Le besoin d'analyse de gaz à l'état de traces s'est accentué ces dernières années en raison des préoccupations du public et de l'industrie sur des questions telles que le contrôle des émissions de polluants atmosphériques, la surveillance de l'environnement au sens large, la santé et la sécurité au travail. Il est donc nécessaire de posséder des instruments de détection sélectifs, sensibles et capables d'effectuer une mesure directe en temps réel. La fiabilité des systèmes de mesure est également un critère important et, selon l'application envisagée, s'ajoute aussi le besoin de miniaturisation pour aller vers des microsystèmes permettant le développement de dispositifs portables pour des opérations sur site.Le travail de thèse présenté dans ce manuscrit est situé dans ce contexte et porte sur l'étude et la mise au point d'un système sensible, efficace et assez simple à mettre en œuvre permettant de réaliser des mesures de traces de gaz sélectives, en temps réel et in-situ. Ce système est basé sur la spectroscopie d'absorption par quartz (QEPAS, Quartz Enhanced PhotoAcoustic Spectrocopy) qui consiste en la mesure d'une onde acoustique générée après la relaxation non-radiative des molécules excitées par l'absorption de la lumière modulée émise par des diodes lasers accordables, à l'aide d'un diapason à quartz (QTF). Le fonctionnement des sources lasers accordables et du QTF ainsi que différentes configurations du spectrophone (association du micro-résonateur et du QTF) utilisés dans cette technique QEPAS sont détaillés. Une modélisation de l'onde acoustique et de la réponse du capteur est également proposée. Deux dispositifs ont été réalisés. Le premier, nommé banc QEPAS prototype, est dédié à la mesure de l'éthylène avec une diode laser DFB émettant à 3,32 µm. Le second dispositif est une nouvelle version de capteur QEPAS, plus compacte que des dispositifs existant actuellement, dans laquelle il est possible de placer tout type de diode laser commerciale montée dans des supports de type T0xx. Ce banc compact est utilisé pour la mesure de méthane avec notamment une diode laser DFB émettant à 3,26 µm. / The need for trace gas analysis has increased in recent years due to an important concern of the public and industry on issues such as the control of emissions of air pollutants, environmental monitoring, health and security. It is therefore necessary to have the trace gas sensors able of high selectivity, sensitivity and a direct measurement in real time. The reliability of the measurement systems is also an important criterion, depending on the intended application, the need to move towards miniaturization of microsystems for the development of portable devices for on-site operations is also interesting.This thesis is in this context and focuses on the study and development of a sensitive, efficient and simple setup to make selective, in-situ and in real time measurements of trace gases. This system is based on quartz enhanced photoacoustic spectrocopy (QEPAS) which consists on the measurement of an acoustic wave generated by the non-radiative relaxation of the excited molecules after light absorption, with a quartz tuning fork (QTF). The operation of tunable laser sources, of QTF and different spectrophone configurations (combination of the micro-resonator and QTF) used in QEPAS technique are detailed. A model of the acoustic wave and the response of the sensor are also proposed. Two devices have been designed. The first one is a QEPAS prototype bench, dedicated to the measurement of ethylene with a DFB laser diode emitting at 3.32 µm. The second device is a new version of QEPAS sensor that is more compact than the currently existing devices and where it is possible to place any type of commercial laser diode. This compact bench is used for methane measurement with a DFB laser diode emitting at 3.26 µm.

This diploma thesis deals with the feasibility of using PVDF nanofibers as an active sensor layer generating electrical signal. PVDF and related electromechanical effects are described. A research study is conducted regarding existing PVDF nanofiber applications and based on it, an event sensor design utilizing triboelectric effect and electrostatic induction is proposed. The electrical response of the layers is experimentally investigated and a pulse detection algorithm is conceived and implemented. Finally, a way of integrating the sensor into a rail track is proposed.

Presented thesis analyses a function of the particular type of the nanopositioner with aim to suggest and construct an electronic device suitable for control of the nanopositioner slider. In presented material there is a description of the control signals and possibility of their generating in the respect of slider movement accuracy. The main goal of the thesis is to describe electronic units ranging from power supply, control processor unit part to end part that directly joint nanopositioner. There is also programme equipment for microcontroller and computer, communication description, movement measuring and calibration and draft for the close-up of the control loop for additional increase of the movement accuracy.

The submitted thesis describes characteristics and use of the ferroelectric material which has their utilization in electronics and electro technical industry. The thesis describes behaviour ferroelectrics in temperature range. A suitable workplace was designed and its functionality was verified in selected ferroelectrics samples dependence of temperature of components of complex permittivity.

This master's thesis deals with the development and verification of the model of the piezoelectric generator, incl. determination of its parameters. This mathematical model should be used as a tool for development of new devices, especially for analysis of applicability of available energy source (vibration) and for design of device itself. At first the review of energy harvesting is described deeply. Subsequently piezoelectric generators and the ways how we can model them, are depicted in details. The methodology of parameters estimation and model development is presented in state space or in MATLAB/Simulink environment and applied on the commercial generator Midé V21BL. A device has been made within the scope of the thesis, which can be used as an universal tool in experiments with generator. Finally the model is applied on the analysis of energy yield from man's walk and there is also brief introduction to model modifications.

The project is about piezoelectric energy harvesters and piezoelectric bio-organic materials.Nowadays, various kinds of energy harvesters based on micro or nano materials are appliedinmanyelectronic applications, such as wearable devices and electricity generators. Amongthem, thepiezoelectric effect-based energy harvesters are more attractive in research and industryfields. Inrecent years, piezoelectric biomaterials become a popular option because they are availabletocouple electrical and mechanical energy in a biological, ecofriendly systemto generate electricityinreal time. Among them, γ- glycine crystals have been recently synthesized in wafer scale throughasimple polyvinyl alcohol (PVA)-assisted evaporation process exhibiting good piezoelectricperformance. However, so far there are no metal-free energy-harvesting devices basedonPVA-glycine film to enable green manufacturing. In this project, we proposed the direct inkwritingorganic PEDOT:PSS electrodes and PVA-glycine-PVA piezoelectric crystals to fabricate metal-freeenergy harvesters. The output voltage reaches 1.5 V at a load resistance of 500 MΩandunderaforce of 10 N. The performance is comparable to other glycine-based devices in recent literature.Our scalable, sustainable and low-cost printing process is expected to greatly contribute tothefieldof biomaterials-based piezoelectric energy harvesting. / Projektet handlar om piezoelektriska energiskördare och piezoelektriska bioorganiska material. Nuförtiden används olika typer av energiskördare baserade på mikro- eller nanomaterial i mångaelektroniska applikationer, såsom bärbara enheter och elgeneratorer. Bland dem är de piezoelektriskaeffektbaserade energiskördarna mer attraktiva inom forsknings- och industriområden. På senare år harpiezoelektriska biomaterial blivit ett populärt alternativ eftersom de är tillgängliga för att koppla elektrisk och mekanisk energi i ett biologiskt, miljövänligt system för att generera elektricitet i realtid. Bland dem har γ-glycinkristaller nyligen syntetiserats i waferskala genom en enkel polyvinylalkohol (PVA)-assisterad förångningsprocess som uppvisar god piezoelektrisk prestanda. Än så länge finnsdet dock inga metallfria energiskördande enheter baserade på PVA-glycinfilm för att möjliggöra gröntillverkning. I detta projekt föreslog vi direkt bläckskrivande organiska PEDOT:PSS-elektroder ochPVA-glycin-PVA piezoelektriska kristaller för att tillverka metallfria energiskördare. Utspänningennår1,5 V vid en belastningsresistans på 500 MΩ och under en kraft på 10 N. Prestandan är jämförbar medandra glycinbaserade enheter i nyare litteratur. Vår skalbara, hållbara och billiga utskriftsprocess förväntas i hög grad bidra till området för biomaterialbaserad piezoelektrisk energiskörd.

Polymer and composite polymer-ceramic nanofibers were prepared by electrospinning process. Solution of 20 wt.% polyvinylidene fluoride (PVDF) in a mixture of dimethyl sulfoxide (DMSO) and acetone in the ratio of 7:3 was chosen as the most suitable precursor. When preparing composite nanofibers, 20 wt.% of barium calcium zirconate titanate (BCZT) or barium titanate (BT) nanoparticles was added to this PVDF solution. Given parameters were defined as the most suitable for the process of electrospinning: voltage of 50 kV, feeding rate of 30 l/min, distance between emitter and collector of 20 cm and needle diameter of 17 G. The effect of polymer molecular weight and the rotation speed of collector was also studied. Various properties of prepared samples were studied: morphology and fiber diameter, phase composition with the use of x-ray diffraction and Fourier transform infrared spectroscopy and also chosen electrical properties. Lower fiber diameters appeared with lower polymer molecular weight and higher rotation speed of the collector. These parameters resulted in higher percentage of the piezoelectric phase as well. The smallest achieved fiber diameter was around 300 nm, the highest percentage of phase was 92 % and the highest piezoelectric constant had a value of 16 pC/N. Composite fibers filled with BT particles showed better properties that the ones filled with BCZT particles.

The content of this thesis is about preparation and processing of lead-free piezoceramic materials with perovskite structure. Potassium sodium niobate (KNN) powder was prepared by solid state reaction (SSR) and liquid phase reaction (sol-gel reaction). The powders were formed by uniaxial and isostatic pressing and further sintered. The density, grain size and morphology were determined on the sintered samples. The powder, synthesised by SSR and sintered in a conventional furnace, was chosen as a standard. The maximum density achieved on samples after optimization of sintering cycle was 93 %TD. The sintering optimization involved a homogenization step at 950 °C, which promotes the correct development of the phase composition and microstructure, followed by sintering at 1120 °C. The same approach and sintering cycle were used for sintering the samples, prepared by sol-gel synthesis. The maximum density of the samples prepared by sol-gel reaction and sintered in a conventional way, was 92 %TD. For further comparison, both of the synthesised powders were sintered using SPS (spark plasma sintering), which increased their final density up to 97 %TD. The approximate value of the piezoelectric coefficient d33 (pC/N) has been measured on selected SSR samples with pure phase composition ((K0,5Na0,5)NbO3). The best measured value of d33 was around 100 pC/N.

The doctoral thesis discusses the measurement of parameters of piezoelectric (PZT) materials and the influence of temperature on their stability. In the introductory sections, the author briefly explains the piezoelectric effect and its use; simultaneously, methods for the preparation of piezoelectric materials and the measurement of their properties are presented to illustrate the analyzed problem. The experimental part of the thesis describes the procedure of measuring and calculating the complete matrix of material coefficients from samples of PZT ceramics. The applied set of piezoelectric samples complying with relevant European and world standards was made in the form of thin plates, thin discs and cylinders, via gradual modification of the large disc. The NCE51 and/or the older PCM51 ceramics obtained from the company Noliac Ceramics were used in determining the complete matrix and describing the measurement method. Both these types are soft piezoceramics composed from a solid solution of lead zirconate and lead titanate with the general chemical formula of Pb(Zr1-x,Tix)O3. The real crystallographic structure and chemical composition of the samples were confirmed by X-ray diffraction spectroscopy and energy dispersive spectroscopy (EDS), respectively. The frequency method was used for the measurement and calculation of all material coefficients. An Agilent 4294A impedance analyzer and a set of measuring tweezers marketed as “Tweezers Contact Test Fixture 16334A” were used in the process. Fast determination of the entire matrix of coefficients without any special requirement for the preparation of the samples to be measured was tested and verified. The charge coefficients of the piezoelectric material were confirmed by direct methods including the laser interferometer technique, the vibrometric method, and the procedure utilizing changes of the force applied to the sample. The advantages and disadvantages of the methods were compared and defined based on measurements and their results. The main part of thesis was focused on the behavior of piezoelectric material at high temperatures near the Curie point. Depolarization performed by means of a high temperature approaching the Curie point constitutes a significant yet hardly measurable material property of PZT ceramics. Commonly available vibrometric methods (d33-meters) do not appear to be suitable for the measurement of temperature dependencies, and for that reason the frequency technique was used. The piezoelectric charge coefficient, whose value can be effectively measured via the above-discussed frequency method, was selected as the indicator showing the depolarization state in the applied piezoelectric ceramics. The accuracy of the procedure was verified via comparison of the vibrometric method in cylinders of the NCE51 ceramics with different sizes, which are designed for the longitudinal length mode. The result is an optimized measurement methodology which facilitates accurate determination of the Curie temperature, namely phase transition to the cubic crystallographic structure. The experiment also proved the applicability of progressive, controlled depolarization of PZT ceramics via high temperature, and it also enabled us to define the temperature limits at which there occur irreversible changes of the piezoelectric properties of piezoceramics. In the measured NCE51 and PCM51 materials, the limit for the irreversible changes was equal to 95% of the Curie temperature.

The main challenge in the design of vibration energy harvesters is the optimization of energy outcome relative to the applied excitation to reach a higher efficiency in spite of the weakness of ambient energy sources. One promising principle of vibration converters is magnetoelectricity due to the outstanding properties of magnetostrictive and piezoelectric laminate composites, which provide interesting possibilities to harvest energy from low amplitude and low frequency vibration with relatively high energy outcome. For these devices, ensuring high deformations in the magnetostricive layers, improvement of the magnto-mechanical and the electro-mechanical couplings are highly required for the optimization of the energy outcome. This thesis primarily aims to develop a model based harvester design for magnetoelectric (ME) converters. Based on a comprehensive understanding of the complex energy flow in magnetoelectric transducers, several design parameters are investigated. For instance, magnetostriction in a Terfenol-D plate is investigated by means of atomic force microscopy under similar conditions as within magnetoelectric transducers. A novel measurement approach was successfully developed to detect the evolution of magnetic domains and measure deformations in a Terfenol-D plate in response to externally non-uniform applied magnetic fields. Furthermore, a finite element model is developed to predict the induced voltage in the ME transducer as a response to the magnet’s displacement, corrected based on atomic force microscopy measurements, and used for the design of the harvester. The presented three- dimensional model takes into consideration the nonlinear behaviour of the magnetostrictive and piezoelectric materials. Additionally, three novel converters having different magnetic circuits are designed and analysed analytically based on Lindstedt-Poincaré method. The effects of the structure parameters, such as the nonlinear magnetic forces, the magnetic field distribution and the resonance frequency are discussed, and the electric output performances of the three designed converters are evaluated. In order to improve both mechanical and electrical coupling between the piezoelectric and the magnetostrictive layers, a bonding technique at room temperature is proposed which uses conductive polymer nanocomposites. Two magnetoelectric transducers are fabricated based on this technique having 1 wt.% and 2 wt.% concentration of multiwalled carbon nanotubes in epoxy resin. Another magnetoelectric transducer is fabricated by a classical technique for comparison purposes. In order to validate the design, a series of demonstrators are designed and fabricated according to the simulation and optimization results. The proposed design is composed by a cantilever beam, a magnetic circuit with several magnet arrangements and a magnetoelectric transducer, which is formed by a piezoelectric PMNT plate bonded to two magnetostrictive Terfenol-D layers. In this design, external vibrations are converted to magnetic field changes acting on the magnetostrictive layers leading to deformations, which are transmitted directly to the piezoelectric layer. The converters are tested under harmonic excitations and real vibration profiles reproduced by an artificial vibration source. Different parameters were investigated experimentally including the magnetic forces between the transducer and the magnetic circuit and the used bonding technique. Tuning the resonance frequency of the ME converter is also addressed using a simple screw/nut system, which allows to control the relative position and therefore the magnetic forces between the magnetic circuit and the transducer. The magnetoelectric transducer bonded with 2 wt.% concentration of multiwalled carbon nanotubes shows better output performances than the two other ME transducers under similar excitations. A maximum power output of 2.42 mW is reached under 1 mm applied vibration at 40 Hz. This performance presents an improvement of minimum 20 % of the reached energy outcome by other magnetoelectric vibration converters using single ME transducer at comparable applied excitations. / Die größte Herausforderung bei der Konstruktion von Vibrations-Energiewandlern ist die Optimierung der gewonnenen Energie im Verhältnis zur angewandten Anregung, um trotz schwacher Umgebungsenergiequellen einen hohen Wirkungsgrad zu erreichen. Ein vielversprechendes Prinzip von Vibrationswandlern ist die Magnetoelektrizität aufgrund der hervorragenden Eigenschaften von magnetostriktiven und piezoelektrischen Verbundwerkstoffen, die interessante Möglichkeiten bieten, Energie aus niederfrequenten Schwingungen mit kleinen Amplituden zu gewinnen. Bei diesen Wandlern ist die Sicherstellung hoher Verformungen in den magnetostriktiven Schichten, die Verbesserung der magnetisch-mechanischen und der elektromechanischen Kopplungen für die Optimierung des Energieertrages sehr wichtig. Diese Arbeit zielt in erster Linie auf die Entwicklung eines modellbasierten Entwurfs für magnetoelektrische (ME) Wandler ab. Basierend auf einem umfassenden Verständnis des komplexen Energieflusses in magnetoelektrischen Wandlern werden mehrere Entwurfsparameter untersucht. So wird beispielsweise die Magnetostriktion in einer Terfenol-D-Platte mittels Rasterkraftmikroskopie unter ähnlichen Bedingungen untersucht wie in magnetoelektrischen Wandlern. Dabei wurde eine neuartige Messmethode erfolgreich entwickelt, um die Entwicklung von magnetischen Domänen zu erfassen und die Deformation in einer Terfenol-D-Platte als Reaktion auf extern ungleichmäßig angelegte Magnetfelder zu messen. Darüber hinaus wird ein Finite-Elemente-Modell entwickelt, um die induzierte Spannung im ME-Wandler als Reaktion auf die Verschiebung des Magneten vorherzusagen, welches auf der Grundlage von Atomkraftmikroskopie Messungen korrigiert und für den Entwurf des Energiewandlers verwendet wird. Das vorgestellte dreidimensionale Modell berücksichtigt das nichtlineare Verhalten der magnetostriktiven und piezoelektrischen Materialien. Zusätzlich werden drei neuartige Wandler mit unterschiedlichen Magnetkreisen nach dem Lindstedt-Poincaré Verfahren konzipiert und analytisch analysiert. Die Auswirkungen der Strukturparameter, wie die nichtlinearen Magnetkräfte, die Magnetfeldverteilung und die Resonanzfrequenz, werden diskutiert und die elektrischen Ausgangsleistungen der drei ausgelegten Wandler ausgewertet. Um die mechanische und elektrische Kopplung zwischen der piezoelektrischen und der magnetostriktiven Schicht zu verbessern, wird eine bei Raumtemperatur prozessierbare Verbindungstechnik vorgeschlagen, bei der leitfähige Nanokomposite verwendet werden. Zwei magnetoelektrische Wandler werden basierend auf dieser Technik mit einer Konzentration von 1 wt.% und 2 wt.% an mehrwandigen Kohlenstoff-Nanoröhren in Epoxidharz hergestellt. Ein weiterer magnetoelektrischer Wandler wurde zu Vergleichszwecken mit einer klassischen Technik hergestellt. Für die Validierung des Entwurfes wird eine Reihe von Demonstratoren entsprechend den Simulations- und Optimierungsergebnissen konstruiert und gefertigt. Der vorgeschlagene Entwurf besteht aus einem Trägerbalken, einem Magnetkreis mit mehreren Magnetanordnungen und einem magnetoelektrischen Wandler, der aus einer piezoelektrischen PMNT-Platte besteht, die mit zwei magnetostriktiven Terfenol-D-Schichten verbunden ist. Bei dieser Konstruktion werden externe Schwingungen in Magnetfeldänderungen umgewandelt, die auf die magnetostriktiven Schichten wirken und zu Verformungen führen, die direkt auf die piezoelektrische Schicht übertragen werden. Die Wandler werden unter harmonischen Anregungen und mit realen Schwingungsprofilen getestet, die von einer künstlichen Schwingungsquelle reproduziert werden. Verschiedene Parameter wurden experimentell untersucht, darunter die magnetischen Kräfte zwischen dem Wandler und dem Magnetkreis sowie die verwendete Verbindungstechnik. Die Abstimmung der Resonanzfrequenz des ME-Wandlers erfolgt ebenfalls über ein einfaches Schrauben-Mutter-System, das es ermöglicht, die relative Position und damit die magnetischen Kräfte zwischen Magnetkreis und Wandler zu steuern. Der magnetoelektrische Wandler, der mit einer Konzentration von 2 wt.% mehrwandiger Kohlenstoff-Nanoröhrchen verbunden ist, zeigt bessere Ausgangsleistungen als die beiden anderen ME-Wandler bei ähnlichen Anregungen. Eine maximale Ausgangsleistung von 2,42 mW wird bei 1 mm angelegter Vibration bei 40 Hz erreicht. Diese Leistung stellt eine Verbesserung von mindestens 20 % im Vergleich zu anderen magnetoelektrischen Schwingungsumrichtern dar, welche mit einem einzigen ME-Wandler bei vergleichbaren Anregungen getestet werden.