Sensors is one of the major areas of current research. Thin film micro/nano sensors are gaining attention worldwide, as there is necessity of miniaturization. There are varieties of sensors available by utilizing different materials in bulk and thin film form for measuring parameters like temperature, pressure, flow, humidity etc. Apart from these, there are various sensors available to measure impact force. Impact sensor offers potential application possibilities in robotics, aerospace, structural & mechanical engineering and related areas. Many physical principles have been explored for the realization of impact sensor. The present thesis reports the efforts made in developing impact sensor using piezoelectric thin film. The necessary brief background information on impact sensors is presented in Chapter 1. This includes the description of available literature on impact sensors and their probable applications. In Chapter 2, a review of the various techniques such as thin film deposition techniques, film thickness measurement techniques, thin film characterization techniques, used in our work are explained in detail. Chapter 3 explains the direct and indirect methods of characterization used for confirming the piezoelectric property of zinc oxide thin films. The detailed experimental work carried out in realizing the impact sensor using piezoelectric thin films is presented in chapter 4. This includes design of the sensor, calibration setup used & the procedure followed and results obtained. Finally, we present the summary of the work carried out in the thesis, conclusions arrived at and the scope for carrying out further work in the direction of making the sensor more efficient.

Cette thèse s’inscrit dans le cadre d’une cotutelle internationale entre l’Université de Bourgogne Franche-Comté en France et l’Université de Sherbrooke au Canada. Elle porte sur le développement d'un biocapteur miniature pour la détection et la quantification de bactéries dans des milieux liquides complexes. La bactérie visée est l’Escherichia coli (E. coli), régulièrement mise en cause dans des épidémies d'infections alimentaires, et parfois meurtrière.La géométrie du biocapteur consiste en une membrane en arséniure de gallium (GaAs) sur laquelle est déposé un film mince piézoélectrique d’oxyde de zinc (ZnO). L'apport du ZnO structuré en couche mince constitue un réel atout pour atteindre de meilleures performances du transducteur piézoélectrique et consécutivement une meilleure sensibilité de détection. Une paire d'électrodes déposée sur le film de ZnO permet de générer sous une tension sinusoïdale une onde acoustique se propageant dans le GaAs, à une fréquence donnée. La face arrière de la membrane, quant à elle, est fonctionnalisée avec une monocouche auto-assemblée (SAM) d'alkanethiols et des anticorps anti-E. coli, conférant la spécificité de la détection. Ainsi, le biocapteur bénéficie à la fois des technologies de microfabrication et de bio-fonctionnalisation du GaAs, déjà validées au sein de l’équipe de recherche, et des propriétés piézoélectriques prometteuses du ZnO, afin d’atteindre potentiellement une détection hautement sensible et spécifique de la bactérie d’intérêt. Le défi consiste à pouvoir détecter et quantifier cette bactérie à de très faibles concentrations dans un échantillon liquide et/ou biologique complexe.Les travaux de recherche ont en partie porté sur les dépôts et caractérisations de couches minces piézoélectriques de ZnO sur des substrats de GaAs. L’effet de l’orientation cristalline du GaAs ainsi que l’utilisation d’une couche intermédiaire de Platine entre le ZnO et le GaAs ont été étudiés par différentes techniques de caractérisation structurale (diffraction des rayons X, spectroscopie Raman, spectrométrie de masse à ionisation secondaire), topographique (microscopie à force atomique), optique (ellipsométrie) et électrique. Après la réalisation des contacts électriques, la membrane en GaAs a été usinée par gravure humide. Une fois fabriqué, le transducteur a été testé en air et en milieu liquide par des mesures électriques, afin de déterminer les fréquences de résonance pour les modes de cisaillement d’épaisseur. Un protocole de bio-fonctionnalisation de surface, validé au sein du laboratoire, a été appliqué à la face arrière du biocapteur pour l’ancrage des SAMs et des anticorps, tout en protégeant la face avant. De plus, les conditions de greffage d’anticorps en termes de concentration utilisée, pH et durée d’incubation, ont été étudiées, afin d’optimiser la capture de bactérie. Par ailleurs, l’impact du pH et de la conductivité de l’échantillon à tester sur la réponse du biocapteur a été déterminé. Les performances du biocapteur ont été évaluées par des tests de détection de la bactérie cible, E. coli, tout en corrélant les mesures électriques avec celles de fluorescence. Des tests de détection ont été réalisés en variant la concentration d’E. coli dans des milieux de complexité croissante. Différents types de contrôles ont été réalisés pour valider les critères de spécificité. En raison de sa petite taille, de son faible coût de fabrication et de sa réponse rapide, le biocapteur proposé pourrait être potentiellement utilisé dans les laboratoires de diagnostic clinique pour la détection d’E. coli. / This thesis was conducted in the frame of an international collaboration between Université de Bourgogne Franche-Comté in France and Université de Sherbrooke in Canada. It addresses the development of a miniaturized biosensor for the detection and quantification of bacteria in complex liquid media. The targeted bacteria is Escherichia coli (E. coli), regularly implicated in outbreaks of foodborne infections, and sometimes fatal.The adopted geometry of the biosensor consists of a gallium arsenide (GaAs) membrane with a thin layer of piezoelectric zinc oxide (ZnO) on its front side. The contribution of ZnO structured in a thin film is a real asset to achieve better performances of the piezoelectric transducer and consecutively a better sensitivity of detection. A pair of electrodes deposited on the ZnO film allows the generation of an acoustic wave propagating in GaAs under a sinusoidal voltage, at a given frequency. The backside of the membrane is functionalized with a self-assembled monolayer (SAM) of alkanethiols and antibodies anti-E. coli, providing the specificity of detection. Thus, the biosensor benefits from the microfabrication and bio-functionalization technologies of GaAs, validated within the research team, and the promising piezoelectric properties of ZnO, to potentially achieve a highly sensitive and specific detection of the bacteria of interest. The challenge is to be able to detect and quantify these bacteria at very low concentrations in a complex liquid and/or biological sample.The research work partly focused on the deposition and characterization of piezoelectric ZnO thin films on GaAs substrates. The effect of the crystalline orientation of GaAs and the use of a titanium / platinum buffer layer between ZnO and GaAs were studied using different structural (X-ray diffraction, Raman spectroscopy, secondary ionization mass spectrometry), topographic (atomic force microscopy), optical (ellipsometry) and electrical characterizations. After the realization of the electrical contacts on top of the ZnO film, the GaAs membrane was micromachined using chemical wet etching. Once fabricated, the transducer was tested in air and liquid medium by electrical measurements, in order to determine the resonance frequencies for thickness shear mode. A protocol for surface bio-functionalization, validated in the laboratory, was applied to the back of the biosensor for anchoring SAMs and antibodies, while protecting the top side. Furthermore, different conditions of antibody grafting such as the concentration, pH and incubation time, were tested to optimize the immunocapture of bacteria. In addition, the impact of the pH and the conductivity of the solution to be tested on the response of the biosensor has been determined. The performances of the biosensor were evaluated by detection tests of the targeted bacteria, E. coli, while correlating electrical measurements with fluorescence microscopy. Detection tests were completed by varying the concentration of E. coli in environments of increasing complexity. Various types of controls were performed to validate the specificity criteria. Thanks to its small size, low cost of fabrication and rapid response, the proposed biosensor has the potential of being applied in clinical diagnostic laboratories for the detection of E. coli.

Man’s desire to replicate/mimic the nature’s creation provided an impetus and inspiration to the rapid advancements and progress made in the sensors and actuators technology. A normal human being has five basic sensory organs, which helps and guides him in performing the routine tasks. This underlines the importance of basic sensory organs in a human life. In a similar fashion, sensors and actuators are of paramount importance for most of the science and engineering applications. The aim of the present thesis work is to explore the application of piezoelectric ZnO thin films deposited on a flexible substrate for the development of sensors and actuators. Detailed study was performed on the suitability of three different flexible substrates namely Phynox, Kapton and Mylar. However, Phynox alloy substrate was found to be a suitable substrate material for the above mentioned applications. Sputtering technique was chosen for the deposition of ZnO thin films on to Phynox substrate. The necessary process parameters were optimized to achieve good quality piezoelectric thin films. In the present work, sensors have been developed by utilizing the direct piezoelectric effect of ZnO thin films deposited on Phynox alloy substrate. These includes a flow sensor for gas flow rate measurement, impact sensor for non-destructive material discrimination study and a Thin Film Sensor Array (TFSA) for monitoring the impact events. On the other hand, using the converse piezoelectric effect of ZnO thin films, actuators have also been developed. These include a thin film micro actuator and a Thin Film Micro Vibrator (TFMV) for vibration testing of micro devices. The thesis is divided into following seven chapters. Chapter 1: This chapter gives a general introduction about sensors and actuators, piezoelectric thin films, flexible substrates, thin film deposition processes and characterization techniques. A brief literature survey of different applications of piezoelectric thin films deposited on various flexible substrates in device development is presented. Chapter 2: A novel flexible metal alloy (Phynox) and its properties along with its applications are discussed in this chapter. ZnO thin films were deposited on Phynox substrate by Rf reactive magnetron sputtering technique. The sputtering process parameters such as: Ar:O2 gas ratio, substrate temperature and RF power were optimized for the deposition of good quality piezoelectric ZnO thin films. The deposited ZnO thin films were characterized using XRD, SEM, AFM and d31 coefficient measurement techniques. Chapter 3: It reports on the comparative study of properties of piezoelectric ZnO thin films deposited on three different types of flexible substrates. The substrate materials employed were a metal alloy (Phynox), polyimide (Kapton), and polyester (Mylar). Piezoelectric ZnO thin films deposited on these flexible substrates were characterized by XRD, SEM, AFM and d31 coefficient measurement techniques. A vibration sensing test was also performed for the confirmation of good piezoelectric property. Compared to the polymer flexible substrates, the metal alloy flexible substrate (Phynox) was found to be more suitable for integrating ZnO thin film for sensing applications. Chapter 4: The development of a novel gas flow sensor for the flow rate measurement in the range of L min-1 is presented in this chapter. The sensing element is a Phynox alloy cantilever integrated with piezoelectric ZnO thin film. A detailed theoretical analysis of the experimental set–up showing the relationship between output voltage generated and force at a particular flow rate has been discussed. The flow sensor is calibrated using an in-house developed testing set-up. Chapter 5: This chapter is divided into two sections. Section 5.1 reports on the development of a novel packaged piezoelectric thin film impact sensor and its application in non-destructive material discrimination studies. Different materials (Iron, Glass, Wood and Plastic) were successfully discriminated by using the developed impact sensor. The output response of impact sensor showed good linearity and repeatability. The impact sensor is sensitive, reliable and cost-effective. Section 5.2 reports on the development of a Thin Film Senor Array (TFSA) for monitoring the location and magnitude of the impact force. The fabricated TFSA consists of evenly distributed ZnO thin film sensor array. Chapter 6: It consists of two sections. Section 6.1 reports on the fabrication of micro actuator using piezoelectric ZnO thin film integrated with flexible Phynox substrate. A suitable concave Perspex mounting was designed for the actuator element. The actuator element was excited at different frequencies for the supply voltages of 2V, 5V and 8V. The developed micro actuator has the potential to be used as a micro pump for pumping nano liters to micro liters of fluids. Section 6.2 reports the design and development of a portable ready to use Thin Film Micro Vibrator (TFMV). The TFMV is capable of providing the vibration amplitude in the range of nanometer to micrometer. A thin silicon diaphragm was used as a test specimen for its vibration testing studies using the developed TFMV. The TFMV is light-weight and have internal battery, hence no external power supply is required for its functioning. Chapter 7: The first section summarizes the salient features of the work presented in this thesis. In the second section the scope for carrying out the further work is given.