Microstructure of epitaxial thin films of the ferromagnetic shape memory alloy Ni 2 MnGa

Gegenstand dieser Arbeit ist die Präparation und die ausführliche Charakterisierung epitaktischer Dünnschicht-Proben der Heusler Verbindung Ni2MnGa. Diese intermetallische Verbindung zeigt einen magnetischen Formgedächtnis-Effekt (MFG), der sowohl im Bezug auf mögliche Anwendungen, als auch im Kontext der Grundlagenforschung äußerst interessant ist. In Einkristallen nahe der Stöchiometrie Ni2MnGa wurden riesige magnetfeldinduzierte Dehnungen von bis zu 10 % nachgewiesen. Der zugrundeliegende Mechanismus basiert auf einer Umverteilung von kristallographischen Zwillings-Varianten, die eine tetragonale oder orthorhombische Symmetrie besitzen. Unter dem Einfluss des Magnetfeldes bewegen sich die Zwillingsgrenzen durch den Kristall, was eine makroskopische Formänderung mit sich bringt. Die somit erzeugten reversiblen Längenänderungen können mit hoher Frequenz geschaltet werden, was Ni2MnGa zu einem vielversprechenden Aktuatorwerkstoff macht. rnDa der Effekt auf einem intrinsischen Prozess beruht, eignen sich Bauteile aus MFG Legierungen zur Integration in Mikrosystemen (z.B. im Bereich der Mikrofluidik). rnrnBislang konnten große magnetfeldinduzierte Dehnungen nur für Einkristalle und Polykristalle mit hoher Porosität („foams") nachgewiesen werden. Um den Effekt für Anwendungen nutzbar zu machen, werden allerdings Konzepte zur Miniaturisierung benötigt. Eine Möglichkeit bieten epitaktische dünne Filme, die im Rahmen dieser Arbeit hergestellt und untersucht werden sollen. Im Fokus stehen dabei die Optimierung der Herstellungsparameter, sowie die Präparation von freitragenden Schichten. Zudem werden verschiedene Konzepte zur Herstellung freistehender Mikrostrukturen erprobt. Mittels Röntgendiffraktometrie konnte die komplizierte Kristallstruktur für verschiedene Wachstumsrichtungen verstanden und die genaue Verteilung der Zwillingsvarianten aufgedeckt werden. In Verbindung mit Mikroskopie-Methoden konnte so die Zwillingsstruktur auf verschiedenen Längenskalen geklärt werden. Die Ergebnisse erklären das Ausbleiben des MFG Effekts in den Proben mit (100) Orientierung. Andererseits wurde für Schichten mit (110) Wachstum eine vielversprechende Mikrostruktur entdeckt, die einen guten Ausgangspunkt für weitere Untersuchungen bietet.rnDurch die spezielle Geometrie der Proben war es möglich, Spektroskopie-Experimente in Transmission durchzuführen. Die Ergebnisse stellen den ersten experimentellen Nachweis der Änderungen in der elektronischen Struktur einer metallischen Verbindung während des martensitischen Phasenübergangs dar. Durch Messen des magnetischen Zirkulardichroismus in der Röntgenabsorption konnten quantitative Aussagen über die magnetischen Momente von Ni und Mn getroffen werden. Die Methode erlaubt überdies die Beiträge von Spin- und Bahn-Moment separat zu bestimmen. Durch winkelabhängige Messungen gelang es, die mikroskopische Ursache der magnetischen Anisotropie aufzuklären. Diese Ergebnisse tragen wesentlich zum Verständnis der komplexen magnetischen und strukturellen Eigenschaften von Ni2MnGa bei.rn

A new microbiopsy system enables rapid preparation of tissue for high-pressure freezing

A microbiopsy system was developed to overcome long sampling times for tissues before they are cryo-fixed by high-pressure freezing. A commercially available biopsy gun was adapted to the needs of small-organ excisions, and biopsy needles were modified to allow small samples (0.6 mm x 1.2 mm x 0.3 mm) to be taken. Specimen platelets with a central slot of the same dimensions as the biopsy are used. A self-made transfer device (in the meantime optimized by Leica-Microsystems [Vienna, Austria]) coordinates the transfer of the excised sample from the biopsy needle into the platelet slot and the subsequent loading in a specimen holder, which is then introduced into a high-pressure freezer (Leica EM PACT; Leica Microsystems, Vienna, Austria). Thirty seconds preparation time is needed from excision until high-pressure freezing. Brain, liver, kidney and muscle excisions of anesthetised rats are shown to be well frozen.

Localized annealing of polysilicon microstructures by inductively heated ferromagnetic films

The monolithic integration of dissimilar microsystems is often limited by conflicts in thermal budget. One of the most prevalent examples is the fabrication of active micro-electromechanical systems (MEMS), as structural films utilized for surface micromachining such as polysilicon typically require processing at temperatures unsuitable for microelectronic circuitry. A localized annealing process could provide for the post-deposition heat treatment of integrated structures without compromising active devices. This dissertation presents a new microfabrication technology based on the inductive heating of ferromagnetic films patterned to define regions for heat treatment. Support is provided through theory, finite-element modeling, and experimentation, concluding with the demonstration of inductive annealing on polysilicon inertial sensing structures. Though still in its infancy, the results confirm the technology to be a viable option for integrated MEMS as well as any microsystem fabrication process requiring a thermal gradient.

Two-Phase Flow In Microchannels: Morphology And Interface Phenomena

The existence and morphology, as well as the dynamics of micro-scale gas-liquid interfaces is investigated numerically and experimentally. These studies can be used to assess liquid management issues in microsystems such as PEMFC gas flow channels, and are meant to open new research perspectives in two-phase flow, particularly in film deposition on non-wetting surfaces. For example the critical plug volume data can be used to deliver desired length plugs, or to determine the plug formation frequency. The dynamics of gas-liquid interfaces, of interest for applications involving small passages (e.g. heat exchangers, phase separators and filtration systems), was investigated using high-speed microscopy - a method that also proved useful for the study of film deposition processes. The existence limit for a liquid plug forming in a mixed wetting channel is determined by numerical simulations using Surface Evolver. The plug model simulate actual conditions in the gas flow channels of PEM fuel cells, the wetting of the gas diffusion layer (GDL) side of the channel being different from the wetting of the bipolar plate walls. The minimum plug volume, denoted as critical volume is computed for a series of GDL and bipolar plate wetting properties. Critical volume data is meant to assist in the water management of PEMFC, when corroborated with experimental data. The effect of cross section geometry is assessed by computing the critical volume in square and trapezoidal channels. Droplet simulations show that water can be passively removed from the GDL surface towards the bipolar plate if we take advantage on differing wetting properties between the two surfaces, to possibly avoid the gas transport blockage through the GDL. High speed microscopy was employed in two-phase and film deposition experiments with water in round and square capillary tubes. Periodic interface destabilization was observed and the existence of compression waves in the gas phase is discussed by taking into consideration a naturally occurring convergent-divergent nozzle formed by the flowing liquid phase. The effect of channel geometry and wetting properties was investigated through two-phase water-air flow in square and round microchannels, having three static contact angles of 20, 80 and 105 degrees. Four different flow regimes are observed for a fixed flow rate, this being thought to be caused by the wetting behavior of liquid flowing in the corners as well as the liquid film stability. Film deposition experiments in wetting and non-wetting round microchannels show that a thicker film is deposited for wetting conditions departing from the ideal 0 degrees contact angle. A film thickness dependence with the contact angle theta as well as the Capillary number, in the form h_R ~ Ca^(2/3)/ cos(theta) is inferred from scaling arguments, for contact angles smaller than 36 degrees. Non-wetting film deposition experiments reveal that a film significantly thicker than the wetting Bretherton film is deposited. A hydraulic jump occurs if critical conditions are met, as given by a proposed nondimensional parameter similar to the Froude number. Film thickness correlations are also found by matching the measured and the proposed velocity derived in the shock theory. The surface wetting as well as the presence of the shock cause morphological changes in the Taylor bubble flow.

A rapid microbiopsy system to improve the preservation of biological samples prior to high-pressure freezing

A microbiopsy system for fast excision and transfer of biological specimens from donor to high-pressure freezer was developed. With a modified, commercially available, Promag 1.2 biopsy gun, tissue samples can be excised with a size small enough (0.6 mm x 1.2 mm x 0.3 mm) to be easily transferred into a newly designed specimen platelet. A self-made transfer unit allows fast transfer of the specimen from the needle into the specimen platelet. The platelet is then fixed in a commercially available specimen holder of a high-pressure freezing machine (EM PACT, Leica Microsystems, Vienna, Austria) and frozen therein. The time required by a well-instructed (but not experienced) person to execute all steps is in the range of half a minute. This period is considered short enough to maintain the excised tissue pieces close to their native state. We show that a range of animal tissues (liver, brain, kidney and muscle) are well preserved. To prove the quality of freezing achieved with the system, we show vitrified ivy leaves high-pressure frozen in the new specimen platelet.

Dielectrophoresis-based analyte separation and analysis

Dielectrophoresis—the tendency of a material of high dielectric permittivity to migrate in an electrical field gradient to a region of maximum field strength—provides an ideal motive force for manipulating small volumes of biological analytes in microfluidic microsystems. The work described in this thesis was based on the hypothesis that dielectrophoresis could be exploited to provide high-resolution cell separations in microsystems as well as a means for the electrically-controllable manipulation of solid supports for molecular analysis. To this end, a dielectrophoretic/gravitational field-flow-fractionation (DEP/G-FFF) system was developed and the separation performance evaluated using various types and sizes of polystyrene microspheres as model particles. It was shown that separation of the polystyrene beads was based on the differences in their effective dielectrophoretic properties. The ability of an improved DEP/G-FFF system to separate genetically identical, but phenotypically dissimilar cell types was demonstrated using mixtures of 6m2 mutant rat kidney cells grown under transforming and non-transforming culture conditions. Additionally, a panel of engineered dielectric microspheres was designed with specific, predetermined dielectrophoretic properties such that their dielectrophoretic behaviors would be controllable and predictable. The fabrication method involved the use of gold-coated polystyrene microsphere cores coated with a self-assembled monolayer of alkanethiol and, optionally, a self-assembled monolayer of phospholipid to form a thin-insulating-shell-over-conductive-interior structure. The successful development of the DEP/G-FFF separation system and the dielectrically engineered microspheres provides proof-of-principle demonstrations of enabling dielectrophoresis-based microsystem technology that should provide powerful new methods for the manipulation, separation and identification of analytes in many diverse fields. ^