Studies of ferrite, borosilicate and intercalation materials

This thesis is concerned with several aspects of the chemistry of iron compounds. The preparation (with particular emphasis on coprecipitation and sol-gel techniques) and processing of ferrites are discussed. Chapter 2 describes the synthesis of Ni-Zn ferrites with various compositions by three methods. These methods include coprecipitation and sol-gel techniques. The Ni-Zn ferrites were characterised by powder X-ray diffactometry (PXRD), scanning electron microscopy (SEM), vibrating sample magnetometry (VSM), Mössbauer spectroscopy and resistivity measurements. The results for the corresponding ferrites prepared by each method are compared. Chapter 3 reports the sol-gel preparation of a lead borosilicate glass and its addition to Ni-Zn ferrites prepared by the sol-gel method in Chapter 2. The glass-ferrites formed were analysed by the same techniques employed in Chapter 2. Alterations in the microstructure, magnetic and electronic properties of the ferrites due to glass addition are described. Chapter 4 introduces compounds containing Fe-O-B, Fe-O-Si or B-O-Si linkages. The synthesis and characterisation of compounds containing Fe-O-B units are described. The structure of [Fe(SALEN)]2O.CH2Cl2 (17), used in attempts to prepare compounds with Fe-O-Si bonds, was determined by X-ray crystallography. Chapter 4 also details the synthesis of three new borosilicate compounds containing ferrocenyl groups, i.e. [FcBO)2(OSiBut2)2] (19), [(FcBO)2(OSiPh2)2] (20) and [FcBOSiPh3] (21). The structure of (19) was determined by X-ray Crystallographic analysis. Chapter 5 reviews the intercalation properties of the layered host compound iron oxychloride (FeOCI). Intercalation compounds prepared with the microwave dielectric heating technique are also discussed. The syntheses of intercalation compounds by the microwave method with FeOCI as host and ferrocene, ferrocenylboronic acid and 4-aminopyridine as guest species are described. Characterisation of these compounds by powder X-ray diffractometry (PXRD) and M{ssbauer spectroscopy is reported. The attempted synthesis of an intercalation compound with the borosilicate compound (19) as guest species is discussed. Appendices A-E describe the theory and instrumentation involved in powder X-ray diffractometry (PXRD), scanning electron microscopy (SEM0, vibrating sample magnetometry (VSM), Mössbauer spectroscopy and electrical resistivity measurements, respectively. Appendix F details the attempted syntheses of compounds with Fe-O-B and Fe-O-Si linkages.

Integrated magnetic components for high-power high-current dc-dc converters

This thesis is focused on the design and development of an integrated magnetic (IM) structure for use in high-power high-current power converters employed in renewable energy applications. These applications require low-cost, high efficiency and high-power density magnetic components and the use of IM structures can help achieve this goal. A novel CCTT-core split-winding integrated magnetic (CCTT IM) is presented in this thesis. This IM is optimized for use in high-power dc-dc converters. The CCTT IM design is an evolution of the traditional EE-core integrated magnetic (EE IM). The CCTT IM structure uses a split-winding configuration allowing for the reduction of external leakage inductance, which is a problem for many traditional IM designs, such as the EE IM. Magnetic poles are incorporated to help shape and contain the leakage flux within the core window. These magnetic poles have the added benefit of minimizing the winding power loss due to the airgap fringing flux as they shape the fringing flux away from the split-windings. A CCTT IM reluctance model is developed which uses fringing equations to accurately predict the most probable regions of fringing flux around the pole and winding sections of the device. This helps in the development of a more accurate model as it predicts the dc and ac inductance of the component. A CCTT IM design algorithm is developed which relies heavily on the reluctance model of the CCTT IM. The design algorithm is implemented using the mathematical software tool Mathematica. This algorithm is modular in structure and allows for the quick and easy design and prototyping of the CCTT IM. The algorithm allows for the investigation of the CCTT IM boxed volume with the variation of input current ripple, for different power ranges, magnetic materials and frequencies. A high-power 72 kW CCTT IM prototype is designed and developed for use in an automotive fuelcell-based drivetrain. The CCTT IM design algorithm is initially used to design the component while 3D and 2D finite element analysis (FEA) software is used to optimize the design. Low-cost and low-power loss ferrite 3C92 is used for its construction, and when combined with a low number of turns results in a very efficient design. A paper analysis is undertaken which compares the performance of the high-power CCTT IM design with that of two discrete inductors used in a two-phase (2L) interleaved converter. The 2L option consists of two discrete inductors constructed from high dc-bias material. Both topologies are designed for the same worst-case phase current ripple conditions and this ensures a like-for-like comparison. The comparison indicates that the total magnetic component boxed volume of both converters is similar while the CCTT IM has significantly lower power loss. Experimental results for the 72 kW, (155 V dc, 465 A dc input, 420 V dc output) prototype validate the CCTT IM concept where the component is shown to be 99.7 % efficient. The high-power experimental testing was conducted at General Motors advanced technology center in Torrence, Los Angeles. Calorific testing was used to determine the power loss in the CCTT IM component. Experimental 3.8 kW results and a 3.8 kW prototype compare and contrast the ferrite CCTT IM and high dc-bias 2L concepts over the typical operating range of a fuelcell under like-for-like conditions. The CCTT IM is shown to perform better than the 2L option over the entire power range. An 8 kW ferrite CCTT IM prototype is developed for use in photovoltaic (PV) applications. The CCTT IM is used in a boost pre-regulator as part of the PV power stage. The CCTT IM is compared with an industry standard 2L converter consisting of two discrete ferrite toroidal inductors. The magnetic components are compared for the same worst-case phase current ripple and the experimental testing is conducted over the operation of a PV panel. The prototype CCTT IM allows for a 50 % reduction in total boxed volume and mass in comparison to the baseline 2L option, while showing increased efficiency.

Electromagnetic tracking and steering for catheter navigation

This thesis explores the use of electromagnetics for both steering and tracking of medical instruments in minimally invasive surgeries. The end application is virtual navigation of the lung for biopsy of early stage cancer nodules. Navigation to the peripheral regions of the lung is difficult due to physical dimensions of the bronchi and current methods have low successes rates for accurate diagnosis. Firstly, the potential use of DC magnetic fields for the actuation of catheter devices with permanently magnetised distal attachments is investigated. Catheter models formed from various materials and magnetic tip formations are used to examine the usefulness of relatively low power and compact electromagnets. The force and torque that can be exerted on a small permanent magnet is shown to be extremely limited. Hence, after this initial investigation we turn our attention to electromagnetic tracking, in the development of a novel, low-cost implementation of a GPS-like system for navigating within a patient. A planar magnetic transmitter, formed on a printed circuit board for a low-profile and low cost manufacture, is used to generate a low frequency magnetic field distribution which is detected by a small induction coil sensor. The field transmitter is controlled by a novel closed-loop system that ensures a highly stable magnetic field with reduced interference from one transmitter coil to another. Efficient demodulation schemes are presented which utilise synchronous detection of each magnetic field component experienced by the sensor. The overall tracking accuracy of the system is shown to be less than 2 mm with an orientation error less than 1°. A novel demodulation implementation using a unique undersampling approach allows the use of reduced sample rates to sample the signals of interest without loss of tracking accuracy. This is advantageous for embedded microcontroller implementations of EM tracking systems. The EM tracking system is demonstrated in the pre-clinical environment of a breathing lung phantom. The airways of the phantom are successfully navigated using the system in combination with a 3D computer model rendered from CT data. Registration is achieved using both a landmark rigid registration method and a hybrid fiducial-free approach. The design of a planar magnetic shield structure for blocking the effects of metallic distortion from below the transmitter is presented which successfully blocks the impact of large ferromagnetic objects such as operating tables. A variety of shielding material are analysed with MuMetal and ferrite both providing excellent shieling performance and an increased signal to noise ratio. Finally, the effect of conductive materials and human tissue on magnetic field measurements is presented. Error due to induced eddy currents and capacitive coupling is shown to severely affect EM tracking accuracy at higher frequencies.

Crystallographic and magnetic identification of secondary phase in orientated Bi 5Fe 0.5Co 0.5Ti 3O 15 ceramics

The fabrication of highly-oriented polycrystalline ceramics of Bi 5Fe 0.5Co 0.5Ti 3O 15, prepared via molten salt synthesis and uniaxial pressing of high aspect ratio platelets is reported. Electron backscatter images show a secondary phase within the ceramic which is rich in cobalt and iron. The concentration of the secondary phase obtained from scanning electron microscopy is estimated at less than 2% by volume, below the detection limit of x-ray diffraction (XRD). The samples were characterized by x-ray diffraction, polarization-electric field measurements, superconducting quantum interference device as a function of sample orientation and vibrating sample magnetometry as a function of temperature. It is inferred from the data that the observed ferromagnetic response is dominated by the secondary phase. This work highlights the importance of rigorous materials characterisation in the study of multiferroics as small amounts of secondary phase, below the limit of XRD, can lead to false conclusions.