Abstract The thesis describes electrically tunable microwave devices utilising low sintering temperature, screen printable Barium Strontium Titanate (BST) thick films. The work has been divided into two parts. In the first section, the fabrication and microwave characterisation of BST material based structures compatible with Low Temperature Cofired Ceramic technology (BST-LTCC) are presented. Three different fabrication techniques, namely: direct writing, screen printing and via filling techniques, were used for the realisation of the structures. A detailed description of these fabrication techniques is presented. The dielectric properties such as relative permittivity, static electric field dependent tunability and loss tangent of BST-LTCC structures at microwave frequencies were characterised using coplanar waveguide transmission line and capacitive element techniques. The measured dielectric properties of BST-LTCC structures realised with the different fabrication methods are presented, compared and discussed. The second section describes tunable microwave devices based on BST-LTCC structures. A frequency tunable folded slot antenna (FSA) with a screen printed, integrated BST varactor is presented. The resonant frequency of the FSA was tuned by 3.2% with the application of 200 V external bias voltage. The impact of the BST varactor on the total efficiency of the antenna was studied through comparison with a reference antenna not incorporating the BST varactor. A compact, frequency tunable ceramic planar inverted-F antenna (PIFA) utilising an integrated BST varactor for mobile terminal application is presented. The antenna's resonant frequency was tuned by 3% with an application of 200 V bias voltage. Frequency tunable antennas with a completely integrated electrically tunable BST varactor with silver metallisation are introduced in this work for the first time. The integration techniques which are described in this thesis have not been previously reported in scientific literature. The last part of the thesis presents a microwave delay line phase shifter operating at 3 GHz based on BST-LTCC structures. The figure of merit (FOM) of the phase shifter was measured to be 14.6 °/dB at 3 GHz and and the device employs a novel structure for its realisation that enabled the required bias voltage to be decreased, while still maintaining compliance with standard screen printing technology. The performance of the phase shifter is compared and discussed with other phase shifters realised with the BST thick film process. The applications of BST-LTCC structures were demonstrated through frequency tuning of antennas, varactors, and phase shifters. The low sintering temperature BST paste not only enables the use of highly conductive silver metallisation, but also makes the devices more compact and monolithic.

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Nanoscale ferroelectric materials have numerous possible applications such as actively tunable photonic crystals, terahertz emitters, ultrasound transducers, and energy harvesters. One of most technologically relevant ferroelectric materials is lead zirconate titanate (PZT) due to its large piezoelectric response. However, there are limited methods currently available for creating nanoscale PZT structures. Current top-down patterning methods include material removal via a high energy beam, which damages the piezoelectric's properties, and wet etching, which is an isotropic process that results in poor edge definition. Similarly, current bottom-up approaches such as hard template-growth and hydrothermal processing have limited control over the aspect ratio of the structures produced and lack site specific registry. In this work, a bottom-up approach for creating PbZr₀.₅₂Ti₀.₄₈O₃ nanotubes was developed using soft-template infiltration by a sol-gel solution. This method allows excellent control of the structures produced, overcoming current manufacturing limitations. PZT nanotubes were fabricated with diameters ranging from 100 to 200 nm, aspect ratios (height to diameter) from 1.25:1 to 5:1, and wall thicknesses from 5 to 25 nm. The piezoelectric and ferroelectric nature of the nanotubes was characterized via scanning probe microscopy in order to investigate nanoscale phenomena. Specifically, the effects of lateral constraint, substrate clamping, and critical size on the extrinsic contribution to the piezoelectric response were studied and the results are discussed.

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Nous avons développé une nouvelle méthode de microscopie par effet électro-optique linéaire (effet Pockels), dite PLEOM, permettant de cartographier la susceptibilité du deuxième ordre Chi(2) d'un matériau non-centrosymétrique [1, 2]. Cette méthode est complémentaire de la microscopie de génération de seconde harmonique, et s’en distingue par différents aspects physiques et pratiques. Grâce à une détection interférométrique stabilisée, le retard de phase provoqué par une variation d'indice locale du matériau non-linéaire sous l'effet d'un champ électrique est détecté à 10-6 radians près, ouvrant la voie à l'imagerie d'échantillons biologiques ou au suivi du mouvement de nano-sondes [3]. PLEOM apporte un type de données nouveau, la "réponse en phase" du matériau, porteuse d'information physiques plus difficilement accessibles en microscopie biphotonique.Ce manuscrit décrit de nouveaux domaines de développement et d’application de PLEOM, qui a évolué vers une plateforme aux applications variées et multi-échelles, allant du nanométrique au millimétrique.Nous avons tout d’abord montré comment déterminer le vecteur de polarisation attaché à des nano-cristaux ferroélectriques uniques, en vue de leur utilisation comme nano-sondes. Cette nouvelle méthode permet, à notre connaissance de façon unique, de distinguer deux nano-cristaux mono-domaines d'orientations exactement opposées, dont les réponses en SHG ne peuvent pas être distinguées. Une image de phase électro-optique, combinée à un diagramme de polarisation, donne accès à l'orientation vectorielle d'un nano-cristal orienté aléatoirement dans le référentiel du laboratoire. Un verrou est ainsi levé pour des applications comme l'imagerie de nano-domaines ferroélectriques, celle de potentiels électrochimiques membranaires, où l'étude de la dynamique de rotation de molécules. Deux spécificités remarquables de PLEOM en font une méthode d'avenir : la faible intensité de pompage qui assure une bien meilleure biocompatibilité ainsi que la simplicité de la source laser continue utilisée.Nous avons ainsi pu utiliser PLEOM pour caractériser les domaines ferroélectriques d'un cristal de KTiOPO4 périodiquement réorienté en vue d’un quasi-accord de phase, ainsi que ceux d'un cristal bidimensionnel quasi-périodique de LiNbO3. Un retournement clair de la phase de 180 degree est observé au travers des parois de domaines, dont les coefficients électro-optiques apparaissent opposés dans le référentiel du laboratoire. PLEOM se présente ainsi comme un outil de caractérisation non destructif des propriétés de ces cristaux artificiels dont les motifs et les défauts (tels qu'une orientation localement incomplète) ont été caractérisés spatialement, et permet de mesurer localement leurs propriétés non-linéaires, dont le caractère tensoriel permet d’aller au-delà des informations acquises en microscopie classique.En outre, nous avons fait la preuve de principe d'une nouvelle expérience biomimétique, visant à étudier les potentiels membranaires cellulaires, en utilisant PLEOM sur des membranes phospholipidiques créées sur puce micro-fluidique et dopées en colorants. / Complementing Second-Harmonic Generation (SHG) microscopy, a new home-made nonlinear microscope named Pockels Linear Electro-Optical Microscopy (PLEOM) based on the linear electrooptic (Pockels) effect, has been developed and used to map the second-order susceptibility Chi(2) of non-centrosymmetric materials with high sensitivity due to a stabilized interferometric homodyne detection scheme [1, 2]. This enables PLEOM to detect the electrooptic phase retardation of light resulting from the variation of the refractive index of nonlinear materials down to 10-6 radian and to investigate nonlinear materials at the nano-scale [3] towards applications in imaging of biological samples and tracking of labels therein. With PLEOM, a new imaging method allows to access, besides the aplitude, the no less crucial phase response, which is not readily amenable to classical SHG microscopy. In the frame of this dissertation, we have further extended the range of applications of PLEOM to investigate nonlinear materials and structures from nano- to millimeter-scale.Firstly, we have proposed and demonstrated a new approach towards the full vector determination of the spontaneous polarization of single ferroelectric nano-crystals used as SHG nano-probes. This method allows to remove the ambiguity inherent to earlier polarization-resolved SHG microscopy experiments, and has permitted full determination of the orientation of single domain ferroelectric nano-crystals. The electrooptic phase response obtained in the form of phase images and polarization diagrams yields the full orientation in the laboratory frame of randomly dispersed single nano-crystals, together with their electric polarization dipole. The complete vector determination of the dipole orientation is a prerequisite to important applications including ferroelectric nano-domain orientation, membrane potential imaging and rotation dynamics of single biomolecules, especially by using a new low-cost non-invasive imaging method with a low intensity illumination beam.The ferroelectric domain pattern of periodically poled KTiOPO4 and of a two-dimensional decagonal quasi-periodic LiNbO3 nonlinear crystal was determined by local measurement of their electro-optically induced phase retardation. Owing to the sign reversal of the electrooptic coefficients upon domain inversion, a 180 degree (pi) phase shift is observed across domain barriers between domains with opposed orientations. PLEOM allows to reveal the nonlinear and electrooptic spatially modulated patterns in ferroelectric crystals in a non-destructive manner and to determine their poling period, duty cycle and short-range order as well as to detect local defects in the domain structure, such due to incomplete poling.In addition, we have also proposed and demonstrated a new method, based on the voltage dependence of the electrooptic dephasing, to mimic the membrane potential in cells, working at this stage on nonlinear dye containing phospholipidic membranes, grown in a microfluidic set-up.