, undertaken with perturbation theory illustrate how the intermediate ZnO layer can be employed to modify the velocity-permittivity product of the supported SAW modes, resulting in highly sensitive conductometric SAW gas sensors. The work contained within this thesis addresses a broad spectrum of issues relating to multilayered SAW gas sensors. Topics include finite-element modelling, perturbation theory, micro-fabrication, metal oxide deposition, material characterisation and experiential evaluation of the layered SAW sensors towards nitrogen dioxide (NO2), hydrogen (H2) and ethanol gas phase analytes. The development of two-dimensional (2D) and three dimensional (3D) finite-element models provides a deep insight and understanding of acoustic wave propagation in layered anisotropic media, whilst also illustrating that the entire surface of the device can and should be used as the active sensing area. Additionally, the unique and distinctive surface morphology of the layered structures are examined by Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM). The crystalline structure and orientation of the ZnO and WO3 layers are also examined by X-ray Diffraction Spectroscopy (XRD). The novel multilayered SAW structures a re shown to be highly sensitive, capable of sensing NO2 and ethanol concentration levels in the parts-per-billion and parts-per-million range, respectively, and H2 concentrations below 1.00% in air. The addition of platinum or gold catalyst activator layers on the WO3 sensitive layer is shown to improve sensitivity and dynamic performance, with response magnitudes up to 50 times larger than bare WO3. The gas sensing performance of the investigated structures provide strong evidence that high sensitivity can be achieved utilising multilayered SAW structures for conductometric gas sensing applications.

It is demonstrated that by using a miniature chemical reaction vessel under adaptive mechatronic control, it is possible to design and construct a low-cost carbon dioxide measurement system. With further development such a system would be potentially suitable for low-cost commercial application, in particular as sacrificial, single-mission instrumentation packages in horticultural cargo monitoring. Current instrumentation systems for carbon dioxide (CO2) gas measurement are reviewed and their limitations with respect to low cost commercial applications determined. These utilise technology intended for laboratory measurements. In particular the optical energy absorbance of CO2 in the infra-red electromagnetic spectrum. These systems require large optical paths (typically 10cm) in order to measure small CO2 concentrations. This in turn has a large impact on the physical size of the sensing system. Of the many applications requiring online CO2 sensing packages (such as medical, petroleum, environmental and water treatment)the horticultural industry is the primary focus for this research. CO2 sensing systems are primarily used in horticulture to monitor the produce environment and help extend storage time. For these applications CO2 concentrations are typically low (in the range 0 to 1%) and the paramount need is for low-cost (and possibly disposable) sensing packages. The basis of the measurement technique is the use of bulk (but small volume) aqueous chemical reaction under mechatronic control. Unlike thin film technologies where very thin membranes are passively exposed to the gaseous sample, here a small volume (approximately 2mL) of simple and very cheap liquid chemical indicator (calcium hydroxide solution) is used to produce an opaque precipitate. CO2 concentration is then assessed by low-cost optical attenuation measurements of the developing opacity of the solution. The instrumentation package comprises pumps, flowmeter, reaction cell and infra-red optics for the turbidity measurement, plus reagent and waste vessels, pipelines and electronics. During each measurement cycle, the reaction cell is flushed, with fresh chemical indicator and a sample of gas admitted. The indicator and the sample gas are then vigorously mixed and the change in the indicators optical properties measured at regular intervals. An embedded 8-bit microcontroller performs the necessary analysis to deduce the CO2 concentration (as percentage by volume) for the sample gas by reference to one or more of five ``Time-To-Threshold'' calibration models. These models evaluate the trend in turbidity development as precipitate is formed. First and second prototypes of the measurement system have been constructed and their (low-cost) components and overall performance evaluated, the first a `proof-of-concept' and the second to investigate methodology shortcomings. As a result the design of a third prototype is outlined. The measurement systems have been shown to work adequately well within expected limitations, resulting in a usable low-cost measurement technique. The current prototypes have a useful range of at least 5% to 100% CO2 with a discrimination of typically +-6%. Deficiencies, particularly performance at low concentrations, are identified and potential enhancements for future prototypes proposed.

Surface acoustic wave (SAW) devices are a solution for today's ever growing need for passive wireless sensors. Orthogonal frequency coding (OFC) together with time division multiplexing (TDM) provides a large number of codes and coding algorithms producing devices that have excellent collision properties. Novel SAW noise-like refector (NLR) structures with pulse position modulation (PPM) are shown to exhibit good auto- and cross-correlation, and anti-collision properties. Multi-track, multi-transducer approaches yield devices with adjustable input impedances and enhanced collision properties for OFC TDM SAW sensor devices. Each track-transducer is designed for optimum performance for loss, coding, and chip reflectivity. Experimental results and theoretical predictions confirm a constant Q for SAW transducers for a given operational bandwidth, independent of device and transducer embodiment. Results on these new NLR SAW structures and devices along with a new novel 915 MHz transceiver based on a software radio approach was designed, built, and analyzed. Passive wireless SAW temperature sensors were interrogated and demodulated in a spread spectrum correlator system using a new adaptive filter. The first-ever SAW OFC four-sensor operation was demonstrated at a distance of 1 meter and a single sensor was shown to operate up to 3 meters. Comments on future work and directions are also presented.
ID: 029809964; System requirements: World Wide Web browser and PDF reader.; Mode of access: World Wide Web.; Thesis (Ph.D.)--University of Central Florida, 2011.; Includes bibliographical references (p. 161-166).
Ph.D.
Doctorate
Electrical and Computer Engineering
Engineering and Computer Science

Récemment, les systèmes multicapteurs ont trouvé de nombreuses applications dans des domaines tels que l’industrie agroalimentaire, l’environnement, la médecine et la défense. Parmi les technologies existantes, les capteurs à ondes acoustiques de surface sont l’une des plusprometteuses et fait l’objet de nombreuses recherches. Les travaux décrits dans ce manuscrit concernent le développement d’algorithmes permettant la reconnaissance de composés chimiques et l’estimation de leur concentration. Cette étude décrit une méthode permettant d’estimer les paramètres des phénomènes de transduction. L’intérêt de ces derniers est mis en évidence expérimentalement dans des applications consistant à identifier des toxiques chimiques, des capsules de café contrefaites et à détecter la présence de DMMP et de 4-NT en présence d’interférents
Recently, gas sensor arrays have found numerous applications in areas such as the food, the environment, the medicine and the defenseindustries. Among the existing technologies, the surface acoustic wave technology is one of the most promising and has been the subject of abundant research. The work described in this manuscript concerns the development of algorithms allowing the recognition of chemical compounds and the estimation of their concentration. This study describes a method for estimating the parameters of transduction phenomena. Their interest is demonstrated experimentally in applications consisting in identifying toxic chemical compounds, counterfeit coffee capsules and in detecting the presence of DMMP and 4-NT in the presence of interfering compounds

En las últimas dos décadas, han surgido diferentes tecnologías acústicas para aplicaciones biosensoras como alternativas a tecnologías de detección bien establecidas ¿acústicas o ópticas¿ como son la Microbalanza de Cuarzo (QCM, por sus siglas en inglés) y la Resonancia de Plasmón de Superficie (SPR, de sus siglas en inglés). En la primera parte de este documento se revisan dichas tecnologías alternativas para aplicaciones en medio líquido. Como resultado de esta revisión, se determina que los dispositivos de onda acústica superficial Love (LW, de sus siglas en inglés) son los más prometedores y viables para conseguir el principal objetivo de esta Tesis, que es establecer una comparativa en las mismas condiciones entre inmnosensores desarrollados con la tecnología seleccionada en esta tesis y los inmunosensores desarrollados con QCMs de Alta Frecuencia Fundamental (HFF-QCM, por sus siglas en inglés). Después de esta revisión se presenta el estado del arte de los dispositivos LW en su aplicación como biosensores, así como una discusión de las tendencias y retos actuales de este tipo de sensores. Posteriormente se reúne la información más actualizada sobre aspectos de diseño, principios de operación y modelado de estos sensores. Algunos aspectos de diseño son estudiados y probados para establecer el diseño final de los dispositivos LW. Previamente a su fabricación, también se realizan simulaciones para modelar el comportamiento del dispositivo elegido previamente a su fabricación. Posteriormente, se describe la fabricación del dispositivo así como la celda de flujo diseñada para trabajar con el dispositivo en medios líquidos. Adicionalmente, un sistema electrónico de caracterización, previamente validado para sensores QCM, se adapta para sensores LW. Como resultados, se valida el sistema electrónico para caracterizar los sensores LW fabricados y montados en la celda de flujo y, finalmente, se desarrolla un inmunosensor para la detección del pesticida carbaril que se compara con otras tecnologías inmunosensoras.
In the last two decades, different acoustic technologies for biosensors applications have emerged as promising alternatives to other better established detection technologies ¿ acoustic or optic ones- such as traditional Quartz Crystal Microbalance (QCM) and Surface Plasmon Resonance (SPR). The alternative acoustic technologies for in liquid measurements are reviewed in this manuscript. Surface Acoustic Wave (SAW) Love Mode or Love Wave (LW) sensors are determined to be the most promising and viable option to work with for achieving the main aim of this Thesis. Such aim is the development of a LW immunosensor for its comparison with the same application based on High Fundamental Frequency-QCM (HFF-QCM) sensors and under the same conditions. Consequently, the state-of-the-art of LW devices for biosensing is provided and a discussion about the current trends and future challenges of these sensors is presented. In order to start working with suitable LW devices, upto- date information regarding the design aspects, operation principles and modeling of such devices is gathered. Some design aspects are explored and tested to establish the design of the final LW device. Different simulations for modeling the chosen device behavior are carried out before its fabrication. Later, the device fabrication is described. Next, to start working with the fabricated device in liquid media, a flow cell is designed and implemented. In addition, an electronic characterization system, previously validated for QCM sensors, is adapted and tested for the fabricated LW device. As results, the adapted electronic characterization system is validated for LW devices mounted in the fabricated flow cell and, finally, a LW-based immunosensor for the determination of carbaryl pesticide was developed and compared with other immunosensor technologies.
Rocha Gaso, MI. (2013). Analysis, implementation and validation of a Love mode surface acoustic wave device for its application as sensor of biological processes in liquid media [Tesis doctoral]. Editorial Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/32492
Alfresco

Les travaux décrits dans ce mémoire ont pour but de conduire à la réalisation de capteurs et de filtres à ondes élastiques de surface (SAW) innovants, passifs et sans fil, dédiés à une utilisation en environnement sévère. Différentes structures de composants SAW sont alors étudiées. Les caractéristiques générales, telles que les pertes d’insertion ou les bandes passantes relatives atteignables, des structures usuelles (résonateurs, lignes à retard, LCRF, filtres en échelle…) sont connues de l’homme de l’art. Cependant, pour concevoir un dispositif SAW qui respecte les critères d’un cahier des charges donné, il est impératif de définir le comportement spécifique de chaque dispositif avant son envoi en production.Pour ce faire, des modèles numériques sont développés, qui incluent à la fois la possibilité d’analyser le comportement de systèmes à la géométrie complexe (filtres en échelles, transducteurs apodisés) et qui prennent en compte la présence de phénomènes perturbateurs (modes transverses, pertes liées à la nature des matériaux). La comparaison entre les calculs numériques et les mesures a mis en avant l’adéquation des résultats expérimentaux et de calculs.La mise en place de ces outils permet le développement de capteurs et filtres SAW innovants grâce à une analyse numérique rapide et fiable de leur comportement.Ainsi, l’étude de résonateurs et capteurs dédiés à une utilisation à des températures excédant les 700°C est menée. Il est démontré qu’en dépit de son inhomogénéité, le Ba2TiSi2O8 est un matériau adapté à la réalisation de SAW soumis à des températures élevées pour des fréquences de l’ordre de 300 MHz jusqu’au GHz.Par ailleurs, une structure disposant d’un transducteur à trois doigts par longueur d’ondes est utilisée dans le but de réaliser des résonateurs insensibles aux effets de la directivité lorsque la température évolue. Cette même configuration a mis en exergue la possibilité de réaliser des capteurs n’utilisant qu’un seul résonateur (contre au moins deux jusqu’à présent). Ce dernier point permet de limiter l’encombrement des composants et résout la problématique du vieillissement différentiel des structures.Un second type de capteurs, passifs et sans fil, fondés sur l’utilisation d’un seul SAW et dédiés à la mesure d’hygrométrie, a été étudié. Dans cette nouvelle configuration, un SAW de type LCRF est utilisé comme transpondeur et la zone sensible est externalisée. La sensibilité des modes (de plus d’un MHz) à la variation d’un élément capacitif ou d’une antenne dipôle a été mise en avant numériquement. En pratique, la fabrication des dispositifs a montré une variation différentielle de plusieurs centaines de kHz des résonances selon la condition électrique appliquée à l’un des ports.Finalement, des filtres, dédiés aux applications stratégiques, agiles en fréquence sont réalisés. L’objectif de faire varier la fréquence centrale des dispositifs au cours de leur fonctionnement est atteinte en modifiant les conditions électriques appliquées aux réflecteurs. Deux types de tirage en fréquence sont observés : un glissement fin, de quelques ‰ de la fréquence centrale, cyclique, et un saut de fréquences lié au glissement et à l’ouverture de la bande de Bragg des miroirs aux hautes fréquences. La fabrication des structures et leur connexion à des interrupteurs MEMS validé la faisabilité de la structure.Ces travaux mettent en lumière les capacités de prédiction du comportement des structures SAW grâce au développement de logiciels dédiés. De plus, l’étude et la réalisation de filtres et capteurs innovants ouvre la voie à de nouvelles fonctionnalités
This thesis aims at designing innovative, passive and wireless surface acoustic waves (SAW) sensors and filters, dedicated to harsh environments. Several types of SAW components are consequently studied. The main characteristics, such as insertion losses or relative bandwidth, of usual structures (resonators, delay lines, LCRF, ladder filters…) are known by men of the art. However, to design a SAW device that respects specific requirements, the definition of the proper behavior of each device must be established before the manufacturing.For this purpose, numerical models are developed. Not only they include the possibility to analyse he beha-vior of systems with complex geometry (ladder filters, apodised transducers) but they take into account disturbing phenomena (transverse modes, losses due to the intrinsic nature of the materials). The comparison between computations and measures points out the match between experimental results and calculations.The implementation of these tools allows the development of innovative SAW sensors and filters thanks to a fast and reliable numerical analysis of their behavior.Thus, the design of resonators and sensors dedicated to a use at temperatures exceeding 700°C is studied. It is demonstrated that despite its inhomogeneity, Ba2TiSi2O8 is suitable for the manufacturing of SAW devices subject to high temperatures and in a frequency range from 300 MHz to the GHz.Furthermore, a structure composed of a three electrodes per wavelength transducer is used to produce re-sonators that are not subject to directivity effects when the temperature changes. This configuration offers the possibility to design sensors that use a single resonator (versus at least two until now). This last point makes smaller components possible and solves the question of a differential aging of the structures.A second type of sensors, also passive and wireless, dedicated to humidity measurements, based on the use of a single SAW, is studied. In this new configuration, a LCRF is used as a transponder and the sensitive area is outsourced. The mode sensitivity (of more than a MHz) to the variation of a capacitance or a dipole antenna is numerically brought to light. In practice, the device manufacturing showed a differential variation of the resonances of about 600 kHz depending on the electric condition applied to one of the ports.Finally, filters, dedicated to strategic applications, with frequency agility are designed. The purpose is to make the frequency vary depending on the electrical conditions applied to the mirrors. Two kinds of agility are identified : a slight sliding, of a few ‰ of the initial central frequency, periodic, and a frequency jump due to the shift of the Bragg band to the high frequencies. The manufacturing of some structures and their connection to MEMS switches attest the feasibility of such a structure.This work highlights the ability to predict the behavior of SAW structures thanks to the development of dedicated software. Moreover, the analysis and the manufacturing of innovative sensors and filters pave the way to new functionalities

Ces travaux ont donc visé le développement d’une plateforme complète de détection de gaz pour environnement sévère haute température. Cette plateforme intègre un dispositif à ondes acoustiques de surface sur substrat Langasite, une résistance chauffante, une couche sensible inorganique nanostructurée et est placée dans une enceinte hermétique. Des températures de l’ordre de 450°C ont été atteintes et des tests de cyclages ont démontré un fonctionnement en accord avec les modèles théoriques et une reproductibilité des mesures. Des tests de détection de composés organiques volatils (éthanol et toluène) ont mis en avant des seuils de détection de l'ordre de quelques ppm
Measuring pollutants concentrations in gas and vapors emissions are important environmental issues. This work presents a stand-alone portable device for high temperature assessment. The system includes a Langasite (LGS) acoustic sensor, a ceramic heater and a platform with RF connections for remote in-situ measurements. The packaging consists in a hermetic stainless steel cell which enables safe gas detection. In situ temperature measurements have been achieved and the thermal behavior was successfully investigated in the temperature range 25-450°C. The designed cell highlights good agreement with theoretical models and reproducibility of the measures. Volatile organic compounds exposures have been investigated and promising ppm level detections have been obtained

Surface acoustic wave (SAW) sensors offer a wireless, passive sensor solution for use in numerous environments where wired sensing can be expensive and infeasible. Single carrier frequency SAW sensor embodiments such as delay lines, and resonators have been used in single sensor environments where sensor identification is not a necessity. The orthogonal frequency coded (OFC) SAW sensor tag embodiment developed at UCF uses a spread spectrum approach that allows interrogation in a multi-sensor environment and provides simultaneous sensing and sensor identification. The SAW device is encoded via proper design of multiple Bragg reflectors at differing frequencies. To enable accurate device design, a model to predict reflectivity over a wide range of electrode metallization ratios and metal thicknesses has been developed and implemented in a coupling of modes (COM) model. The high coupling coefficient, reflectivity and temperature coefficient of delay (TCD) of YZ LiNbO[sub3] makes it an ideal substrate material for a temperature sensor, and the reflectivity model has been developed and verified for this substrate. A new concept of pseudo-orthogonal frequency coded (POFC) SAW sensor tags has been investigated, and with proper design, the POFC SAW reduces device insertion loss and fractional bandwidth compared to OFC. OFC and POFC sensor devices have been fabricated at 250 MHz and 915 MHz using fundamental operation, and 500 MHz and 1.6 GHz using second harmonic operation. Measured device results are shown and compared with the COM simulations using the enhanced reflectivity model. Additionally, the first OFC devices at 1.05 GHz were fabricated on 128[superscript o] YX LiNbO[sub3] to explore feasibility of the material for future use in OFC sensor applications. Devices at 915 MHz have been fabricated on YZ LiNbO[sub3] and integrated with an antenna, and have then been used in a transceiver system built by Mnemonics, Inc. to wirelessly sense temperature.; The first experimental wireless POFC SAW sensor device results and predictions will be presented.
ID: 029809657; System requirements: World Wide Web browser and PDF reader.; Mode of access: World Wide Web.; Thesis (Ph.D.)--University of Central Florida, 2011.; Includes bibliographical references (p. 148-152).
Ph.D.
Doctorate
Electrical Engineering and Computer Science
Engineering and Computer Science

Les capteurs à ondes de surface (SAW) présentent plusieurs intérêts, tels que leur robustesse, leur adaptabilité et leur faible coût de fabrication. Un des facteurs de performance de ce type de capteur est sa sensibilité. Généralement pour l’améliorer les efforts se concentrent sur la couche sensible. Une alternative innovante est l’augmentation de la surface active en porosifiant le substrat. L’ouverture du matériau piézoélectrique le long du chemin de propagation permettra, ainsi, la captation des espères dans les pores du substrat. L’objectif de cette thèse est de proposer une nouvelle architecture de capteur permettant l’usage du silicium poreux en tant que couche guidante et sensible
Surface wave sensors (SAW) have several advantages, such as robustness, adaptability and low manufacturing costs. One of the key performance factors of this type of sensor is its sensitivity. Generally to improve it, the efforts focus on the sensitive layer. An innovative alternative is the increase of the active surface by porosifying the substrate. The opening of the piezoelectric material along the path of propagation and its replacement by porous silicon will thus enable the capture of the species to be detected in the pores. The objective of this thesis is to propose a new sensor architecture allowing the use of porous silicon as a guiding and sensing layer

This thesis concentrates on the interaction between SAWs (surface acoustic wave) and low-dimensional systems studied using optical techniques. In particular SAW-driven luminescence from a lateral p-n junction is demonstrated. The lateral p-n junction is formed by molecular beam epitaxy regrowth on a patterned GaAs substrate. Silicon is used as an amphoteric dopant to create a high mobility two-dimensional electron gas on flat (100) planes and a two-dimensional hole gas on angled (311)A facets. A lateral p-n junction is formed at the interface between these planes. SAWs with a frequency of ~1 GHz are generated using an interdigitated transducer. When a continuous radio frequency (RF) signal is used to excite the transducer, SAW-driven light emission from the p-n junction is demonstrated by peaks in the current/light emission at the resonant frequency of the transducer. To investigate the nature of the luminescence further, short RF pulses are used to drive the transducer. The short pulses temporally isolate the SAW-driven light emission from any emission due unwanted pick-up of the free space electromagnetic wave. In the final section the modulation of the emission energies of a single self-assembled quantum dot by a SAW is investigated. The compression and expansion of the crystal due to the strain wave causes the energy of the dot lines to oscillate around their equilibrium values. The shape of the SAW broadened emission lines was seen to depend on the nature of the transition in the dot offering an alternative way of identifying charged and neutral species in this sample. The modulation of the dot energy levels by the SAW is used to control the time of photon emission from the system.

In the last decade, miniaturised “lab-on-a-chip” (LOC) devices have attracted significant interest in academia and industry. LOC sensors for electrochemical analysis now commonly reach picomolar in sensitivities, using only microliter-sized samples. One of the major drawbacks of this platform is the diffusion layer that appears as a limiting factor for the sensitivity level. In this thesis, a new technique was developed to enhance the sensitivity of electroanalytical sensors by increasing the mass transfer in the medium. The final device design was to be used for early detection of cancer diseases which causes bleeding in the digestive system. The diagnostic device was proposed to give reliable and repeatable results by additional modifications on its design. The sensitivity enhanced-sensor model was achieved by combining the surface acoustic wave (SAW) technology with the electroanalytical sensing platform. The technique was practically tested on a diagnostic device model and a biosensing platform. A novel, substrate (TMB) based label-free Hb sensing method is developed and tested. Moreover, the technique was further developed by changing the sensing process. Instead of forming the sensitive layer on the electrodes it was localised on polystyrene wells by a rapid one-step process. Results showed that the use of acoustic streaming, generated by SAW, increases the current flow and improves the sensitivity of amperometric sensors by a factor of 6 while only requiring microliter scale sample volumes. The heating and streaming induced by the SAW removes the small random contributions made by the natural convection and temperature variation which complicate the measurements. Therefore, the method offers stabilised conditions for more reliable and repeatable measurements. The label-free detection technique proved to be giving relevant data, according to the hemoglobin concentration. It has fewer steps than ELISA and has only one antibody. Therefore, it is quick and the cross-reactivity of the second antibody is eliminated from the system. The additional modifications made on the technique decreased the time to prepare the sensing platform because the passivation steps (i.e., pegylation), prior to structuring a sensitive layer were ignored. This avoidance also increased the reliability and repeatability of the measurements.

Les capteurs à ondes acoustiques de surfaces (SAW : Surface Acoustic Waves) présentent de nombreux avantages, dont une grande sensibilité, un paramètre clé dans diverses applications. Dans cette thèse, deux voies sont explorées pour améliorer la sensibilité des dispositifs SAWs : le passage en mode de Love, avec une couche guide d’onde en résine époxyde SU-8, et la montée en fréquence de 104 à 208 MHz. Avant de réaliser de tels dispositifs en salle blanche puis de les utiliser en tant que capteurs chimiques, des simulations numériques ont été entreprises, en utilisant tout d’abord le logiciel MATLAB, puis par la méthode des éléments finis, via le logiciel COMSOL Multiphysics. L’épaisseur optimale de la couche guide d’onde, permettant un gain important en sensibilité, a été estimée. Un écart entre l’expérience et la simulation a été trouvé soulignant la nécessité de poursuivre les phases d’optimisation dans cette voie. Une confrontation calculs/expériences a été menée avec succès pour les structures SH-SAW. Ces dispositifs ont été fonctionnalisés avec un dérivé d’anthracène pour détecter les ions zinc en milieu aqueux. Les résultats gravimétriques ont montré un gain en sensibilité d’un facteur 2.3, en augmentant la fréquence de travail de 104 MHz à 208 MHz
Surface Acoustic Wave (SAW) sensors have many advantages mainly a high sensitivity, which is a key parameter in various applications. Two strategies were explored, in this thesis, to enhance the sensitivity of SAW devices: switching to Love mode, with a waveguide layer in SU-8 epoxy resin, and frequency increase from 104 to 208 MHz. Prior to the realization of such devices in a clean room and their further use as chemical sensors, numerical simulations were done, first with MATLAB software, and then with the finite element method, via COMSOL Multiphysics software. The optimum thickness of the waveguide layer, allowing a significant gain in sensitivity, was estimated. A disagreement between experience and simulation was found highlighting the need to continue optimization steps. A confrontation between calculations / experiments was carried out for the SH-SAW structures. These devices were functionalized with an anthracene derivate for zinc ions detection in aqueous media. Gravimetric results indicate that increasing the operating frequency from 104 MHz to 208 MHz permits a gain in sensitivity by a factor of 2.3

Immunofluorescence assays are capable of both detecting the amount of a protein and the location of the protein within a cell or tissue section. Unfortunately, the traditional technique is not capable of detecting concentrations on the nanoscale. Also, the technique suffers from non-specific attachment, which can cause false-positives, as well as photobleaching when detecting lower concentrations is attempted. There is also a time constraint problem since the technique can take from many hours to a few days in some cases. In this work, metal-enhanced fluorescence (MEF) is used to lower the detection limit and reduce photobleaching. Unfortunately, MEF also increases the intensity of non-specifically bound proteins (NSBPs). Therefore, a surface acoustic wave (SAW) device is used to remove the more weakly bound NSBPs. Previously, this has been shown on lithium niobate, but it is used with a quartz substrate in this work. The SAW device is also used to cause micro-mixing which speeds the process up significantly. In this research, it was found that silver nanocubes can lower the detection limit down to below 1 ng/mL. Quartz SAW devices are shown to remove NSBPs at a power of 10 mW applied for five minutes. Micro-mixing is shown to be improved by a factor of six at 10 mW for 10 minutes by saturating the antibody used in this research, which takes 1 hour without micro-mixing. Finally, all three components are combined. In this work, the whole device is used to detect 50 ng/mL. After micro-mixing, the intensity is the same as with MEF, and, after removal, it has been lowered by 7 a.u.

A semiconductor optical source monolithically integrated with a surface acoustic wave (SAW) Bragg-cell to operate as a functional device is proposed in this thesis. The practical structure of such an integrated device is demonstrated and design guidelines are presented. Compared with conventional optical beam processed devices, this functional integrated semiconductor optical source (FISOS) is revised to be compact in size, flexible in function and potentially robust in performance.
The FISOS is analyzed as two sub-divisions, optical source and acoustic processor, which have the common substrate structure. The optical beams excited from the optical source part of the device undergoes a scattering in the Bragg grating formed by SAWs that are generated by an IDT positioned on top of the acoustic processing part of device. By altering the property (power, frequency, etc.) of the SAW, versatile functionalities such as modulation, filtering, beam steering and so on of the optical beams can be realized in this optical source device.
A multilayer structure based on GaN/InGaN MQWs grown on sapphire is designed for the FISOS to be blue light emitting and efficiently launching SAWs. An etch-down technique employed in the SAW processing part is taken to improve the overlap between the optical and acoustic waves and then the interaction efficiency. Optimizations to the geometrical dimensions of the FISOS, such the width of the ridge waveguide, the position of the IDT and the etching depth, etc., are discussed in the given structure.
Numerical models are investigated to access the operational characteristics and then to provide design guidelines for the proposed integrated device. The Bragg diffraction of optical waves occurring within the acoustic waves in the proposed structure are simulated as a two-dimensional interaction between two guided optical modes and an acoustic surface wave.
The modal distributions and propagation velocities of SAWs in a multilayer system are calculated using Adler’s matrix method. The electrical characteristics of an IDT, such as impedance, insertion loss, electromechanical constant and so on are also discussed.
Transverse and lateral optical modes in the given multilayer structure are analyzed by the transfer matrix method. The interaction of optical waves and acoustic waves are modeled using the rigorous grating diffraction theory. Starting from Floquet’s theory, the well-known coupled-wave method and modal method can both be derived from the rigorous grating diffraction theory. Discussions of some useful approximate methods are also presented. In this thesis, the simulations of the acoustooptic interaction are performed using the coupled-wave method.
From the simulation results, the angular distribution profile and spatial profile of the output of the FISOS are evaluated. An improvement to the expression of the diffraction efficiency in such an integrated device is proposed. The so-called beam diffraction efficiency gives a more complete measure to the acoustooptic diffraction and is used to investigate the features of FISOS different from conventional acoustooptic devices. Contour plots of the beam efficiency varying with acoustic frequency and power in a FISOS is demonstrated to be a convenient and powerful approach in the device design.
The operational performances of an integrated deflector and a modulator in FISOS are analyzed to investigate the feasibility of FISOS. The trade-off of the efficiency-resolution in an integrated deflector design is discussed. Short interaction length, high acoustic frequency and narrow ridge are proved to be helpful for a larger number of resolvable spots with a fairly high efficiency. In the case of the integrated modulator, given that the figure of merit Q is fixed, it is demonstrated that the smaller the Q, the longer the interaction length, larger ridge width and lower acoustic frequency will give rise to a larger bandwidth, though the highest efficiency might appear at a higher frequency.
Some practical issues such as the misalignment of planar elements on the device and the incoherence of the integrated optical source are also discussed. A modified working frequency can be used to compensate the efficiency loss in the former case; in the latter case, it is demonstrated that a distortion of beam diffraction efficiency versus acoustic power with an incoherent optical source arises due to the wide spectrum of the incident optical waves.

The object of this thesis research is to facilitate the appraisal and analysis of the signatures of the modern acoustic wave biosensors, as well as to improve the experimental methodology to enhance sensor performance. For this purpose, both theoretical characterization of acoustic wave sensor signatures and experimental studies for the most frequently used acoustic wave biosensors, the liquid phase QCM (quartz crystal microbalance) and the vapor phase SAW (surface acoustic wave) sensors, are presented. For the study of SAW vapor phase detection, the author fabricated different types of two-port SAW resonator sensors on quartz substrates and designed and performed a significant number of detection experiments. These were conducted both with calibrated or known target samples under laboratory conditions at Georgia Tech Hunt Lab and with samples of unknown concentrations such as seized crack cocaine (courtesy of Georgia Bureau of Investigation, GBI) to see the sensors capability to work in the field conditions. In addition, the dependence of the SAW sensor signatures on specific locations of the surface perturbation was investigated to account for some observed abnormal responses. Finally, a novel approach to classify and visualize chemically analogous substances is introduced. The author expects that the thesis work herein may contribute to the study of the modern acoustic wave biosensors which includes but is not limited to: the establishment of underpinning theory that will aid in the evaluation of the signatures; the practical aspects of design and fabrication of SAW devices specific to the vapor phase immunoassay; the development of efficient experimental methodologies; the strategic immobilization of a biolayer on SAW resonator based biosensors; and, the acquisition of reference data for the development of commercial acoustic wave sensors.

Mechanical properties are important tissue parameters of skin that are useful for understanding skin patho-physiology, and aiding disease diagnosis and treatment. They are indicators of functional changes and pathological variations in the micro-structure. This research thesis studies the intersection of acoustics, optics and biomechanics for skin mechanical properties measurement. Surface acoustic wave (SAW) is induced and applied to a range of different tissue mimicking phantom models, Thiel cadavers and in vivo human skin. Different optical systems, i.e. low coherence interferometer and phase sensitive optical coherence tomography (PhS-OCT), are employed to detect the SAW. The Young’s moduli and thicknesses of model layers are assessed by the analysis of the wave phase velocity curves. The PhS-OCT detection system can also provide the real time high resolution depth-resolved cross-sectional microstructure imaging of the interrogated sample to assist the elasticity evaluation of the heterogeneous tissue. Results prove that the novel combination of optical imaging technology with SAW method is able to assess the elasticity change in both axial and transverse directions in soft material. It can be used to evaluate the mechanical properties of single, double-layer soft tissue mimicking phantoms and different sites of human skin ex vivo and in vivo non-invasively. This study also demonstrates that the SAW method can be successfully utilized to map the elasticity of soft heterogeneous tissues quantitatively. The results represent an important step towards the development of SAW method as a clinical diagnosis tool in dermatology, and may offer potential in diagnostic and therapeutic clinical applications.

For centuries scientific ingenuity and innovation have been influenced by Mother Natures perfect design. One of her more elusive designs is that of the sensory olfactory system, an array of highly sensitive receptors responsible for chemical vapor recognition. In the animal kingdom this ability is magnified among canines where ppt (parts per trillion) sensitivity values have been reported. Today, detection dogs are considered an essential part of the US drug and explosives detection schemes. However, growing concerns about their susceptibility to extraneous odors have inspired the development of highly sensitive analytical detection tools or biosensors known as electronic noses. In general, biosensors are distinguished from chemical sensors in that they use an entity of biological origin (e.g. antibody, cell, enzyme) immobilized onto a surface as the chemically-sensitive film on the device. The colloquial view is that the term biosensors refers to devices which detect the presence of entities of biological origin, such as proteins or single-stranded DNA and that this detection must take place in a liquid. Our biosensor utilizes biomolecules, specifically IgG monoclonal antibodies, to achieve molecular recognition of relatively small molecules in the vapor phase.

The objective of this dissertation is to improve the performance of surface acoustic wave (SAW) biosensors for use in point-of-care-testing (POCT) applications. SAW biosensors have the ability to perform fast, accurate detection of an analyte in real time without the use of labels. However, the technology suffers from the inability to differentiate between specific and non-specific binding. Due to this limitation, direct testing of bodily fluids using SAW sensors to accurately determine an analyte's concentration is difficult. In addition, these sensors are challenged by the need to detect small concentrations of a biomarker that are typically required to give a clinical diagnosis. Sensitivity, selectivity and reliability are three critical aspects for any sensing platform. To improve sensitivity the delay path of a SAW sensor has been modified with microcavities filled with various materials. These filled cavities increased sensitivity by confining wave energy to the surface by way of constructive interference and waveguiding. Thus, the improved sensitivity will result in a lower limit of detection. In addition, insertion loss is decreased as a consequence of increased wave confinement to the surface. Sensor selectivity and reliability are adversely affected by non-specific binding of unwanted species present in a sample. To address this issue a multifunctional SAW sensor is presented. The sensor consists of two SAW delay lines oriented orthogonal to each on ST-quartz in order to generate two distinct wave modes. One wave mode is used for sensing while the other is used to remove loosely bound material. By using the same transduction mechanism for both removal and sensing, the sensor chip is simplified and complex electronics are avoided. The findings of this research involve the technological advances for SAW biosensors that make their use in POCT possible.

Volatile organic compounds (VOCs) are a precursor to the formation of ground-level ozone and airborne particulate matter, both of which are hazardous to human health. Currently in Canada, other air pollutants such as ozone and nitrous oxides are measured by an air quality monitoring network in real-time, while VOCs are collected in canisters and sent to a central laboratory for analysis. This is a time-consuming and non real-time method, and due to the spatial variability of air pollution, many points of measurement are needed. A distributed point sensor network could address the resolution and real-time challenges, but would impose an added operating expenditure burden on air quality monitoring agencies. Low-cost, yet sensitive chemical sensors could contribute to lowering operating expenditures of a network’s sensing units over the installed lifetime of the units. The objective of this work was to lay the groundwork for a sensing platform from which low-cost yet sensitive chemical sensors can be developed. The sensing platform is an all-polymer surface acoustic wave (SAW) device, and the materials selected for its fabrication are Polyvinylidene Fluoride (PVDF) for the sensor substrate and Poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate) (PEDOT:PSS) for the interdigital transducer electrodes. In this work, an apparatus and a process for preparing piezoelectric PVDF film was developed. PVDF-based resonators were successfully demonstrated. In addition, repeatable processes for inkjet micropatterning highly electrically conductive PEDOT:PSS electrode tracks on PVDF were developed for three inkjet nozzle orifice sizes (20, 30, 40 µm). For tracks micropatterned using the same process, the electrical resistances have a standard deviation of 8.5% of the average. The electrical conductivity of micropatterned tracks is approximately 150 S/cm, or one-sixth of the manufacturer’s claimed bulk film conductivity. Using the 30 µm nozzle, the smallest electrode track width that can be micropatterned repeatably is 75 µm. A track width of 55 µm was achieved using the 20 µm nozzle.

This thesis addresses the development of new gas sensor using surface acoustic wave (SAW) technology. SAW sensors detect the change in mass, modulus, and conductivity of a sensing layer material via absorption or adsorption of an analyte. The advantage of SAW sensor includes low cost, small size, high sensitivity. We investigated the use of nano-crystalline palladium film for sensing hydrogen gas. We also investigated SAW fabrication for radio frequency (RF) range operation where high signal-to-noise ratios can be achieved. A test-bed consisting of a gas dilution system, a temperature-controlled test cell, a network analyzer, and computer-based measurement system was used for evaluating the performance of SAW gas sensors at very low concentrations. Both single and dual delay line SAW devices were fabricated by means of photolithography on a lithium niobate substrate. Tests are carried to determine response speed, resolution, reproducibility, and linear characteristics, over a range of analyte concentrations.

Surface acoustic wave (SAW) sensors provide versatility in that they can offer wireless, passive operation in numerous environments. Various SAW device embodiments may also be employed for retrieval of the sensed data. Single sensor systems typically use a single carrier frequency and a simple device embodiment since tagging is not required. However, it is necessary in a multi-sensor environment to both identify the sensor and retrieve the information. Overlapping sensor data signals in time and frequency present problems when attempting to collect the sensed data at the receiver. This dissertation defines a system simulation environment exclusive to SAW sensors. The major parameters associated with a multi-device system include the transmitter, the channel, and the receiver characteristics. These characteristics are studied for implementation into the simulation environment. A coupling of modes (COM) model for SAW devices is utilized as an accurate software representation of the various SAW devices. Measured device results are presented and compared with COM model predictions to verify performance of devices and system. Several coding techniques to alleviate code collisions and detection errors were investigated and evaluated. These specialized techniques apply the use of time, frequency, and spatial diversity to the devices. Utilizing these multiple-access techniques a multi-device system is realized. An optimal system based on coding technique, frequency of operation, range, and related parameters is presented. Funding for much of this work was provided through STTR contracts from NASA Kennedy Space Center.
Ph.D.
School of Electrical Engineering and Computer Science
Engineering and Computer Science
Electrical Engineering PhD

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Bachelors
Engineering and Computer Science
Engineering

Surface acoustic wave (SAW) devices find uses in a plethora of applications including but not limited to chemical, biological sensing, and microfluidic actuation. The primary aim of this dissertation is to develop a SAW biosensor, capable of simultaneous detection of target biomarkers in fluid media at concentrations of picogram/ml to nanogram/ml levels and removal of non-specific proteins from sensor surface using the process of acoustic streaming, for potential chemical sensing, medical, and clinical diagnostic applications. The focus is on the development of three dimensional finite element structural and fluid-structure interaction models to study wave propagation and acoustic actuation of fluids in a SAW biosensor. This work represents a significant improvement in understanding fluid flow over SAW devices, over the currently available continuum model of Nyborg. The developed methodology includes use of a novel substrate, namely, Langasite coupled with various combinations of novel multidirectional interdigital transducer (IDT) configurations such as orthogonal, focused IDTs as well as sensor surface modifications, such as micro-cavities. The current approach exploits the capability of the anisotropic piezoelectric crystal to launch waves of different characteristics in different directions, which can be put to the multiple uses including but not limited to sensing via shear horizontal waves and biofouling elimination via Rayleigh wave induced acoustic streaming. Orthogonal IDTs gives rise to constructive interference, thereby enhancing the magnitudes of device displacements and fluid velocities. The net effect is an increase in device sensitivity and acoustic streaming intensity. The use of micro-cavities in the delay path provides a synergistic effect, thereby further enhancing the device sensitivity and streaming intensity. Focused IDTs are found to enhance the device displacements and fluid velocities, while focusing the device displacements and fluid motion at the device focal point, thereby enhancing the SAW device biosensing performance. The work presented in this dissertation has widespread and immediate use for enhancing sensor sensitivity and analyte discrimination capabilities as well as biofouling removal in medical diagnostic applications of SAW sensors. This work also has a broad relevance to the sensing of multiple biomarkers in medical applications as well as other technologies utilizing these devices such as microfluidic actuation.

Surface acoustic wave (SAW) technology has been in use for well over one century. In the last few decades, due to its low cost and high performance, this technology has been widely adopted in modern wireless communication systems, to build filtering devices at radio frequency (RF). SAW filters and duplexers can be virtually found inside every mobile handset. SAW devices are traditionally recognized as passive devices with high linear signal processing behavior. However, recent deployments of third generation (3G) and fourth generation (4G) mobile networks require the handsets to handle an increasing number of frequency bands with more complex modulation /demodulation schemes and higher data rate for more subscribers. These requirements directly demand more stringent linearity specifications on the front end devices, including the SAW duplexers. In the past, SAW duplexer design was based on empirically obtained design rules to meet the linearity specifications. Lack of predictability and an understanding of the root cause of the nonlinearity have limited the potential applications of SAW duplexers. Therefore, research on the nonlinearity characterization and an accurate modeling of SAW nonlinearity for mobile device applications are very much needed. The Ph.D. work presented here primarily focuses on developing a general nonlinear model for SAW resonators/duplexers. Their nonlinear characteristics were investigated by measuring the harmonic and intermodulation distortions of resonators. A nonlinear Mason model is developed and the characterization results are integrated into SAW duplexer design flows to help to simulate the nonlinear effects accurately and improve the linearity performance of the products. In this dissertation, first, a novel nonlinear Mason equivalent circuit model including a third order nonlinear coefficient in the wave propagation is presented. Next, the nonlinear distortions of SAW resonators are analyzed by measuring large-signal harmonic and intermodulation spurious emission on resonators using a wafer probe station. The influence of the setups on the measurement reliability and reproducibility is discussed. Further, the nonlinear Mason model is validated by comparing its simulation results with harmonic and intermodulation measurements on SAW resonators and a WCDMA Band 5 duplexer. The Mason model developed and presented here is the first and only nonlinear physical model for SAW devices based on the equivalent circuit approach. By using this new model, good simulation measurement agreements are obtained on both harmonic and intermodulation distortions for SAW resonators and duplexers. These outcomes demonstrate the validity of the research on both the characterization and modeling of SAW devices. The result obtained confirms that the assumption of the representation of the 3rd order nonlinearity in the propagation by a single coefficient is valid.
Ph.D.
Doctorate
Electrical Engineering and Computer Science
Engineering and Computer Science
Electrical Engineering

We studied the possibility of achieving an order of magnitude reduction in the energy dissipation needed to write bits in perpendicular magnetic tunnel junctions (p-MTJs) by simulating the magnetization dynamics under a combination of resonant surface acoustic waves (r-SAW) and spin-transfer-torque (STT). The magnetization dynamics were simulated using the Landau-Lifshitz-Gilbert equation under macrospin assumption with the inclusion of thermal noise. We studied such r-SAW assisted STT switching of nanomagnets for both in-plane elliptical and circular perpendicular magnetic anisotropy (PMA) nanomagnets and show that while thermal noise affects switching probability in in-plane nanomagnets, the PMA nanomagnets are relatively robust to the effect of thermal noise. In PMA nanomagnets, the resonant magnetization dynamics builds over few 10s of cycles of SAW application that drives the magnetization to precess in a cone with a deflection of ~45⁰ from the perpendicular direction. This reduces the STT current density required to switch the magnetization direction without increasing the STT application time or degrading the switching probability in the presence of room temperature thermal noise. This could lead to a pathway to achieve energy efficient switching of spin-transfer-torque random access memory (STT-RAM) based on p-MTJs whose lateral dimensions can be scaled aggressively despite using materials with low magnetostriction by employing resonant excitation to drive the magnetization away from the easy axis before applying spin torque to achieve a complete reversal.

Diese Dissertation beschäftigt sich mit der Entwicklung eines neuartigen Konzepts für Herstellung und Handhabung von Mikrofluidiksystemen auf der Basis akustischer Oberflächenwellen (SAW) sowie der Nutzung dieses Konzepts zur Fertigung anwendungsrelevanter Teststrukturen. Schwerpunkte sind dabei unter anderem eine hohe Leistungsbeständigkeit und Lebensdauer der Chipbauelemente und eine hohe technologische Flexibilität bezüglich Herstellung und Einsatz. Ausgehend von einer modularen Betrachtungsweise der Bauelemente wurden vielseitig einsetzbare, elektrisch-optimierte Interdigitalwandler entworfen, verschiedene Herstellungsvarianten für vergrabene Interdigitalwandler hoher Leistungsbeständigkeit auf piezoelektrischen Lithiumniobat-Substraten entwickelt und experimentell verifiziert, ein Sputterverfahren für amorphe SiO2-Dünnschichten hoher Qualität optimiert und eine Federstiftkontakt-Halterung entworfen. Durch Kombination dieser Technologien wurden SAW-Bauelemente für die mikrofluidische Aktorik mit hoher Performance und Reproduzierbarkeit entworfen, charakterisiert und beispielhaft für das elektroakustische Zerstäuben von Fluiden und das Mischen in Mikrokanälen eingesetzt.

The analysis and development of robust sensing platforms based on solidly-mounted ZnO bulk acoustic wave devices was proposed. The exploitation of acoustic energy trapping was investigated and demonstrated as a method to define active sensing areas on a substrate. In addition, a new "hybrid" acoustic mode experiencing acoustic energy trapping was studied theoretically and experimentally. This mode was used as an explanation of historical inconsistencies in observed thickness-shear mode velocities. Initial theoretical and experimental results suggest that this mode is a coupling of thickness-shear and longitudinal particle displacements and, as such, may offer more mechanical and/or structural information about a sample under test. Device development was taken another step further and multi-mode ZnO resonators operating in the thickness-shear, hybrid, and longitudinal modes were introduced. These devices were characterized with respect to sample viscosity and conductivity and preliminary results show that, with further development, the multi-mode resonators provide significantly more information about a sample than their single-mode counterparts. An alternative to resonator-based platforms was also presented in the form of bulk acoustic delay lines. Initial conceptual and simulation results show that these devices provide a different perspective of typical sensing modalities by using properly designed input pulses, device tuning, and examining overall input and output signal spectra.

[EN] Different electronic interfaces have been proposed to measure major parameters for the characterization of quartz crystal microbalance (QCM) during the last two decades. The measurement of the adequate parameters of the sensor for a specific application is very important, since an error in this measure can lead to an error in the interpretation of the results. The requirements of the system of characterization depend on the application. In this thesis we propose two characterization systems for two types of applications that involve the majority of sensor applications: 1) Characterization of materials under variable damping conditions and 2) Detection of substances with high measurement resolution. The proposed systems seek to solve the problems detected in the systems currently in use. For applications in which the sensor damping varies during the experiment, we propose a system based on a new configuration of the technique of automatic capacitance compensation (ACC). This new configuration provides the measure of the series resonance frequency, the motional resistance and the parallel capacitance of the sensor. Moreover, it allows an easy calibration of the system that improves the precision in the measurement. We show the experimental results for 9 and 10 MHz crystals in fluid media, with different capacitances in parallel, showing the effectiveness in the capacitance compensation. The system presents some deviation in frequency with respect to the series resonance frequency, as measured with an impedance analyser. These deviations are due to the non-ideal, specific behaviour of some of the components of the circuit. A new circuit is proposed as a possible solution to this problem. For high-resolution applications we propose an integrated platform to characterize high-frequency acoustic sensors. The proposed system is based on a new concept in which the sensor is interrogated by means of a very stable, low-noise external source at a constant frequency, while the changes provoked by the charge in the phase of the sensor are monitored. The use of high-frequency sensors enhances the sensitivity of the measure, whereas the design characterization system reduces the noise in the measurement. The result is an improvement in the limit of detection (LOD). This way, we achieve one of the challenges in the acoustic high-frequency devices. The validation of the platform is performed by means of an immunosensor based in high fundamental frequency QCM crystals (HFF-QCM) for the detection of two pesticides: carbaryl and thiabendazole. The results obtained for carbaryl are compared to the results obtained by another high-frequency acoustic technology based in Love sensors, with the optical technique based in surface plasmonic resonance and with the gold standard technique Enzyme Linked Immunoassay (ELISA). The LOD obtained with the acoustic sensors HFF-QCM and Love is similar to the one obtained with ELISA and improves by one order of magnitude the LOD obtained with SPR. The conceptual ease of the proposed system, its low cost and the possibility of miniaturization of the quartz resonator, allows the characterization of multiple sensors integrated in an array configuration, which will allow in the future to achieve the challenge of multianalyte detection for applications of High-Throughput Screening (HTS).
[ES] Durante las dos últimas décadas se han propuesto diferentes interfaces electrónicos para medir los parámetros más importantes de caracterización de los cristales de microbalanza de cuarzo (QCM). La medida de los parámetros adecuados del sensor para una aplicación específica es muy importante, ya que un error en la medida de dichos parámetros puede resultar en un error en la interpretación de los resultados. Los requerimientos del sistema de caracterización dependen de la aplicación. En esta tesis se proponen dos sistemas de caracterización para dos ámbitos de aplicación que comprenden la mayoría de las aplicaciones con sensores QCM: 1) Caracterización de materiales bajo condiciones de amortiguamiento variable y 2) detección de sustancias con alta resolución de medida. Los sistemas propuestos tratan de resolver la problemática detectada en los ya existentes. Para aplicaciones en las que el amortiguamiento del sensor varía durante el experimento, se propone un sistema basado en una nueva configuración de la técnica de compensación automática de capacidad (ACC). La nueva configuración proporciona la medida de la frecuencia de resonancia serie, la resistencia dinámica y la capacidad paralelo del sensor. Además, permite una fácil calibración del sistema que mejora la precisión en la medida. Se presentan resultados experimentales para cristales de 9 y 10MHz en medios fluidos, con diferentes capacidades en paralelo, demostrando la efectividad de la compensación de capacidad. El sistema presenta alguna desviación en frecuencia con respecto a la frecuencia resonancia serie, medida con un analizador de impedancias. Estas desviaciones son explicadas convenientemente, debidas al comportamiento no ideal específico de algunoscomponentes del circuito. Una nueva propuesta de circuito se presenta como posible solución a este problema. Para aplicaciones de alta resolución se propone una plataforma integrada para caracterizar sensores acústicos de alta frecuencia. El sistema propuesto se basa en un nuevo concepto en el que el sensor es interrogado, mediante una fuente externa muy estable y de muy bajo ruido, a una frecuencia constante mientras se monitorizan los cambios producidos por la carga en la fase del sensor. El uso de sensores de alta frecuencia aumenta la sensibilidad de la medida, por otro lado, el sistema de caracterización diseñado reduce el ruido en la misma. El resultado es una mejora del límite de detección (LOD). Se consigue con ello uno de los retos pendientes en los dispositivos acústicos de alta frecuencia. La validación de la plataforma desarrollada se realiza con una aplicación de un inmunosensor basado en cristales QCM de alta frecuencia fundamental (HFF-QCM) para la detección de dos pesticidas: carbaryl y tiabendazol. Los resultados obtenidos para el Carbaryl se comparan con los obtenidos con otra tecnología acústica de alta frecuencia basada en sensores Love, con la técnica óptica basada resonancia superficial de plasmones (SPR) y con la técnica de referencia Enzyme Linked Immuno Assay (ELISA). El LOD obtenido con los sensores acústicos HFFQCM y Love es similar al obtenido con las técnicas ELISA y mejora en un orden de magnitud al obtenido con SPR. La sencillez conceptual del sistema propuesto junto con su bajo coste, así como la capacidad de miniaturización del resonador de cuarzo hace posible la caracterización de múltiples sensores integrados en una configuración en array, esto permitirá en un futuro alcanzar el reto de la detección multianalito para aplicaciones High-Throughput Screening (HTS).
[CAT] Durant les dues últimes dècades s'han proposat diferents interfases electrònics per a mesurar els paràmetres més importants de caracterització dels cristalls de microbalança de quars (QCM). La mesura dels paràmetres adequats del sensor per a una aplicació específica és molt important, perquè un error en la interpretació dels resultats pot resultar en un error en la interpretació dels resultats. Els requeriments del sistema de caracterització depenen de l'aplicació. En aquesta tesi, es proposen dos sistemes de caracterització per a dos àmbits d'aplicació que comprenen la majoria de les aplicacions amb sensors QCM: 1) Caracterització de materials sota condicions d'amortiment variable i 2) detecció de substàncies amb alta resolució de mesura. Els sistemes proposats tracten de resoldre la problemàtica detectada en els ja existents. Per a aplicacions en les quals l'amortiment del sensor varia durant l'experiment, es proposa un sistema basat en una nova configuració de la tècnica de compensació automàtica de capacitat (ACC). La nova configuració proporciona la mesura de la freqüència de ressonància sèrie, la resistència dinàmica i la capacitat paral¿lel del sensor. A més, permet un calibratge fàcil del sistema que millora la precisió de la mesura. Es presenten els resultats experimentals per a cristalls de 9 i 10 MHz en mitjans fluids, amb diferents capacitats en paral¿lel, demostrant l'efectivitat de la compensació de capacitat. El sistema presenta alguna desviació en freqüència respecte a la freqüència ressonància sèrie, mesurada amb un analitzador d'impedàncies. Aquestes desviacions són explicades convenientment, degudes al comportament no ideal específic d'alguns components del circuit. Una nova proposta de circuit es presenta com a possible solució a aquest problema. Per a aplicacions d'alta resolució es proposa una plataforma integrada per a caracteritzar sensors acústics d'alta freqüència. El sistema proposat es basa en un nou concepte en el qual el sensor és interrogat mitjançant una font externa molt estable i de molt baix soroll, a una freqüència constant mentre es monitoritzen els canvis produïts per la càrrega en la fase del sensor. L'ús de sensors d'alta freqüència augmenta la sensibilitat de la mesura, per altra banda, el sistema de caracterització dissenyat redueix el soroll en la mateixa. El resultat és una millora en el límit de detecció (LOD). S'aconsegueix amb això un dels reptes pendents en els dispositius acústics d'alta freqüència. La validació de la plataforma desenvolupada es realitza amb una aplicació d'un immunosensor basat en cristalls QCM d'alta freqüència fonamental (HFF-QCM) per a la detecció de dos pesticides: carbaryl i tiabendazol. Els resultats obtinguts per al carbaryl es comparen amb els obtinguts amb altra tecnologia acústica d'alta freqüència basada en sensors Love, amb la tècnica òptica basada en ressonància superficial de plasmons (SPR) i amb la tècnica de referència Enzyme Linked Immuno Assay (ELISA). El LOD obtingut amb els sensors acústics HFF-QCM i Love és similar al obtingut amb les tècniques ELISA i millora en un ordre de magnitud el obtingut amb SPR. La senzillesa conceptual del sistema proposat junt amb el seu baix cost, així com la capacitat de miniaturització del ressonador de quars fa possible la caracterització de múltiples sensors integrats en una configuració en array, el que permetrà en un futur assolir el repte de la detecció multianalit per a aplicacions High-Throughput Screening (HTS).
García Narbón, JV. (2016). Improved characterization systems for quartz crystal microbalance sensors: parallel capacitance compensation for variable damping conditions and integrated platform for high frequency sensors in high resolution applications [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/63249
TESIS

Le développement de matériaux avec différents ordres ferroïques couplés (multiferroïques) motive d’intenses activités de recherche. Une combinaison particulièrement intéressante est celle des paramètres d'ordre magnétique et électrique qui, dans le cas favorable où ceux-ci sont couplés, ouvre la voie au contrôle électrique de l’aimantation. Celui-ci peut être envisagé via la manipulation de la polarisation d’un ferroélectrique ou des déformations d’un piézoélectrique Les propriétés du matériau ferroélectrique/piézoélectrique peuvent être inversement modifiées par l’état d’aimantation, ce qui laisse envisager des applications dans le domaine des capteurs de champs magnétiques. Ce travail s’inscrit dans l’étude de systèmes piézoélectrique/ magnétostrictif, avec un intérêt spécifique porté à l’influence de l’aimantation sur les ondes acoustiques de surface (SAW) générées dans le dispositif. Nous avons ainsi déposé des couches polycristallines de Ni, des multicouches [Co/IrMn], ainsi que des couches épitaxiées de TbFe2 sur des substrats de Niobate de Lithium (LNO) de différentes orientations. Sur LNO Z-cut, la croissance de TbFe2 est réalisée en utilisant différentes couches tampons simples ou doubles qui permettent d’obtenir des directions de croissance [111] ou [110] avec des anisotropies magnétiques respectivement perpendiculaire et planaire. Sur des substrats de coupe 128Y et 41Y, la croissance s’avère beaucoup plus complexe mais il est néanmoins possible d’obtenir un film cristallisé de TbFe2 multidomaines avec des relations d’orientation 3D similaires à celles obtenus sur LNO Z-cut, que ce soit entre la couche magnétique et la couche tampon, ou entre la couche tampon et le substrat. Des dispositifs magnétiques à ondes acoustiques de surface (MSAW) ont été ensuite fabriqués dans une géométrie de résonateur permettant une interrogation à distance aisée. La fréquence de résonance des dispositifs MSAW est sensible à l’application d’un champ magnétique externe, via des effets statiques liés à l’orientation de l’aimantation sous champ et via des effets dynamiques d’origine magnétoélastique liés à l’excitation acoustique. Nous avons examiné les réponses magnéto-acoustiques des différents dispositifs, en corrélation étroite avec les propriétés magnétiques statiques, en particulier l’anisotropie, la coercivité et l’hystérèse. Un modèle piézomagnétique équivalent a été utilisé pour simuler certaines de ces réponses. De manière générale, nous montrons qu’un choix judicieux du matériau magnétique et le contrôle de ses propriétés permettent d’élaborer des capteurs spécifiques : un matériau magnétique doux permet de contrôler l’anisotropie de la réponse acoustique via la forme des IDT; un matériau magnétique dur ouvre la voie au développement de capteurs de forts champs magnétiques; un système à anisotropie d’échange dont on peut contrôler la réversibilité de la réponse magnétique permet d’envisager un capteur de champ magnétique hors plan
The development of materials with different coupled ferroic orders (multiferroics) drives an intense research activity. A particularly interesting combination is the case where magnetic and electrical orders are simultaneously present, which, in the favorable case where these are coupled, opens the way to the electrical control of magnetization. This can be achieved in manipulating the polarization in a ferroelectric or the strains in a piezoelectric compound. Ferroelectric or piezoelectric properties can inversely be influenced by the magnetic state, an interesting feature for the development of magnetic field sensors. This work aims in the investigation of piezoelectric/magnetostrictive systems, more especially in the role of the magnetization and of the magnetization versus field behavior on the surface acoustic waves (SAW). Polycristalline Ni films, [Co/IrMn] multilayers and epitaxial TbFe2 films have been deposited on Lithium Niobate (LNO) substrates of different orientations. On LNO Z-cut, various single or double buffer layers have been used to achieve the TbFe2 epitaxial growth, along either [111] or [110] directions and with either perpendicular or in-plane magnetic anisotropy. On LNO 128Y and 41Y substrates, the growth is more complex but it is nevertheless possible to obtain crystalline multidomains TbFe2 films with 3D orientation relationships similar to those obtained on LNO Z-cut, both between the magnetic and the buffer layers, and between the buffer layer and the substrate. Magnetic surface acoustic wave (MSAW) devices have been patterned in a resonator geometry that enables an easy wireless interrogation. The MSAW device resonance frequency is sensitive to an external magnetic field, both via static effects related to the field-induced magnetization changes, and via magnetoelastic dynamic effects related to the acoustic excitation. We have investigated the MSAW magneto acoustic responses of the various devices in close connection with the static magnetic properties, especially the anisotropy, the coercivity and the hysteresis. An equivalent piezomagnetic model could support some of these observations. We show more generally that the proper choice of magnetic material and the control of the magnetic properties helps to build up specific sensors: soft magnetic materials enable to tailor the anisotropy of the MSAW response by engineering the IDT’s shape; hard magnetic materials enable to achieve high field unipolar or bipolar field response; exchange-biased systems in which the reversibility of the magnetic response is achieved let envision the development of sensors for out-of-plane magnetic fields

Higher frequencies in the MHz and GHz range and the increasing miniaturization lead to a higher load of the SAW (surface acoustic wave) metallizations. This higher SAW load and the intrinsic stresses result in a stress induced material transport, called acoustomigration. These microstructural changes can destroy the characteristic of the SAW device. Different Al based material combinations were investigated by different authors to improve the reliability of the metallizations and to delay the cost-intensive change to Cu based metallizations. The Cu based metallizations with TaSiN diffusion barriers were also investigated in this work. The barrier layers are necessary to impede the oxygen diffusion into the Cu layer and the Cu diffusion into the piezoelectric substrate. Also in this work the analytical TEM were used as a tool to investigate these microstructural changes in the SAW electrodes. Chemical changes in the metallizations were analysed by EDXS and EELS. The locally high resolved stress measurement in metallizations is a challenge for the future. The CBED (convergent beam electron diffraction) technique has shown the best resolution, however, it can only be applied to TEM lamellas. The aim of this work was to measure the stress within the SAW metallizations by using the CBED method. With it, we could correlate the microstructural changes with the causing stresses within the metallizations. To qualify the CBED method the thermal expansion of Al and Cu single crystals was measured by using a new model for thin TEM lamallas.