Imaging of current in internal conductors through magnetic field detection by magnetic force microscopy (MFM) is of growing interest in the analysis of integrated circuits (ICs). This thesis presents a systematic study of the MFM based mapping of current in model circuits by using force and force gradient techniques. In comparing these two techniques, force was found to have a much higher signal to noise ratio (from ~150 to ~580 times) than force gradient at large tip-sample distances considering the presence of thick overlayers in ICs. As a result, force will have better sensitivity and can therefore be used to detect much smaller minimum currents. We have achieved a sensitivity of ~0.64 µA per square-root Hertz in air and ~0.095 µA per squre-root Hertz in vacuum for force with a pinning field with a probe-circuit separation of 1.0 µm. We conclude that the force technique is superior for the application of MFM current imaging of buried conductors, albeit with reduced spatial resolution. Numerical modeling of the MFM images has shown that the simple point probe approximation is insufficient to model MFM images. An extended model, which considers realistic MFM probe geometries and the forces acting on the whole probe, has been shown to be necessary. Qualitative and quantitative comparisons of the experimental and simulation results with this model are in agreement to within experimental uncertainty. The comparisons suggested that the CoCr film thickness is not uniform on the probe, which was verified by scanning electron microscope cross-section images of the probes cut by a focused ion beam. Most notably, the CoCr film was 1.5 times thicker on the cantilever than on the tip. Based on the simulation and experimental results, we have devised a method to accurately locate the current path from MFM images with submicrometer uncertainty. The method was tested for different patterns of model conducting lines. It was shown to be a useful technique for fault location in IC failure analysis when current flows through the devices buried under overlayers and no topographic features are on the surface to provide clues about the positions of the devices.

Im Rahmen der Dissertation wurde das Phänomen der Wechselwirkungsdomänen sowohl experimentell als auch unter Zuhilfenahme mikromagnetischer Simulationen untersucht. Gegenstand der Untersuchungen waren einphasige NdFeB-Magnete, die durch Heißpressen und anschließender Warmumformung hergestellt wurden. Zusätzlich wurden über den gleichen Herstellungsweg Kompositproben aus NdFeB und Fe mit unterschiedlichen Partikelausgangsgrößen erhalten und studiert. Korrelationsuntersuchungen verschiedener Messmethoden haben gezeigt, dass im thermisch entmagnetisierten Zustand die Grenzen der Wechselwirkungsdomänen an der Oberfläche größtenteils entlang von Korngrenzen verlaufen. Mittels in-situ MFM wurden erstmalig Untersuchungen von Wechselwirkungsdomänen an massiven NdFeB-Magneten im Magnetfeld durchgeführt. Die Ummagnetisierung erfolgt dabei über die Bewegung der Domänengrenze durch schrittweises Wandern von einer Korngrenze zur benachbarten. Die Beweglichkeit der Domänengrenzen ist durch das Haften an den Korngrenzen gehemmt, was sich in der geringeren Suszeptibilität der warmumgeformten Magnete im Vergleich zu Sintermagneten bemerkbar macht. Aufgrund der eingestellten Mikrostruktur in den warmumgeformten Magneten kann folglich gesagt werden, dass die Ummagnetisierungsprozesse sowohl Merkmale von klassischen Nukleations-, als auch von klassischen Pinningmagneten aufweisen. Mit Hilfe von mikromagnetischen Simulationen konnte eine Eindomänenteilchengröße prismatischer Partikel mit quadratischer Grundfläche ermittelt werden. Außerdem konnte gezeigt werden, dass der Winkel des Streufeldvektors eine entscheidende Rolle bei Ummagnetisiserungsprozessen in solchen Partikeln spielt. Die Superposition des Streufeldvektors mit dem Vektor des angelegten Feldes führt zu einem Gesamtfeldvektor, dessen Winkelabhängigkeit ein Stoner-Wohlfarth ähnliches Verhalten zeigt.

Iron filled carbon nanotubes (FeCNT) can be described as carbon nanotubes which contain an iron nanowire of several micrometers length and a diameter of approximately 10-100 nm. The carbon shells protect the iron core from oxidation and mechanical damage thus enabling a wide range of applications that require a long-term stability. The magnetic properties of the enclosed nanowire are in part determined by its small size and elongated shape. Magnetic force microscopy (MFM) measurements show that the iron wire exhibits a single domain behavior. Due to the large shape anisotropy it is magnetized along the long wire axis in the remanent state. Two magnetic monopoles of opposing polarity are located at the wire extremities. Depending on the structure and geometry of the individual nanowire, switching fields in the range of 100-400 mT can be found when the external field is applied along the FeCNT’s easy axis. Cantilever magnetometry shows that the switching can be attributed to a thermally assisted magnetization reversal mechanism with the nucleation and propagation of a domain wall. The defined magnetic properties of individual FeCNT combined with their mechanical strength make them ideal candidates for an application as high resolution high stability MFM probes. The fabrication of such probes can be achieved with the help of a micromanipulation setup in a scanning electron microscope. FeCNT MFM probes achieve a sub 25 nm lateral magnetic resolution. MFM measurements with FeCNT MFM probes in external fields show that the magnetization of these probes is exceptionally stable compared to conventional coated MFM probes. This greatly simplifies the data evaluation of such applied field MFM measurements. The emphasis of this work was put on the calibration of FeCNT probes to enable straightforward quantitative MFM measurements. The defined shape of the magnetically active iron nanowire allows an application of a point monopole description. Microscale parallel current carrying lines that produce a defined magnetic field are used as calibration structures to determine the effective magnetic moment of different MFM probes. The line geometry is varied in order to produce multiple magnetic field decay lengths and investigate the influence on the effective probe moment. The results show that while the effective magnetic monopole moment of a conventional MFM probe increases with an increasing sample stray field decay length, the effective moment of a FeCNT MFM probe remains constant. This enables a MFM probe calibration that stays valid for a large variety of magnetic samples. Furthermore, the fitted monopole moment of a FeCNT probe (in the order of 10E-9 Am) is consistent with the moment calculated from the nanowire geometry and the saturation magnetization of iron.

Made available in DSpace on 2016-04-18T21:39:49Z (GMT). No. of bitstreams: 2 Carolina Duca Novaes1.pdf: 3168515 bytes, checksum: 4bc2a4d21f8e08b61653940548fcd0d3 (MD5) Carolina Duca Novaes2.pdf: 2186508 bytes, checksum: 51278edae485082fdb365b9e34ad3fda (MD5) Previous issue date: 2010-02-10 / This dissertation presents details of a structure needed to create a Single Frequency Network (SFN) using low-power transmitters, and a comparison with a network composed of a single transmitter with high power. Among the difficulties to implement networks which distribute signals in SFN, has prioritized the synchronization issue and equalization techniques to achieve better performance of this system. Thus, there was a theoretical research comparing the different methods of timing of single frequency networks and simulations of coverage and performance in order to discuss the implementation of such a network system in the Brazilian digital TV (SBTVD). / Este trabalho apresenta um detalhamento da estrutura necessária para se criar uma rede Single Frequency Network (SFN) utilizando transmissores de baixa potência, bem como um comparativo com uma rede composta por um transmissor único de alta potência. Dentre as dificuldades de se implementar as redes de redistribuição de sinais em SFN foi priorizada a questão do sincronismo e técnicas de equalização que permitam um melhor desempenho desse sistema. Para isso foi realizada uma pesquisa teórica comparativa entre os diferentes métodos de sincronismo de redes de frequência única e simulações de cobertura e desempenho, visando discutir a implementação desse tipo de rede no sistema Brasileiro de TV digital (SBTVD).

Low-temperature magnetic force microscopy was used to study the phase diagram of a La1/3Pr1/3Ca1/3MnO3 thin film grown on a (110) NdGaO3 (NGO) substrate by pulsed laser deposition. Traditionally, one can observe the phase change at the nanoscale level as the sample is cooled from room temperature through the transition temperature to liquid nitrogen temperatures, but in this case a fixed voltage ranging from 0 V to 31 V was applied before each cooling cycle. From in and ex situ transport measurements, it is observed that the temperature of the peak of the transition increases with applied field; however, the MFM images show that the magnetic transition begins at a lower temperature with the same increase in field. Thus, this dissertation shows that a new voltage control exists for the phase transition in certain manganites. / text

Le couplage d'un métal ferromagnétique (MF) et d'un semiconducteur (SC) permettrait d'intégrer un nouveau degré de liberté - le spin - aux propriétés logiques et optiques des semiconducteurs. Cependant, l'élaboration de jonctions tunnel magnétiques (JTM) couplant ces deux types de matériaux (barrières MF/SC/MF) présente des difficultés majeures. En effet, à la température de croissance optimale de la barrière semiconductrice (∼580 ◦C), le métal de l'électrode inférieure diffuse à travers l'interface pour s'incorporer à la barrière et ainsi réduire les effets de magnétorésistance. Pour éviter l'interdiffusion, la barrière doit être élaborée à basse température. Ce procédé implique l'incorporation d'antisites d'As dans la barrière SC qui réduit, encore une fois, les effets magnétorésistifs. Le couple MnAs/GaAs est considéré comme un bon candidat pour la réalisation de jonction hybride MF/SC /MF à cause de la faible réactivité et de la forte polarisation à l'interface. Afin de faire croître des JTM de bonne qualité chimique et cristalline, nous avons étudié des jonctions tunnel originales où l'électrode inférieure est une couche de clusters de MnAs dans une matrice de GaAs (GaAs:MnAs). Cet électrode est couvert par une barrière de SC III-V et par une électrode supérieure composée par une couche continue de MnAs. Le protocole de croissance de l'électrode inférieure (recuit in situ d'une couche de GaMnAs à T>500řC) permet simultanément de recuire la barrière semiconductrice et d'augmenter considérablement la qualité structurale et chimique de la barrière. Ce travail a été réalisé en trois parties. Dans un premier temps, les conditions d'élaboration de couches de GaAs:MnAs/GaAs(001) et de MnAs/GaAs(001) ont été optimisées. Ensuite, nous avons mené des études originales de microscopie à gradient de force magnétique et de spectroscopie de photoémission (in situ et au synchrotron). Ces mesures ont permis de faire ressortir des informations pertinentes pour l'intégration de ces couches en tant qu'électrode magnétique pour l'électronique de spin. Enfin, une étude du transport tunnel polarisé en spin a été conduite sur des jonctions tunnel MnAs/SC III-V/GaAs:MnAs.

Zur Aufklärung der lokalen Magnetisierungs- und magnetischen Streufeldstruktur in ferromagnetischen und supraleitenden Materialien wurden magnetkraftmikroskopische (Magnetkraftmikroskopie-MFM) Untersuchungen durchgeführt und quantitativ ausgewertet. Für eine solch quantitative Auswertung muss der Einfluß der verwendeten MFM-Spitzen auf das MFM-Bild bestimmt und in geeigneter Weise subtrahiert werden. Hierzu wurden Spitzenkalibrierungsroutinen und ein Verfahren zur Entfaltung der gemessenen MFM-Daten implementiert, das auf der Wiener Dekonvolution basiert. Mit Hilfe dieser Prozedur können sowohl die räumliche Ausdehnung als auch die Größe der Streufelder direkt aus gemessenen MFM-Bildern bestimmt werden. Gezeigt wurde diese Anwendung für die Durchmesserbestimmung von Blasendomänen in einer (Co/Pd)-Multilage und für die Bestimmung der temperaturabhängigen magnetischen Eindringtiefe in einem supraleitendem BaFe2(As0.24P0.76)2 Einkristall. Desweiteren konnte durch die Kombination von mikromagnetischen Rechnungen und der quantitativen MFM-Datenanalyse die Existenz einer dreidimensionalen Vortex-Struktur am Ende von Co48Fe52-Nanodrähten nachgewiesen werden. Damit ist es gelungen die Tiefensensitivität der Magnetkraftmikroskopie erfolgreich in die Rekonstruktion der vermessenen Magnetisierungsstruktur einzubeziehen.

This diploma thesis is focused on investigation of metallic thin films and nanostructures using scanning probe microscopy. Magnetic properties of these objects are studied by magnetic force microscopy, which is modification of scanning probe microscopy. In the theoretical part basic principles of scanning probe microscopy and magnetic force microscopy are summarized, and also principle of creation of magnetic domains and some special properties of ferromagnetic and antiferromagnetic materials. Further, two techniques of fabricating nanostructures are described. Experimental part is focused on imaging and simulating of magnetic domains. Further, exchange bias is revealed. This phenomenon is present in systems composed from ferromagnetic and antiferromagnetic materials. One part of this diploma thesis is also focused on discussion of problems with magnetic force microscopy.

Zur Aufklärung der lokalen Magnetisierungs- und magnetischen Streufeldstruktur in ferromagnetischen und supraleitenden Materialien wurden magnetkraftmikroskopische (Magnetkraftmikroskopie-MFM) Untersuchungen durchgeführt und quantitativ ausgewertet. Für eine solch quantitative Auswertung muss der Einfluß der verwendeten MFM-Spitzen auf das MFM-Bild bestimmt und in geeigneter Weise subtrahiert werden. Hierzu wurden Spitzenkalibrierungsroutinen und ein Verfahren zur Entfaltung der gemessenen MFM-Daten implementiert, das auf der Wiener Dekonvolution basiert. Mit Hilfe dieser Prozedur können sowohl die räumliche Ausdehnung als auch die Größe der Streufelder direkt aus gemessenen MFM-Bildern bestimmt werden. Gezeigt wurde diese Anwendung für die Durchmesserbestimmung von Blasendomänen in einer (Co/Pd)-Multilage und für die Bestimmung der temperaturabhängigen magnetischen Eindringtiefe in einem supraleitendem BaFe2(As0.24P0.76)2 Einkristall. Desweiteren konnte durch die Kombination von mikromagnetischen Rechnungen und der quantitativen MFM-Datenanalyse die Existenz einer dreidimensionalen Vortex-Struktur am Ende von Co48Fe52-Nanodrähten nachgewiesen werden. Damit ist es gelungen die Tiefensensitivität der Magnetkraftmikroskopie erfolgreich in die Rekonstruktion der vermessenen Magnetisierungsstruktur einzubeziehen.:Introduction 6 1 Contrast formation in Magnetic Force Microscopy (MFM) 9 1.1 Type of interactions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9 1.1.1 Relevant interaction forces . . . . . . . . . . . . . . . . . . . . . . . 9 1.1.2 Magnetic interaction mechanisms . . . . . . . . . . . . . . . . . . . 11 1.2 Basic magnetostatics of the tip-sample system . . . . . . . . . . . . . . . . 12 1.2.1 General magnetostatic expressions . . . . . . . . . . . . . . . . . . . 12 1.2.2 Description of the tip sample system . . . . . . . . . . . . . . . . . 14 1.2.3 Magnetostatics in Fourier space . . . . . . . . . . . . . . . . . . . . 15 2 Instrumentation 20 2.1 Scanning Force Microscopy (SFM) . . . . . . . . . . . . . . . . . . . . . . . 20 2.1.1 Measurement principle and operation modes . . . . . . . . . . . . . 20 2.1.2 Dynamic mode SFM . . . . . . . . . . . . . . . . . . . . . . . . . . 21 2.2 Lift mode MFM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24 2.3 Non-contact MFM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25 2.4 Vibrating Sample Magnetometry . . . . . . . . . . . . . . . . . . . . . . . 26 3 Quantitative Magnetic Force Microscopy 28 3.1 The challenge of MFM image inversion . . . . . . . . . . . . . . . . . . . . 28 3.1.1 Description of the problem and state of the art . . . . . . . . . . . 28 3.1.2 The point probe approximations . . . . . . . . . . . . . . . . . . . . 31 3.1.3 The transfer function approach . . . . . . . . . . . . . . . . . . . . 33 3.2 Tip calibration: Adapted Wiener deconvolution . . . . . . . . . . . . . . . 39 3.2.1 Details of the procedure . . . . . . . . . . . . . . . . . . . . . . . . 39 3.2.2 Evaluation of possible errors . . . . . . . . . . . . . . . . . . . . . . 44 3.3 Noise measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47 3.4 MFM probes and their specific characteristics . . . . . . . . . . . . . . . . 49 3.5 Calibration samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54 3.6 Detection of tip-sample modification . . . . . . . . . . . . . . . . . . . . . 55 4 Quantitative MFM with iron filled carbon nanotube sensors (Fe-CNT) 56 4.1 The monopole character of Fe-CNT sensors . . . . . . . . . . . . . . . . . . 57 4.1.1 Calibration within the point probe approximation . . . . . . . . . . 57 4.1.2 Calibration results and discussion . . . . . . . . . . . . . . . . . . . 59 4.1.3 Quantitative MFM on a [Co/Pt]/Co/Ru multilayer . . . . . . . . . 62 4.2 Inplane sensitive MFM with Fe-CNT sensors . . . . . . . . . . . . . . . . . 63 4.2.1 Bimodal MFM technique . . . . . . . . . . . . . . . . . . . . . . . . 63 4.2.2 Comparison between calculated and measured in-plane contrast . . 66 5 Quantification of magnetic nanoobjects in MFM measurements 70 5.1 Bubble domains in a [Co/Pd]80 multilayer . . . . . . . . . . . . . . . . . . 71 5.1.1 Micromagnetic model . . . . . . . . . . . . . . . . . . . . . . . . . . 72 5.1.2 MFM image simulation . . . . . . . . . . . . . . . . . . . . . . . . . 72 5.1.3 Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . 74 5.2 Quantitative assessment of the magnetic penetration depth in superconductors 78 5.2.1 Comparison of methods . . . . . . . . . . . . . . . . . . . . . . . . 79 5.2.2 Experimental determination of the temperature dependent penetration depth in a BaFe2(As0:24P0:76)2 single crystal . . . . . . . . . . . 83 6 Magnetization studies of CoFe nanowire arrays on a local and global scale 87 6.1 Revisiting the estimation of demagnetizing fields in magnetic nanowire arrays 88 6.1.1 Available approaches . . . . . . . . . . . . . . . . . . . . . . . . . . 88 6.1.2 Calculation of demagnetizing fields in nanowire arrays . . . . . . . . 91 6.2 Micromagnetic Simulations . . . . . . . . . . . . . . . . . . . . . . . . . . . 99 6.3 Combination of demagnetizing field calculations and micromagnetic simulation100 6.4 Experimental details . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102 6.5 Global hysteresis measurements of CoFe nanowire arrays with varying length 104 6.6 Local magnetic characterization of a CoFe nanowire array by quantitative MFM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107 6.6.1 Magnetic structure of individual nanowires . . . . . . . . . . . . . . 107 6.6.2 Magnetization reversal of the nanowire array . . . . . . . . . . . . . 110 6.7 Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117 Conclusions and Outlook 119 Bibliography 121 Acknowledgements 135

Ph.D. / Electrical Engineering / A novel combinatory on-line technique coupling Electrochemistry (EC) with Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) for in-situ quantitative determination of the corrosion mechanism in magnetic thin film structures has been developed in this research. Detailed construction of a system and a comprehensive methodology was described in this dissertation. Uniformly coated multi-layer magnetic thin film samples with multi-elemental alloys containing CoCrPtB and CrMo/Cr on the Ni/P substrate were used in this research for demonstrations. In-situ quantifications conducted in a series of experiments revealed that elemental dissolution was a predominant mechanism during corrosion courses of metallic thin film materials. At the microscopic scale, using results from depletion rate determination as well as cross-sectional analyses of microstructures and magnetic features, elemental passivity was observed to occur, depending on corrosion conditions. Without external influences, surface topographic measurements indicated that passive film could be produced at the macro-scale. The dependence of the dissolution rate of each metallic ion of alloys on electrolyte concentration, potential bias, scanning rate, and corrosion duration suggested that the most critical influential factor in corrosion mechanisms was epitaxial microstructures with strongly-oriented arrangements of grains and grain boundaries. Through the use of cross-sectional microstructural analysis, including high resolution TEM micrography, electron FFT diffraction, and nano-probe with EDS profiling, variations of elemental spatial distributions at grains and grain boundaries due to the corrosion phenomena were discovered, which provided a comprehensive understanding of occurrences of micro-corrosion in thin film structures. Because of the unique magnetic property of magnetic thin films, extensive studies of field strengths from the surface were also performed in this research. Important magnetization variations were noticed when cross-sectional images were obtained. Finally, models of corrosion kinetics in the multiple layers of magnetic thin film structures were proposed.