Kohlenstoffnanoröhrchen (engl. carbon nanotubes, CNTs) sind Dank ihrer außergewöhnlichen elektrischen Eigenschaften Kandidaten für eine Vielzahl von Anwendungen im Bereich der Mikroelektronik. Ihre ballistischen Transporteigenschaften und die geringe Anfälligkeit auf Elektromigration sind vorteilhaft für die Anwendung von CNTs in Interconnectsystemen. Die Abhängigkeit der elektrischen Transporteigenschaften von mechanischer Verformung bildet weiterhin die Grundlage für die Produktion neuartiger Sensoren auf CNT-Basis. Durch die Besetzung mit Adatomen können diese Eigenschaften dabei weiter verbessert und bei der Herstellung gezielt eingestellt werden. Die Verformung besetzter CNTs ist dabei ein noch relativ unerforschtes Gebiet. In dieser Arbeit wird dieses Verhalten untersucht. Zu Beginn wird gezeigt, dass die Eigenschaften von CNTs durch die Besetzung mit verschiedenen Metallen auf unterschiedliche Weise beeinflusst werden können. Dazu gehören auch Unterschiede zwischen den Spinzuständen, welche bei einigen der untersuchten Metalle auftreten. Durch die axiale Verformung der CNTs wird abschließend gezeigt, dass die Sensoreigenschaften von CNTs auch nach der Besetzung mit Metallen erhalten bleiben.:Zusammenfassung 1. Einleitung 2. Übersicht über Kohlenstoffnanoröhrchen 2.1. Geometrische Eigenschaften 2.1.1. Kohlenstoff als Grundbaustein für Graphen und CNTs 2.1.2. Geometrie von CNTs ausgehend von Graphen 2.2. Elektrische Struktur von Graphen und CNTs 2.3. Piezoelektrisches Verhalten 3. Theoretische Grundlagen 3.1. Dichtefunktionaltheorie 3.1.1. Grundproblem und Motivation 3.1.2. Grundstein der DFT - das Hohenberg-Kohn-Theorem 3.1.3. Praktische Umsetzung - die Kohn-Sham-Gleichungen 3.1.4. Abschätzung des Austausch-Korrelations-Funktionals 3.2. Grundlagen zum elektrischen Transport 3.2.1. Kurze Einführung zu Transportrechnungen 3.2.2. Landauer-Büttiker-Formalismus 4. Numerische Methoden 4.1. Initialisierung und Manipulation der Strukturen 4.2. Umsetzung der DFT 5. Berechnungen und Ergebnisse 5.1. Wahl des Modellsystems 5.1.1. Das zu untersuchende CNT 5.1.2. Auswahl der Adatome 5.2. Wahl der Parameter 5.3. Einige Überlegungen zum unbesetzten (8,4)-CNT 5.4. Untersuchung der Gleichgewichtspositionen 5.5. Analyse der Bandstruktur des besetzten CNTs 5.6. Einfluss auf Leitfähigkeit und Widerstand 5.7. Untersuchung der Spineigenschaften 5.8. Besetzungsgrad von Pd 5.9. Verformung der funktionalisierten CNTs 5.9.1. Implementation 5.9.2. Veränderungen der Struktur 5.9.3. Verhalten der Bandlücke bei einfacher Besetzung 5.9.4. Verhalten der Bandlücke bei mehrfacher Besetzung 5.9.5. Vergleich der verschieden besetzten CNTs bei Streckung 5.9.6. Verhalten des elektrischen Widerstandes bei Streckung 6. Zusammenfassung der Ergebnisse und Ausblick Literaturverzeichnis A. Bandstrukturen bei Verformung B. Transmissionsfunktionen für Besetzungsgrade C. Danksagung D. Selbstständigkeitserklärung

During the last decade, ultrasonic manipulation has matured into an important tool with a wide range of applications, from fundamental cell biological research to clinical and industrial implementations. The contactless nature of ultrasound makes it possible to manipulate living cells in a gentle way, e.g., for positioning, sorting, and aggregation. However, when manipulating cells using ultrasound, especially using high acoustic amplitudes, a great deal of heat can be generated. This constitutes a challenge, since the viability of cells is dependent on a stable physiological temperature around 37°C.      In this Thesis we present applications of ultrasonic manipulation of fluids, particles, and cells in temperature-controlled micrometer-sized devices fabricated using well established etching techniques, directly compatible with high-resolution fluorescence microscopy. Furthermore, we present ultrasonic manipulation in larger up to centimeter-sized devices optimized for fluid mixing and cell lysis. In the present work, two new ultrasonic manipulation platforms have been developed implementing temperature control. These platforms are much improved with increased performance and usability compared to previous platforms. Also, two new ultrasonic platforms utilizing low-frequency ultrasound for solubilization and cell lysis of microliter-volumed and milliliter-volumed samples have been designed and implemented.      We have applied ultrasound to synchronize the interaction between large numbers of immune, natural killer cells, and cancer cells to study the cytotoxic response, on a single cell level. A heterogeneity was found among the natural killer cell population, i.e., some cells displayed high cytotoxic response while others were dormant. Furthermore, we have used temperature-controlled ultrasound to form up to 100, in parallel, solid cancer HepG2 tumors in a glass-silicon multi-well microplate. Next, we investigated the immune cells cytotoxic response against the solid tumors. We found a correlation between the number of immune cells compared to the size of the tumor and the cytotoxic outcome, i.e., if the tumor could be defeated.             Finally, the effect of high acoustic pressure amplitudes in the MPa-range on cell viability has been studied in a newly developed platform optimized for long-term stable temperature control, independent on the applied ultrasound power. Lastly, we present two applications of ultrasonic fluid mixing and lysis of cells. One platform is optimized for small microliter-sized volumes in plastic disposable chips and another is optimized for large milliliter-sized volumes in plastic test tubes. The latter platform has been implemented for clinical sputum sample solubilization and cell lysis for genomic DNA extraction for subsequent pathogen detection / Ultraljudsmanipulering har under de senaste tio åren mognat och utvecklats till ett verktyg med ett brett användningsområde. Idag kan man finna applikationer inom allt från cellbiologisk grundforskning till industri samt sjukvård. Ultraljudsmanipuleringens kontaktlösa natur gör det till en varsam metod för att manipulera celler, till exempel inom positionering, sortering och aggregering. När ultraljud med hög amplitud används kan värmeutvecklingen, som är oundviklig, bli ett problem. För att kunna säkerställa hög cellviabilitet krävs temperaturkontroll som kan hålla en fysiologisk, stabil temperatur på 37°C.      I denna avhandling presenterar vi tillämpningar av temperaturkontrollerad ultraljudsmanipulering i mikrometerstora anordningar fabricerade med väletablerade etsningstekniker.  Dessa anordningar är optimerade för att vara fullt kompatibla med högupplöst fluorescensmikroskopi.  Vi demonstrerar även ultraljudsmanipulering i centimeterstora anordningar optimerade för omrörning och blandning av vätskor samt lysering av celler. Två nya plattformar för ultraljudsmanipulering med inbyggd temperaturkontroll har utvecklats. Dessa två plattformar erbjuder ökad prestanda, flexibilitet samt även användarvänlighet. Utöver dessa plattformar har ytterligare två anordningar för lågfrekvent ultraljudssolubilisering och cellysering av mikroliter- och milliliterstora prover konstruerats.      I denna avhandling har vi tillämpat ultraljud för att synkronisera interaktionen mellan populationer utav immunceller (natural killer-celler) och cancerceller för att på cellnivå studera det cytotoxiska gensvaret. Vi fann en heterogenitet hos immuncellspopulationen. Det manifesterade sig i en fördelning av immuncellerna, från celler med stort cytotoxiskt gensvar till inaktiva immunceller. Vi har dessutom använt temperaturkontrollerad ultrasljudsmanipulering för att skapa solida cancertumörer utav HepG2-cancerceller, upp till 100 stycken parallellt, i en multihåls-mikrotiterplatta bestående av glas och kisel. Med hjälp av dessa tumörer har vi studerat det cytotoxiska gensvaret från immuncellerna. Vi fann att förhållandet mellan antalet immunceller och storleken på tumören bestämde utfallet, det vill säga om tumören kunde bekämpas.      Vi presenterar dessutom effekten utav högamplitudsultraljudsexponering av cancerceller i en plattform speciellt designad för höga tryckamplituder med implementerad ultraljudseffektsoberoende temperaturkontroll. Slutligen presenterar vi två tillämpningar av ultraljud för vätskeblandning och cellysering. Den första tillämpningen är anpassad för små volymer i plastchip för engångsbruk och den andra är optimerad för större volymer i plastprovrör. Den senare tillämpningen är speciellt framtagen för ultraljudssolubilisering och cellysering utav kliniska sputumprover för att möjliggöra DNA-extrahering för detektion av smittämnen. / <p>QC 20150522</p>

No description available.

Die Arbeit befasst sich mit der effizienten Simulation des funktionellen Verhaltens von Piezoverbundmodulen als Aktor oder Sensor zur Schwingungsbeeinflussung mechanischer Strukturen. Ausgehend von einem FE-Modell werden über den Ansatz energetischer Äquivalenz die effektiven elektro-mechanischen Materialparameter ermittelt. Zur Berücksichtigung im Inneren der Einheitszelle liegender Elektroden werden die elektrischen Randbedingungen der Homogenisierungslastfälle angepasst. Die Homogenisierungslastfälle werden auch genutzt, um Phasenkonzentrationen für die Beanspruchungen der Verbundkomponenten zu ermitteln. Diese Phasenkonzentrationen werden eingesetzt, um aus dem effektiven Gesamtmodell die Beanspruchungen der Komponenten zu extrahieren. Zur dynamischen Modellbildung wird die Zustandsraumbeschreibung verwendet. Die Überführung einer piezo-mechanischen FE-Diskretisierung in ein Zustandsraummodell gelingt mit der Betrachtung der mechanischen Freiheitsgrade als Zustandsvariablen. Zur Abbildung der elektrischen Impedanz im Zustandsraum muss die elektrische Kapazitätsmatrix als Durchgangsmatrix einbezogen werden. Die Reduktion des Zustandsraums basiert auf der modalen Superposition. Die modale Transformationsbasis wird um Moden ergänzt, die die Verformung bei statischer elektrischer Erregung charakterisieren. Die Zustandsraumbeschreibung wird sowohl für eine Potential- als auch für eine Ladungserregung ausgeführt. Das Zustandsraummodell wird unter Verwendung von Filtermatrizen um Ausgangssignale für die mechanischen und elektrischen Beanspruchungsgrößen erweitert. Dies gestattet eine Kopplung der Zustandsraummodelle mit den Beanspruchungsanalysen. Die Anwendung der Berechnungsmethode wird am Beispiel der im SFB/TRR PT-PIESA entwickelten Piezo-Metall-Module demonstriert, die durch direkte Integration von piezokeramischen Basiselementen in Blechstrukturen gekennzeichnet sind.:1 Einleitung 2 Grundlagen 3 Stand der Forschung 4 Beanspruchungsermittlung für piezo-mechanische Verbunde 5 Zustandsraumbeschreibung piezo-mechanischer Systeme 6 Gesamtmodell 7 Zusammenfassung / This thesis deals with the efficient simulation of the functional behaviour of piezo composite modules for applications as actuators or sensors to influence vibrations of machine structures. Based on a FE-discretisation the effective electro-mechanical material parameters of the piezo composite modules are determined with an ansatz of energetic equivalence. To consider electrodes which are located inside the representative volume element the electrical boundary conditions of the load cases for homogenisation are adapted. The load cases for homogenisation are also used to determine the phase concentrations (or fluctuation fields) of stress/strain and electric field/electric displacement field in the composite constituents. These phase concentrations are required to extract stress and strain of the composite components based on the overall model with effective material parameters. For dynamical modelling a state space representation is used. The transformation of a FE-discretisation of the piezo-mechanical system into a state space model is possible by choosing the mechanical degree of freedom as state variables. For consideration of the electrical impedance in the state space model the electrical stiffness respectively capacitance matrix has to incorporate as feedthrough matrix. The dynamical model reduction of the state space model is based on modal superposition. For the correct reproduction of the electrical impedance the modal transformation basis has to be amended by deformation modes which represent the deformation behaviour due to static electrical excitation at the electrodes. The state space representation is built for potential and charge excitation. The state space model is enhanced by filter matrices to incorporate output signals for stress/strain and also for electric field/electric displacement field. This allows the coupling of the state space models with the stress analyses. The application of the simulation method is demonstrated using the example of the piezo-metal-modules developed in the CRC/TR PT-PIESA (German: SFB/TRR PT-PIESA). These piezo-metal-modules are characterised by direct integration of piezoceramic base elements in sheet metal structures.:1 Einleitung 2 Grundlagen 3 Stand der Forschung 4 Beanspruchungsermittlung für piezo-mechanische Verbunde 5 Zustandsraumbeschreibung piezo-mechanischer Systeme 6 Gesamtmodell 7 Zusammenfassung

Tesis por compendio / Neutrino telescopes are a new way of looking at the Universe. For more than a decade these structures are being designed to study the Universe from a new point of view, that is, from the particles generated in the cosmic accelerators of particles. These infrastructures are not only useful to study the Universe, but they can also be used in the field of Particle Physics and even in the study of underwater life. Most of these telescopes are based on the detection of the so-called Cherenkov light using photomultipliers, the difference between them lies in the medium in which they are located (ice or water) and in the infrastructure used. Specifically, European telescopes mount these photomultipliers in an underwater vertical structure anchored at great depth, which is under the influence of sea currents. For this reason they suffer displacements that affect the location of the photomultipliers and it becomes necessary to implement a positioning system for the telescope to be functional. For this, an acoustic system consisting of emitters anchored to the sea floor and receivers located at the different levels of the vertical structure is used. One of the objectives of the present thesis is the development of these acoustic emitters. For this purpose we have developed different laboratory prototypes with different features until obtaining an improved prototype that was installed and tested in ANTARES and NEMO telescopes. This showed that the prototype worked perfectly within the established requirements and then, we proceed to design a final version of the much more powerful and functional emitter, acoustic beacon, to be mounted inside aluminum vessels together with an omnidirectional acoustic transducer, which will be located in anchored positions of the new KM3NeT neutrino telescope. In collaboration with the MSM Company, 18 acoustic beacons were developed for KM3NeT-ARCA being two of them installed in the first marine campaign at the end of 2015, and being able then to verify their correct operation. On the other hand, interaction of ultraenergetic neutrinos with matter also produces a thermoacoustic pulse with bipolar form, axial symmetry and highly directive. The feasibility of the acoustic detection technique and the possibility of implementing it in these telescopes have been under study for years. In order to test and calibrate this technique, it is necessary to have an acoustic emitter system able of generating a signal similar to the neutrino signature. This has been the second objective developed in this thesis. To achieve this objective, a compact and versatile calibrator based on an array of acoustic transducers using parametric generation has been designed. Given the complexity of the pulse to emulate and the novelty of the technique to be used, it has been necessary to carry out different laboratory tests in order to obtain suitable transducers and electronics able of making them to work at the required power and efficiency. The positive results obtained in this line suggest that we will be able to obtain a full functional neutrino acoustic calibrator soon. Finally, I would like to mention that I have participated in the different research and activities described in the thesis, putting especial emphasis in the development of the electronics and the software/firmware of the developed acoustic emitters. / Los telescopios de neutrinos son una nueva forma de observar el Universo. Desde hace más de una década se están diseñando este tipo de estructuras con el propósito de estudiar el Universo desde un nuevo punto de vista, el de las partículas que se generan en los aceleradores de partículas cósmicos. Estas infraestructuras no solo se limitan al estudio del Universo, sino que también pueden ser utilizadas en el campo de la Física de partículas e incluso en el estudio de la vida submarina. La mayoría de estos telescopios se basan en la detección de la llamada luz de Cherenkov mediante fotomultiplicadores, la diferencia entre ellos radica en el medio en que se ubican (hielo o agua) y en la infraestructura utilizada. Concretamente, los telescopios europeos montan dichos fotomultiplicadores en una estructura vertical submarina anclada a gran profundidad, la cual está sometida a la influencia de las corrientes marinas. Por este motivo sufren desplazamientos que afectan a la localización de los fotomultiplicadores y se hace necesaria la implementación de un sistema de posicionamiento para que el telescopio sea funcional. Para ello se utiliza un sistema acústico consistente en unos emisores anclados al suelo marino y unos receptores situados en los diferentes niveles de la estructura vertical. Uno de los objetivos de la presente tesis es el desarrollo de estos emisores acústicos. Con este fin se han desarrollado diferentes prototipos de laboratorio con los que se han ido escalando prestaciones hasta obtener un prototipo que ha sido instalado y testeado en los telescopios ANTARES y NEMO. Así se demostró que el prototipo funcionaba perfectamente dentro de los requisitos establecidos, pasándose a diseñar una versión final del emisor acústico mucho más potente y funcional para ser montada dentro de vasijas de aluminio junto con un traductor omnidireccional en las anclas del nuevo telescopio de neutrinos KM3NeT. Conjuntamente con la empresa MSM se elaboraron 18 equipos para KM3NeT-ARCA, dos de los cuales fueron instalados en la primera campaña marina a finales de 2015 comprobándose su correcto funcionamiento. Por otro lado, la interacción de los neutrinos ultraenergéticos con la materia también produce un pulso termoacústico con forma bipolar, simetría axial y altamente directivo. Desde hace años se está estudiando la viabilidad de la técnica de detección acústica y la posibilidad de implementarla en dichos telescopios. Para poder poner a prueba y calibrar dicha técnica es necesario disponer de un sistema emisor acústico que sea capaz de generar una señal similar a la descrita. Este ha sido el segundo objetivo desarrollado en esta tesis. Para ello se ha diseñado un calibrador compacto y versátil basado en un array de transductores acústicos usando generación paramétrica. Dada la complejidad del pulso a emular y lo novedoso de la técnica a utilizar, se ha requerido la realización de numerosas pruebas de laboratorio con el fin de conseguir unos transductores adecuados y la electrónica capaz de hacerlos funcionar a la potencia y eficiencia requerida. Los positivos resultados obtenidos en esta línea hacen prever que, en breve, podremos obtener un calibrador acústico de neutrinos funcional. Finalmente, cabe reseñar que he participado en las diferentes investigaciones y actividades que se describen en la tesis, siendo mi cometido principal el desarrollo tanto de la electrónica como de los diferentes softwares/firmwares implicados en los emisores acústicos desarrollados. / Els telescopis de neutrins són una nova forma d'observar l'Univers. Des de fa més d'una dècada s'estan dissenyant aquest tipus d'estructures amb el propòsit d'estudiar l'Univers des d'un nou punt de vista, el de les partícules que es generen en els acceleradors de partícules còsmics. Estes infraestructures no sols es limiten a l'estudi de l'Univers, sinó que també poden ser utilitzades en el camp de la Física de partícules i fins i tot en l'estudi de la vida submarina. La majoria d'aquests telescopis es basen en la detecció de l'anomenada llum de Cherenkov per mitjà de fotomultiplicadors, la diferència entre ells radica en el mig en què s'ubiquen (gel o aigua) i en la infraestructura utilitzada. Concretament, els telescopis europeus munten dits fotomultiplicadors en una estructura vertical submarina ancorada a gran profunditat, la qual està sotmesa a la influència dels corrents marins. Per este motiu pateixen desplaçaments que afecten a la localització dels fotomultiplicadors i es fa necessària la implementació d'un sistema de posicionament per a què el telescopi siga funcional. Per a això s'utilitza un sistema acústic consistent en uns emissors ancorats al sòl marí i uns receptors situats en els diferents nivells de l'estructura vertical. Un dels objectius de la present tesi és el desenvolupament d'aquests emissors acústics. Amb este fi s'han desenvolupat diferents prototips de laboratori amb els quals s'han anat escalant prestacions fins a obtindre un prototip que ha sigut instal·lat i testeat en els telescopis ANTARES i NEMO. Així es va demostrar que el prototip funcionava perfectament dins dels requisits establerts, passant-se a dissenyar una versió final de l'emissor acústic molt més potent i funcional per a ser muntada dins d'atuells d'alumini junt amb un traductor omnidireccional en les àncores del nou telescopi de neutrins KM3NeT. Conjuntament amb l'empresa MSM es van elaborar 18 equips per a KM3NeT-ARCA, dos dels quals van ser instal·lats en la primera campanya marina a finals de 2015 comprovant-se el seu correcte funcionament. D'altra banda, la interacció dels neutrins ultraenergètics amb la matèria també produeix un pols termoacústic amb forma bipolar, simetria axial i altament directiu. Des de fa anys s'està estudiant la viabilitat de la tècnica de detecció acústica i la possibilitat d'implementar-la en els esmentats telescopis. Per a poder posar a prova i calibrar esta tècnica és necessari disposar d'un sistema emissor acústic que siga capaç de generar un senyal semblant al descrit. Aquest ha sigut el segon objectiu desenvolupat en aquesta tesi. Per a això s'ha dissenyat un calibrador compacte i versàtil basat en un array de transductores acústics utilitzant generació paramètrica. Donada la complexitat del pols a emular i la novetat de la tècnica a utilitzar, s'ha requerit la realització de nombroses proves de laboratori a fi d'aconseguir uns transductors adequats i l'electrònica capaç de fer-los funcionar a la potència i eficiència requerida. Els positius resultats obtinguts en esta línia fan preveure que, en breu, podrem obtindre un calibrador acústic de neutrins funcional. Finalment, cal ressenyar que he participat en les diferents investigacions i activitats que es descriuen en la tesi, sent la meua comesa principal el desenvolupament tant de l'electrònica com dels diferents softwares/firmwares implicats en els emissors acústics desenvolupats. / Llorens Alvarez, CD. (2017). Diseño y desarrollo de la electrónica de los emisores acústicos para los sistemas de posicionamiento y calibración de telescopios submarinos de neutrinos [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/88401 / Compendio

Researchers have offered a variety of solutions for overcoming the old and challenging problem of undesired vibrations. The optimum vibration-control solution that can be a passive, semi-active or active solution, is chosen based on the desired level of vibration-control, the budget and the nature of the vibration source. Mechanical vibration-control systems, which work based on variable stiffness control, are categorized as semi-active solutions. They are advantageous for applications with multiple excitation frequencies, such as seismic applications. The available mechanical variable stiffness systems that are used for vibration-control, however, are slow and usually big, and their slowness and size have limited their application. A new semi-active variable stiffness solution is introduced and developed in this thesis to address these challenges by providing a faster vibration-control system with a feasible size. The new solution proposed in this thesis is a semi-active variable stiffness mount/isolator called the antagonistic Variable Stiffness Mount (VSM), which uses a variable stiffness spring called the Antagonistic Variable stiffness Spring (AVS). The AVS is a kinematically singular prestressable mechanism. Its stiffness can be changed by controlling the prestress of the mechanisms links. The AVS provides additional stiffness for a VSM when such stiffness is needed and remains inactive when it is not needed. The damping of the VSM is constant and an additional constant stiffness in the VSM supports the deadweight. Two cable-mechanisms - kinematically singular cable-driven mechanisms and Prism Tensegrities - are developed as AVSs in this thesis. Their optimal configurations are identified and a general formulation for their prestress stiffness is provided by using the notion of infinitesimal mechanism. The feasibility and practicality of the AVS and VSM are demonstrated through a case study of a typical engine mount by simulation of the mathematical models and by extensive experimental analysis. A VSM with an adjustable design, a piezo-actuation mechanism and a simple on-off controller is fabricated and tested for performance evaluation. The performance is measured based on four criteria: (1) how much the VSM controls the displacement near the resonance, (2) how well the VSM isolates the vibration at high frequencies, (3) how well the VSM controls the motion caused by shock, and (4) how fast the VSM reacts to control the vibration. For this evaluation, first the stiffness of the VSM was characterized through static and dynamic tests. Then performance of the VSM was evaluated and compared with an equivalent passive mount in two main areas of transmissibility and shock absorption. The response time of the VSM is also measured in a realistic scenario.

No description available.

Conselho Nacional de Desenvolvimento Científico e Tecnológico / Hybrid nanostructures which integrate two or more technologically interesting physical properties are fundamental for developing new generations of electronic devices. Exhibiting at least two coupled ferroic orders, multiferroics are an outstanding class of multifunctional materials. Compounds which present coupling between ferromagnetism and ferroelectricity are specially interesting. Although natural multiferroics are rarely found, the possibility of obtaining strain-mediated magnetoelectric coupling in composite structures, by integrating magnetostrictive and piezoelectric layers, paves the way to control electric properties by applying magnetic field or to the electric control of magnetism. Nevertheless, most scientific efforts have been on monophasic compounds or bulk composites. Considering the incorporation of magnetoelectric nanostructures in devices, expanding the scope of the magnetoelectric effect and targetting it to different kinds of applications is needed. Besides new characterization techniques, seeking new alternative materials to the lead-based piezoelectrics or oxide-based magnetostrictives is necessary. Recently, a few works using semiconductors such as ZnO and AlN, or amorphous magnetic alloys such as those based on Co, Fe and Ni, have been reported. In spite of not presenting remarkable piezoelectric and magnetostrictive effects, the features of such materials are promising for high frequency applications, for instance. Considering these issues, four independent surveys are presented. Firstly, the origin of the coupling, latest advances and current scenario of the field are reviewed. Then magnetostriction measurements in thin films are addressed by employing a direct technique based on the cantilever-capacitance method. The goals are to study magnetoelastic properties of some materials whose magnetostriction are not found very often in literature, and to check the reliability of this technique for investigating thin films. In this sense, measurements of some amorphous magnetic alloys mainly based on Co, Fe and Ni are performed. Most samples presents larger magnetoelastic response for magnetic field applied along the magnetization easy axis, as opposed to the theoretically expected. Two investigations on aluminum nitride thin films are reported. Firstly, the growth of AlN films onto several different substrates and buffer layers is studied. Films grown onto glass and polyimide show excellent structural properties for eletromechanical systems and flexible electronics applications. Samples with low residual stress on silicon substrates, suitable for incorporating in existing technologies, are obtained. Secondly, bilayers composed by AlN and ferromagnetic films are investigated. In addition to the structural and morphological properties of the AlN films which are checked, the magnetic characterization of the structures also contributes to design multilayers for exploring the magnetoelectric effect. Finally, problems involving electric fields in scanning probe microscopies are adressed. Surface images of AlN piezoelectric films are systematically acquired. Among other major observations, the possibility of getting reliable piezoresponse images of strongly polarized areas as well as of visualizing ferroelastic domains, is demonstrated. Furthermore, a new microscopy for investigating a sample s ferro and piezoelectric properties is proposed, exploring the direct piezoelectric effect. By utilizing acoustic excitation and electrical detection, the potency of this technique is illustrated with measurements on quartz and AlN surfaces. / Nanoestruturas híbridas, integrando duas ou mais propriedades físicas de grande interesse tecnológico, são fundamentais para o desenvolvimento de novas gerações de dispositivos eletrônicos. Uma classe interessante de materiais multifuncionais são os multiferróicos, que exibem pelo menos duas ordens ferróicas acopladas. Dentre eles, os que apresentam acoplamento entre ferromagnetismo e ferroeletricidade despertam interesse especial. Apesar de serem raros de ocorrer naturalmente, a possibilidade de gerar efeito magnetoelétrico em estruturas compósitas, intermediado pela deformação elástica entre camadas magnetostrictivas e piezoelétricas, abre caminho para que seja possível controlar propriedades elétricas aplicando-se campo magnético, ou propriedades magnéticas aplicando-se campo elétrico. Todavia, a maior parte das pesquisas atuais ainda envolve compostos monofásicos ou compósitos em forma massiva. Tendo em vista a incorporação de nanoestruturas magnetoelétricas em dispositivos, é fundamental ampliar a abrangência do efeito magnetoelétrico e direcioná-lo para diferentes tipos de aplicações. Para isto, além de novas técnicas de caracterização, é necessário buscar-se materiais alternativos aos tradicionais piezoelétricos baseados em chumbo e magnetostrictivos baseados em óxidos. Recentemente tem-se encontrado trabalhos pontuais onde são utilizados piezoelétricos semicondutores como ZnO e AlN, e ligas magnéticas amorfas como as baseadas em Co, Fe e Ni. Mesmo sem apresentar efeitos piezoelétrico e magnetostrictivo com magnitudes notáveis, as características destes materiais são promissoras para aplicações envolvendo altas frequências, por exemplo. Neste necessário, são apresentados quatro estudos independentes entre si. Primeiramente, é realizada uma revisão sobre a origem do acoplamento, os últimos avanços e o panorama atual das pesquisas na área. Em seguida, através de uma técnica direta baseada no método do cantiléver-capacitância, aborda-se o problema das medidas de magnetostricção em amostras na forma de filmes finos. Os objetivos são estudar as propriedades magnetoelásticas em alguns materiais que não são frequentemente abordados pela literatura, e avaliar a potencialidade da técnica para a análise de filmes finos. Para isto, são realizadas medidas principalmente em ligas ferromagnéticas amorfas baseadas em Co, Fe e Ni. Para a maioria das amostras analisadas, a resposta magnetoelástica é maior quando o campo magnético é aplicado na direção do eixo de fácil magnetização, de forma contrária à esperada teoricamente. São apresentadas duas investigações envolvendo filmes finos de nitreto de alumínio. Primeiro é estudado o crescimento de filmes de AlN sobre vários substratos e camadas semente. Filmes crescidos sobre vidro e poliimida apresentam excelentes propriedades estruturais para aplicações em sistemas eletromecânicos e eletrônica flexível. Amostras obtidas com baixos valores de tensão residual, sobre substratos de silício, são interessantes para incorporação em tecnologias existentes. Segundo, são investigadas bicamadas de AlN com filmes ferromagnéticos. Além das propriedades estruturais e morfológicas dos filmes de AlN, a análise das características magnéticas das estruturas contribui para o design de multicamadas que exploram o efeito magnetoelétrico. Finalmente, são abordados problemas em medidas de microscopias de varredura por sonda envolvendo campos elétricos. Imagens da superfície de filmes piezoelétricos de AlN foram coletadas sistematicamente. Entre outras observações importantes, demonstra-se que é possível adquirir imagens confiáveis de piezo-resposta em regiões fortemente polarizadas, e visualizar a formação de domínios ferroelásticos. Também é proposta uma nova técnica de microscopia, para investigar as propriedades ferro e piezoelétricas de uma amostra, explorando o efeito piezoelétrico direto. Utilizando excitação acústica e detecção elétrica, o potencial da nova técnica é demonstrado com imagens de superfícies cristalinas de quartzo e AlN.

Ferroelectric materials are very promising for a variety of applications such as high-permittivity capacitors, ferroelectric memories, pyroelctric sensors, piezoelectric and electrostrictive transducers and electro-optic devices, etc. In the area of ferroelectric ceramics, lead-based compounds, which include lead zirconatetitanate (PZT) solid solutions, occupy an important place because of their superior physical properties. However, due to the toxicity of lead, there is an increasing concern over recycling and disposing of the devices made out of these compounds, which has compelled the researchers around the globe to search for lead-free compounds with promising piezo and ferroelectric properties. Ferroelectric materials that belong to Aurivillius family of oxides have become increasingly important from the perspective of industrial applications because of their high Curie-temperatures, high resistivity, superior polarization fatigue resistanceand stable piezoelectric properties at high temperatures. These bismuth layer-structured ferroelectrics (BLSF) comprise an intergrowth of [Bi2O2]2+ layers and [An+1Bn O3n+1]2- pseudo-perovskite units, where ‘n’ represents the number of perovskite-like layers stacked along the c-axis. ‘A’ stands for a mono-, di- or trivalent ions or a combination of them, ‘B’ represents a small ion with high valencysuch as Ti4+, Nb5+, Ta5+or a combination of them.Ferroelectricity in the orthorhombic phase of these compounds was generally attributed to the cationic displacement along the polar a-axis and the tilting of octahedra around the a- and c-axes. Sr2Bi4Ti5O18(SBT) is ann = 5 member of the Aurivillius family and possess promising ferroelectric and piezoelectric properties that could be exploited for a wide range of applications, including ferroelectric random access memories (FeRAM), piezoelectric actuators, transducers and transformers. Reports in the literaturereveal that the ferroelectricand piezoelectric properties of these oxides can be tuned depending on synthesis routes vis-a-vis micro-structural aspects (texture, grain size) and site specific dopant substitutions.In the present study, textured SBT ceramics were fabricated using pre-reacted precursors and their anisotropic dielectric, piezoelectric and ferroelectric properties were demonstrated. Grain size tunability with regard to their physical properties was accomplished in the ceramics, fabricated using fine powders obtained from citrate assisted sol-gel synthesis. The grain size dependent second harmonic generation activity of SBT ceramics was investigated. Enhancement in the piezoelectric and ferroelectric properties of SBT ceramics was achieved by substituting A site ions (Sr2+) with a combination of Na+ and Bi3+. From the perspective of non-linear optical device applications, physical properties associated with the SBT crystallized in a transparent lithium borate glass matrix were studied. The results obtained in the present investigations are organized as follows, Chapter 1 gives a brief exposure to the field of ferroelectrics. The emphasis has been on the ferroelectric oxides belonging to the Aurivillius family. Structural aspects and the underlying phenomena associated with ferroelectricity in these compounds are discussed. A brief introduction to the glasses, thermodynamic aspects of glass formation and fabrication of glass- ceramics are included. Basic principles involved in the non-linear optical activities are highlighted. Chapter 2 describes the various experimental techniques that were employed to synthesize and characterize the materials under investigation. The experimental details pertaining to the measurement of various physical properties are included. Chapter 3 deals with the fabrication of Sr2Bi4Ti5O18 ceramics using the pre-reacted Bi4Ti3O12 and SrTiO3 powders viasolid-state reaction route. These in stoichiometric ratio were uniaxially pressed and sintered at 1130oC for 3 h resulting in textured Sr2Bi4Ti5O18 ceramics. The obtained dense ceramics exhibited crystallographic anisotropy with prominent c-axis oriented grains (Lotgering factor of 0.62) parallel to the uniaxially pressed direction. The resultant anisotropy in the ceramics was attributed to the reactive template-like behavior of Bi4Ti3O12 that was used as a precursor to fabricate Sr2Bi4Ti5O18 ceramics. Dielectric, ferro and piezoelectric properties measured on the ceramics in the direction perpendicular to the uniaxially pressed axis were found to be superior to that measured in the parallel direction. Chapter 4 reports the details pertaining to the synthesis of strontium bismuth titanate (Sr2Bi4Ti5O18) powders comprising crystallites of average sizes in the range of 94–1400 nm via citrate-assisted sol-gel route. X-ray powder diffraction, Transmission Electron Microscopy (TEM) and Raman spectroscopy were employed for the structural studies. A crystallite size-dependent variation in the lattice parameters and the shift in the Raman vibration modes were observed. Second harmonic signal (532 nm) intensity of the Sr2Bi4Ti5O18 powders increased with the increase in the average crystallite size and the maximum intensity obtained in the reflection mode was 1.4 times as high as that of the powdered KH2PO4. Piezo force microscopic analyses carried out on an isolated crystallite of size 74 nm, established its single domain nature with the coercive field as high as 347 kV/cm. There was a systematic increase in the d33 value with an increase in the size of the crystallite and a high piezoelectric coefficient of ~27 pm/V was obtained from an isolated crystallite of size 480 nm. Chapter 5 illustrates the details concerning the fabrication of Sr2Bi4Ti5O18(SBT) ceramics with different grain sizes (93 nm–1.42 μm) using nano-crystalline powders synthesized via citrate assisted sol-gel method. The grain growth in these powder compacts was found to be controlled via the grain boundary curvature mechanism, associated with anactivation energy of 181.9 kJ/mol. Interestingly with a decrease in grain size there was an increase in the structural distortion which resulted in a shift of Curie-temperature (phase transition) towards higher temperatures than that of conventional bulk ceramics. Extended Landau phenomenological theory for the ferroelectric particles was invoked to explain experimentally observed size dependent phase transition temperature and the critical size for SBT is predicted to be 11.3 nm. Grain size dependent dielectric, ferroelectric and piezoelectric properties of the SBT ceramics were studied and the samples comprising average grain size of 645 nm exhibited superior physical properties that include remnant polarization (2Pr) = 16.4 μC cm-2, coercive field (Ec) = 38 kV cm-1, piezoelectric coefficient (d33) = 22 pC N-1 and planar electromechanical coupling coefficient (kp) = 14.8 %. In Chapter 6, the studies pertaining to the fabrication of Sr(2-x)(Na0.5Bi0.5)xBi4Ti5O18 (SNBT) ceramics for various x values (0, 0.1, 0.25, 0.3, 0.4 and 0.5), using fine powders synthesized via sol-gel route are dealt with. X-ray powder diffraction, transmission electron microscopy and Raman spectroscopic studies were carried out to confirm composition dependent structural changes taking place in the SNBT ceramics. Scanning electron microscopic studies carried out on ceramics revealed that dopants played an important role in inhibiting the grain growth. Dielectric constants of the ceramics were found to decrease with an increase in ‘x’. The increase in Curie temperature with increase in ‘x’ is attributed to the decrease in the tolerance factor. Particularly,x = 0.3 composition of the SNBT ceramics exhibited better piezo and ferroelectric properties with a higher Curie-temperature (569 K). The piezoelectric coefficient (d33) and the planar electromechanical coupling coefficient (kp) of SNBT(x = 0.3) were enhanced by 25% and 42% respectively as compared to that of the undoped ceramics. Chapter 7 deals with the glasses in the system (100 –x) {Li2O + 2B2O3} ─x {2SrO + 2Bi2O3 +5TiO2} (where, x = 10, 25 and 35) fabricated via conventional melt-quenching technique. The amorphous and glassy characteristics of the samples were confirmed respectively using X-ray diffraction (XRD) and differential scanning calorimetric (DSC) methods. All the compositions under investigation exhibited two distinct crystallization peaks (exothermic peaks in the DSC traces): the first peak at ~ 545 °C and the second at ~610 °C that were found to be associated with the crystallization of the phases (as confirmed from the XRD studies) Sr2Bi4Ti5O18 (SBT)and Li2B4O7 (LBO) respectively. Non-isothermal crystallization kinetics (using modified Ozawa-type plots) for SBT crystallization in the LBO glass matrix for the compositions x = 10 and 35, indicated three dimensional growth of the crystallites from pre-existing nuclei present in the as-quenched samples and their effective activation energies for crystallization were found to be around 686 ± 85 kJ/mol and 365 ± 53 kJ/mol, respectively. The optical band gap of the as-quenched glasses for the composition x = 35 was 2.52 eV, is less than that of the composition x = 10 (2.91 eV). The Urbach energies for the as-quenched glasses of compositions x = 10, 25 and 35 were found to be 118 ± 2 meV, 119 ± 2 meV and 192 ± 1 meV respectively.The glasses associated with the composition x = 35, on controlled heat-treatment at 515 °C for various durations (1―20 h), yielded glass-ceramics comprising SBT nano-crystals (18―28 nm) embedded in the LBO glass matrix. Compressive strain in the nano-crystallites of SBT, analyzed using Williamson-Hall method was found to decrease with an increase in the crystallite size. The second harmonic generation signal (532 nm) intensity emanating from glass-nanocrystal composites comprising 22.1 nm SBT crystallites was nearly 0.3 times that of a KDP single crystal. Although each chapter is provided with conclusions and a list of references, thesis ends with a separate summary and conclusions.

Im ESF geförderten Projekt E-PISA sind verschiedene, hoch innovative, von der globalen Forschungslandschaft ausgezeichnete und gleichzeitig industrierelevante technische Entwicklungen im Bereich der Mikrosystemtechnik, Medizintechnik und Industrie 4.0 vorangetrieben worden. Fokus der technischen Entwicklung waren zum einen Grundlagenforschung und zum anderen Applikationen von Mikrosystemen auf Basis piezoelektrischer Dünnschichten mit Aluminiumnitrid und Elektronik mit Carbon-Nano-Tubes.:Liebe LeserInnen, 5 E-PISA Team 6 Innovative Applikationen 11 Innovative Technologien 13 Regionaler Bezug 15 Wissenstransfer in Zahlen 17 Piezoelektrisches Dünnschicht-Aluminiumnitrid für Mikrosysteme 19 Mikro-opto-elektro-mechanische Systeme 23 Acoustic Emission Sensoren 29 Drucksensoren für medizinische Katheter 33 Kristallwachstum 37 Innovationssysteme, Märkte und Forschungsnetzwerke 45 Zuverlässigkeit piezoelektrischer Schichtsysteme der Mikrotechnologie 51 Veröffentlichungen und Auszeichnungen 53 Zukunftsfähigkeit 61 Danksagung 63