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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
41

Resolving Local Magnetization Structures by Quantitative Magnetic Force Microscopy

Vock, Silvia 09 May 2014 (has links)
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
42

Performance characterisation of duplex stainless steel in nuclear waste storage environment

Ornek, Cem January 2016 (has links)
The majority of UK’s intermediate level radioactive waste is currently stored in 316L and 304L austenitic stainless steel containers in interim storage facilities for permanent disposal until a geological disposal facility has become available. The structural integrity of stainless steel canisters is required to persevere against environmental degradation for up to 500 years to assure a safe storage and disposal scheme. Hitherto existing severe localised corrosion observances on real waste storage containers after 10 years of exposure to an ambient atmosphere in an in-land warehouse in Culham at Oxfordshire, however, questioned the likelihood occurrence of stress corrosion cracking that may harm the canister’s functionality during long-term storage. The more corrosion resistant duplex stainless steel grade 2205, therefore, has been started to be manufactured as a replacement for the austenitic grades. Over decades, the threshold stress corrosion cracking temperature of austenitic stainless steels has been believed to be 50-60°C, but lab- and field-based research has shown that 304L and 316L may suffer from atmospheric stress corrosion cracking at ambient temperatures. Such an issue has not been reported to occur for the 2205 duplex steel, and its atmospheric stress corrosion cracking behaviour at low temperatures (40-50°C) has been sparsely studied which requires detailed investigations in this respect. Low temperature atmospheric stress corrosion cracking investigations on 2205 duplex stainless steel formed the framework of this PhD thesis with respect to the waste storage context. Long-term surface magnesium chloride deposition exposures at 50°C and 30% relative humidity for up to 15 months exhibited the occurrence of stress corrosion cracks, showing stress corrosion susceptibility of 2205 duplex stainless steel at 50°C.The amount of cold work increased the cracking susceptibility, with bending deformation being the most critical type of deformation mode among tensile and rolling type of cold work. The orientation of the microstructure deformation direction, i.e. whether the deformation occurred in transverse or rolling direction, played vital role in corrosion and cracking behaviour, as such that bending in transverse direction showed almost 3-times larger corrosion and stress corrosion cracking propensity. Welding simulation treatments by ageing processes at 750°C and 475°C exhibited substantial influences on the corrosion properties. It was shown that sensitisation ageing at 750°C can render the material enhanced susceptible to stress corrosion cracking at even low chloride deposition densities of ≤145 µm/cm². However, it could be shown that short-term heat treatments at 475°C can decrease corrosion and stress corrosion cracking susceptibility which may be used to improve the materials performance. Mechanistic understanding of stress corrosion cracking phenomena in light of a comprehensive microstructure characterisation was the main focus of this thesis.

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