Tailoring Magnetic Properties of Co-Fe Thin Films by Topographical Modifications Using Thermal Annealing and Swift Heavy Ion Irradiation and Fabrication of Magnetoelectric Multilayers for Device Applications

Magnetism and magnetic materials have been playing a lead role in improving the quality of life. They are increasingly being used in a wide variety of applications ranging from compasses to modern technological devices. Metallic glasses occupy an important position among magnetic materials. They assume importance both from a scientific and an application point of view since they represent an amorphous form of condensed matter with significant deviation from thermodynamic equilibrium. Metallic glasses having good soft magnetic properties are widely used in tape recorder heads, cores of high-power transformers and metallic shields. Superconducting metallic glasses are being used to produce high magnetic fields and magnetic levitation effect. Upon heat treatment, they undergo structural relaxation leading to subtle rearrangements of constituent atoms. This leads to densification of amorphous phase and subsequent nanocrystallisation. The short-range structural relaxation phenomenon gives rise to significant variations in physical, mechanical and magnetic properties. Magnetic amorphous alloys of Co-Fe exhibit excellent soft magnetic properties which make them promising candidates for applications as transformer cores, sensors, and actuators. With the advent of microminiaturization and nanotechnology, thin film forms of these alloys are sought after for soft under layers for perpendicular recording media. The thin film forms of these alloys can also be used for fabrication of magnetic micro electro mechanical systems (magnetic MEMS). In bulk, they are drawn in the form of ribbons, often by melt spinning. The main constituents of these alloys are Co, Fe, Ni, Si, Mo and B. Mo acts as the grain growth inhibitor and Si and B facilitate the amorphous nature in the alloy structure. The ferromagnetic phases such as Co-Fe and Fe-Ni in the alloy composition determine the soft magnetic properties. The grain correlation length, a measure of the grain size, often determines the soft magnetic properties of these alloys. Amorphous alloys could be restructured in to their nanocrystalline counterparts by different techniques. The structure of nanocrystalline material consists of nanosized ferromagnetic crystallites embedded in an amorphous matrix. When the amorphous phase is ferromagnetic, they facilitate exchange coupling between nanocrystallites. This exchange coupling results in the vanishing of magnetocrystalline anisotropy which improves the soft magnetic properties. From a fundamental perspective, exchange correlation length and grain size are the deciding factors that determine the magnetic properties of these nanocrystalline materials. In thin films, surfaces and interfaces predominantly decides the bulk property and hence tailoring the surface roughness and morphology of the film could result in modified magnetic properties. Surface modifications can be achieved by thermal annealing at various temperatures. Ion irradiation is an alternative tool to modify the surface/structural properties. The surface evolution of a thin film under swift heavy ion (SHI) irradiation is an outcome of different competing mechanism. It could be sputtering induced by SHI followed by surface roughening process and the material transport induced smoothening process. The impingement of ions with different fluence on the alloy is bound to produce systematic microstructural changes and this could effectively be used for tailoring magnetic parameters namely coercivity, saturation magnetization, magnetic permeability and remanence of these materials. Swift heavy ion irradiation is a novel and an ingenious tool for surface modification which eventually will lead to changes in the bulk as well as surface magnetic property. SHI has been widely used as a method for the creation of latent tracks in thin films. The bombardment of SHI modifies the surfaces or interfaces or creates defects, which induces strain in the film. These changes will have profound influence on the magnetic anisotropy and the magnetisation of the specimen. Thus inducing structural and morphological changes by thermal annealing and swift heavy ion irradiation, which in turn induce changes in the magnetic properties of these alloys, is one of the motivation of this study. Multiferroic and magneto-electrics is a class of functional materials with wide application potential and are of great interest to material scientists and engineers. Magnetoelectric materials combine both magnetic as well as ferroelectric properties in a single specimen. The dielectric properties of such materials can be controlled by the application of an external magnetic field and the magnetic properties by an electric field. Composites with magnetic and piezo/ferroelectric individual phases are found to have strong magnetoelectric (ME) response at room temperature and hence are preferred to single phasic multiferroic materials. Currently research in this class of materials is towards optimization of the ME coupling by tailoring the piezoelectric and magnetostrictive properties of the two individual components of ME composites. The magnetoelectric coupling constant (MECC) (_ ME) is the parameter that decides the extent of interdependence of magnetic and electric response of the composite structure. Extensive investigates have been carried out in bulk composites possessing on giant ME coupling. These materials are fabricated by either gluing the individual components to each other or mixing the magnetic material to a piezoelectric matrix. The most extensively investigated material combinations are Lead Zirconate Titanate (PZT) or Lead Magnesium Niobate-Lead Titanate (PMNPT) as the piezoelectric, and Terfenol-D as the magnetostrictive phase and the coupling is measured in different configurations like transverse, longitudinal and inplane longitudinal. Fabrication of a lead free multiferroic composite with a strong ME response is the need of the hour from a device application point of view. The multilayer structure is expected to be far superior to bulk composites in terms of ME coupling since the piezoelectric (PE) layer can easily be poled electrically to enhance the piezoelectricity and hence the ME effect. The giant magnetostriction reported in the Co-Fe thin films makes it an ideal candidate for the ferromagnetic component and BaTiO3 which is a well known ferroelectric material with improved piezoelectric properties as the ferroelectric component. The multilayer structure of BaTiO3- CoFe- BaTiO3 is an ideal system to understand the underlying fundamental physics behind the ME coupling mechanism. Giant magnetoelectric coupling coefficient is anticipated for these multilayer structures of BaTiO3-CoFe-BaTiO3. This makes it an ideal candidate for cantilever applications in magnetic MEMS/NEMS devices. SrTiO3 is an incipient ferroelectric material which is paraelectric up to 0K in its pure unstressed form. Recently few studies showed that ferroelectricity can be induced by application of stress or by chemical / isotopic substitution. The search for room temperature magnetoelectric coupling in SrTiO3-CoFe-SrTiO3 multilayer structures is of fundamental interest. Yet another motivation of the present work is to fabricate multilayer structures consisting of CoFe/ BaTiO3 and CoFe/ SrTiO3 for possible giant ME coupling coefficient (MECC) values. These are lead free and hence promising candidates for MEMS applications. The elucidation of mechanism for the giant MECC also will be the part of the objective of this investigation.

Characterization of Novel Fabry Pérot Filter Arrays for Nanospectrometers in Medical Applications

Optische Spektroskopie ist eine sehr wichtige Messtechnik mit einem hohen Potential für zahlreiche Anwendungen in der Industrie und Wissenschaft. Kostengünstige und miniaturisierte Spektrometer z.B. werden besonders für moderne Sensorsysteme “smart personal environments” benötigt, die vor allem in der Energietechnik, Messtechnik, Sicherheitstechnik (safety and security), IT und Medizintechnik verwendet werden. Unter allen miniaturisierten Spektrometern ist eines der attraktivsten Miniaturisierungsverfahren das Fabry Pérot Filter. Bei diesem Verfahren kann die Kombination von einem Fabry Pérot (FP) Filterarray und einem Detektorarray als Mikrospektrometer funktionieren. Jeder Detektor entspricht einem einzelnen Filter, um ein sehr schmales Band von Wellenlängen, die durch das Filter durchgelassen werden, zu detektieren. Ein Array von FP-Filter wird eingesetzt, bei dem jeder Filter eine unterschiedliche spektrale Filterlinie auswählt. Die spektrale Position jedes Bandes der Wellenlänge wird durch die einzelnen Kavitätshöhe des Filters definiert. Die Arrays wurden mit Filtergrößen, die nur durch die Array-Dimension der einzelnen Detektoren begrenzt werden, entwickelt. Allerdings erfordern die bestehenden Fabry Pérot Filter-Mikrospektrometer komplizierte Fertigungsschritte für die Strukturierung der 3D-Filter-Kavitäten mit unterschiedlichen Höhen, die nicht kosteneffizient für eine industrielle Fertigung sind. Um die Kosten bei Aufrechterhaltung der herausragenden Vorteile der FP-Filter-Struktur zu reduzieren, wird eine neue Methode zur Herstellung der miniaturisierten FP-Filtern mittels NanoImprint Technologie entwickelt und präsentiert. In diesem Fall werden die mehreren Kavitäten-Herstellungsschritte durch einen einzigen Schritt ersetzt, die hohe vertikale Auflösung der 3D NanoImprint Technologie verwendet. Seit dem die NanoImprint Technologie verwendet wird, wird das auf FP Filters basierende miniaturisierte Spectrometer nanospectrometer genannt. Ein statischer Nano-Spektrometer besteht aus einem statischen FP-Filterarray auf einem Detektorarray (siehe Abb. 1). Jeder FP-Filter im Array besteht aus dem unteren Distributed Bragg Reflector (DBR), einer Resonanz-Kavität und einen oberen DBR. Der obere und untere DBR sind identisch und bestehen aus periodisch abwechselnden dünnen dielektrischen Schichten von Materialien mit hohem und niedrigem Brechungsindex. Die optischen Schichten jeder dielektrischen Dünnfilmschicht, die in dem DBR enthalten sind, entsprechen einen Viertel der Design-Wellenlänge. Jeder FP-Filter wird einer definierten Fläche des Detektorarrays zugeordnet. Dieser Bereich kann aus einzelnen Detektorelementen oder deren Gruppen enthalten. Daher werden die Seitenkanal-Geometrien der Kavität aufgebaut, die dem Detektor entsprechen. Die seitlichen und vertikalen Dimensionen der Kavität werden genau durch 3D NanoImprint Technologie aufgebaut. Die Kavitäten haben Unterschiede von wenigem Nanometer in der vertikalen Richtung. Die Präzision der Kavität in der vertikalen Richtung ist ein wichtiger Faktor, der die Genauigkeit der spektralen Position und Durchlässigkeit des Filters Transmissionslinie beeinflusst.

Fabrication of diamond nanostructures and investigation of the imbedded NV centers

Diamant ist ein Material mit vielen außerordentlichen Eigenschaften, die ihn zu einem äußerst vielversprechenden Kandidaten für Anwendungen in Wissen-schaft und Technik machen. In den letzten Jahren wurde Diamant häufig als einzigartige Plattform für neue Anwendungen beispielsweise in der Quanteninformationstechnologie (QIT) oder in der Magnetometrie im Nanometermaßstab eingesetzt, wobei einer der wichtigsten lumineszierenden Gitterdefekte im Diamantgitter eingesetzt wird. Dabei handelt es sich um die sogenannten Stickstoff/Fehlenstellen-Farbzentren (NV-Zentren), die im sichtbaren Bereich mit einer absoluten Photostabilität bei Raumtemperatur emittieren. In dieser Arbeit wurden NV-Zentren in Diamantnanokristalliten und –nanosäulen untersucht, die während des Wachstumsprozesses erzeugt wurden. Einzelne Diamantnanokristallite und nanokristalline Diamantschichten (NCD), aus denen Nanosäulen geätzt wurden, wurden mithilfe der Hot Filament Chemical Vapour Deposition (HFCVD) abgeschieden. Zu Vergleichszwecken wurden auch ultrananokristalline Diamantschichten (UNCD) mittels Mikrowellen-CVD (MWCVD) hergestellt. Die Filme wurden sorgfältig in Bezug auf ihre Morphologie, kristallinen Eigenschaften und Zusammensetzung untersucht. Um die Möglichkeit einer Integration dieser Diamantschichten mit temperaturempfindlichen Materialien wie III/V-Halbleitern, Metallen mit niedrigem Schmelzpunkt oder Polymeren zu untersuchen, wurde der Einfluss der Substrattemperatur ermittelt. Eindimensionale NCD- und UNCD-Diamantnanostrukturen wurden mithilfe der Elektronenstrahllithographie (EBL) und reaktivem Ionenätzen in einem induktiv gekoppelten O2-Plasma (ICP-RIE) hergestellt. Zur Vorbereitung wurden zunächst die Ätzraten in Abhängigkeit von den vier wichtigsten Parametern ermittelt. Weitere Erkenntnisse über die Ätzmechanismen wurden durch Ätzexperiment mit unstrukturierten NCD- und UNCD-Schichten erhalten Mittels der EBL konnten mithilfe von Gold-Ätzmasken Nanosäulen mit Durchmessern von 50 nm bis zu 1 μm hergestellt werden.Eine optische Charakterisierung der NCD- und UNCD-Nanosäulen erfolgte mithilfe von Fluorenzenz-Mapping und Photomumineszenz-Spektroskopie. Diese Messungen ergaben, dass in beiden Arten von Säulen NV-Zentren vorhanden sind. Allerdings wurden nur in NCD-Säulen die gewünschten NV--Zentren gefunden, in UNCD-Säulen hingegen nur NV0-Zentren.

Optimization in the Technological Steps for the Fabrication of Large Area Micromirror Arrays

Micromirror arrays are a very strong candidate for future energy saving applications. Within this work, the fabrication process for these micromirror arrays has been optimized and some steps for the large area fabrication of micromirror modules were performed. At first the surface roughness of the insulation layer of silicon dioxide (SiO2) was investigated. This SiO2 thin layer was deposited on three different type of substrates i.e. silicon, glass and Polyethylene Naphthalate (PEN) substrates. The deposition techniques which has been used are Plasma Enhanced Chemical Vapor Deposition (PECVD), Physical Vapor Deposition (PVD) and Ion Beam Sputter Deposition (IBSD). The thickness of the SiO2 thin layer was kept constant at 150nm for each deposition process. The surface roughness was measured by Stylus Profilometry and Atomic Force Microscopy (AFM). It was found that the layer which was deposited by IBSD has got the minimum surface roughness value and the layer which was deposited by PECVD process has the highest surface roughness value. During the same investigation, the substrate temperature of PECVD was varied from 80° C to 300° C with the step size of 40° C and it was found that the surface roughness keeps on increasing as the substrate holder temperature increases in the PECVD process. A new insulation layer system was proposed to minimize the dielectric breakdown effect in insulation layer for micromirror arrays. The conventional bilayer system was replaced by five layer system but the total thickness of insulation layer remains the same. It was found that during the actuation of micromirror arrays structure, the dielectric breakdown effect was reduced considerably as compared to the bilayer system. In the second step the fabrication process of the micromirror arrays was successfully adapted and transferred from glass substrates to the flexible PEN substrates by optimizing the conventional process recipe. In the last section, a large module of micromirror arrays was fabricated by electrically interconnecting four 10cm×10cm micromirror modules on a glass pane having dimensions of 21cm×21cm.

Micro-layered-photolithography for Micro-Fabrication and Micro-Molding

A novel process based on the principle of layered photolithography has been proposed and tested for making real three-dimensional micro-structures. An experimental setup was designed and built for doing experiments on this micro-fabrication process. An ultraviolet (UV) excimer laser at the wavelength of 248 nm was used as the light source and a single piece of photo-mask carrying a series of two dimensional (2D) patterns sliced from a three dimensional (3D) micro-part was employed for the photolithography process. The experiments were conducted on the solidification of liquid photopolymer from single layer to multiple layers. The single-layer photolithography experiments showed that certain photopolymers could be applied for the 3D micro-fabrication, and solid layers with sharp shapes could be formed from the liquid polymer identified. By using a unique alignment technique, multiple layers of photolithography was successfully realized for a micro-gear with features at 60 microns. Electroforming was also conducted for converting the photopolymer master to a metal cavity of the micro-gear, which proved that the process is feasible for micro-molding.

On the Fabrication of Microparticles Using Electrohydrodynamic Atomization Method

A new approach for the control of the size of particles fabricated using the Electrohydrodynamic Atomization (EHDA) method is being developed. In short, the EHDA process produces solution droplets in a controlled manner, and as the solvent evaporates from the surface of the droplets, polymeric particles are formed. By varying the voltage applied, the size of the droplets can be changed, and consequently, the size of the particles can also be controlled. By using both a nozzle electrode and a ring electrode placed axisymmetrically and slightly above the nozzle electrode, we are able to produce a Single Taylor Cone Single Jet for a wide range of voltages, contrary to just using a single nozzle electrode where the range of permissible voltage for the creation of the Single Taylor Cone Single Jet is usually very small. Phase Doppler Particle Analyzer (PDPA) test results have shown that the droplet size increases with increasing voltage applied. This trend is predicted by the electrohydrodynamic theory of the Single Taylor Cone Single Jet based on a perfect dielectric fluid model. Particles fabricated using different voltages do not show much change in the particles size, and this may be attributed to the solvent evaporation process. Nevertheless, these preliminary results do show that this method has the potential of providing us with a way of fine controlling the particles size using relatively simple method with trends predictable by existing theories.

Fabrication of Controlled Release Devices Using Supercritical Antisolvent Method

In this study, the supercritical antisolvent with enhanced mass transfer method (SASEM) is used to fabricate micro and nanoparticles of biocompatible and biodegradable polymer PLGA (poly DL lactide co glycolic acid). This process may be extended to the encapsulation of drugs in these micro and nanoparticles for controlled release purposes. Conventional supercritical antisolvent (SAS) process involves spraying a solution (organic solvent + dissolved polymer) into supercritical fluid (CO[subscript 2]), which acts as an antisolvent. The high rate of mass transfer between organic solvent and supercritical CO[subscript 2] results in supersaturation of the polymer in the spray droplet and precipitation of the polymer as micro or nanoparticles occurs. In the SASEM method, ultrasonic vibration is used to atomize the solution entering the high pressure with supercritical CO[subscript 2]. At the same time, the ultrasonic vibration generated turbulence in the high pressure vessel, leading to better mass transfer between the organic solvent and the supercritical CO₂. In this study, two organic solvents, acetone and dichloromethane (DCM) were used in the SASEM process. Phase Doppler Particle Analyzer (PDPA) was used to study the ultrasonic atomization of liquid using the ultrasonic probe for the SASEM process. Scanning Electron Microscopy (SEM) was used to study the size and morphology of the polymer particles collected at the end of the process.

Microstructure and magnetic properties of Ni50 Mn37 Sn13 Heusler alloy ribbons

The Heusler alloy Ni50 Mn37 Sn13 was successfully produced as ribbon flakes of thickness around 7-10 μm melt spinning. Fracture cross section micrographs in the ribbon show the formation of a microcrystalline columnarlike microstructure, with their longer axes perpendicular to the ribbon plane. Phase transition temperatures of the martensite-austenite transformation were found to be MS =218 K, Mf =207 K, AS =224 K, and Af =232 K; the thermal hysteresis of the transformation is 15 K. Ferromagnetic L 21 bcc austenite phase shows a Curie point of 313 K, with cell parameter a=0.5971 (5) nm at 298 K, transforming into a modulated 7M orthorhombic martensite with a=0.6121 (7) nm, b=0.6058 (8) nm, and c=0.5660 (2) nm, at 150 K

Numerical model of solid phase transformations governed by nucleation and growth: microstructure development during isothermal crystallization

A simple numerical model which calculates the kinetics of crystallization involving randomly distributed nucleation and isotropic growth is presented. The model can be applied to different thermal histories and no restrictions are imposed on the time and the temperature dependences of the nucleation and growth rates. We also develop an algorithm which evaluates the corresponding emerging grain-size distribution. The algorithm is easy to implement and particularly flexible, making it possible to simulate several experimental conditions. Its simplicity and minimal computer requirements allow high accuracy for two- and three-dimensional growth simulations. The algorithm is applied to explore the grain morphology development during isothermal treatments for several nucleation regimes. In particular, thermal nucleation, preexisting nuclei, and the combination of both nucleation mechanisms are analyzed. For the first two cases, the universal grain-size distribution is obtained. The high accuracy of the model is stated from its comparison to analytical predictions. Finally, the validity of the Kolmogorov-Johnson-Mehl-Avrami model SSSR, is verified for all the cases studied

Signal processing of microstructure profiles: integrating turbulent spatial scales in aquatic ecological modeling

The main objective of this thesis was the integration of microstructure information in synoptic descriptors of turbulence, that reflects the mixing processes. Turbulent patches are intermittent in space and time, but they represent the dominant process for mixing. In this work, the properties of turbulent patches were considered the potential input for integrating the physical microscale measurements. The development of a method for integrating the properties of the turbulent patches required solving three main questions: a) how can we detect the turbulent patches from he microstructure measurements?; b) which are the most relevant properties of the turbulent patches?; and ) once an interval of time has been selected, what kind of synoptic parameters could better reflect the occurrence and properties of the turbulent patches? The answers to these questions were the final specific objectives of this thesis.

Spontaneous otoacoustic emissions in a chinchilla: audiometric correlates as seen in audiogram microstructure

This paper reviews a study to evaluate the audiogram microstructure of a chinchilla with a documented spontaneous otoacoustic emission.

Influence of molecular composition on the development of microstructure from sheared polyethylene melts: Molecular and lamellar templating

A combination of in situ and ex situ X-ray scattering techniques and transmission electron microscopy has been used to study the crystallization behaviour of polyethylene, following the imposition of melt shear. In the case of a branched material, the imposition of shear flow up to a rate of 30 s(-1) was found to induce no anisotropy. Although shearing the linear material only ever induced a very small degree of anisotropy in the melt, for shear rates > 0.15 s(-1), subsequent crystallization resulted in increasing anisotropy. Blends of the above two polyethylenes were produced, in which the linear material constituted the minority fraction (similar to 10%). Isothermal crystallization at temperatures where extensive crystallization of the branched material does not occur demonstrated that the behaviour of the linear component of the sheared blend mirrored that of the linear polyethylene alone. However, in addition, it was found that when crystallized in the presence of an oriented morphology, the branched polymer also formed anisotropic structures. We have termed the process templating, in which the crystallization behaviour of the bulk of the system (similar to 90% branched material) is completely altered (spherulitic to oriented lamellar) by mapping it onto a pre-existing minority structure (similar to 10% linear polymer). (c) 2006 Elsevier Ltd. All rights reserved.

Electrochemical fabrication and electrocatalytic properties of nanostructured mesoporous platinum microelectrodes

Electrodeposition from a lyotropic liquid crystal template medium was used to produce nanostructured platinum microelectrodes with high specific surface area and high mass transport efficiency. Compared to polished and conventional platinized microelectrodes, well-ordered nanostructured platinum microelectrodes exhibited enhanced electrocatalytic properties for oxygen and ascorbic acid, whilst well-ordered nanostructured platinum microelectrodes offered improved electrocatalytic properties for oxygen reduction compared to disordered nanostructured platinum microelectrodes.