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Cancer is a leading case of mortality worldwide. Governments spent multibillion expenses on treatment and palliative care of diseased people. Despite these generous funding and intensive research with aim to find a cure or efficient treatment for cancer, until now there is a lack in selective cancer management strategies. Conventional treatment strategies for cancer, such as surgery, cytotoxic chemotherapy, radiation therapy, hormone therapy don’t have selectivity toward cancer – the property of discrimination of healthy organs and tissues from the diseased site. Chemotherapy is very challenging as the difference between effective and lethal doses is very minuscule in most cases. Moreover, devastating side effects dramatically changes the quality of life for cancer patients. To address these issues two main strategies are intensively utilized in chemistry: (I) the design and synthesis of novel anticancer organic compounds with higher selectivity and low toxicity profiles and the second, design and preparation of biocompatible nanocarriers for imaging and anticancer compound selective delivery nanomedicine. The following dissertation combines the above two strategies as bellows: First project is related to the design and synthetic route development toward novel nature-inspired group of heterocyclic compounds – iso-Phidianidines. The second project focused on design, preparation and evaluation of hybrid theranostics (therapeutic and diagnostic in a single entity). Chapter 1 is a general background review of the major topics that will be discussed in this dissertation. The first efficient and high-yielding synthetic route toward iso-phidianidines, containing regioisomeric form of 1,2,4-oxadiazole linked to the indole via methylene bridge is reported in Chapter 2. In vitro test of the synthesized library of iso-phidianidines revealed micromolar range of cytotoxicity toward human cervical cancer cell line. Structure activity relationship revealed the importance of presence of monosubsituted amine in 3 position of oxadiazole to maintain activity. Moreover, gradual increase of activity was detected in increasing of the length of the diamine. Polyamine (spermidine) side chain demonstrated strongest anticancer activity, identified as lead compound and may be studied further as a good candidate for cervical cancer treatment. Finally, the remaining high activity of amino-terminated iso-phidianidines demonstrated that presence of guanidine group in termini is not necessary for high cytotoxicity. The second part of this dissertation (Chapter 3) discusses the rational design, wet protocol synthesis and complete characterization of the novel hybrid material – polydopamine coated iron-cobalt nanocubes (PDFCs). This material was loaded with anticancer model drug doxorubicin in one step procedure (PDFC-DOX) and the resulting drug-delivery vehicle was found to be successfully internalized by cervical cancer cells. The cytotoxicity test demonstrated inhibition of 50% of the cells at the concentration of 30μg/ml for PDFC-DOX. Moreover, the release was highly attenuated and pH-sensitive in acidic range. PDFC was also modified with fluorescein leading to green fluorescent nanoparticles PDFC-FITC, which demonstrated excellent intracellular molecular imaging property. PDFCs with one of the highest magnetic saturation among the materials used in biomedicine (226 emu/g based on core) showed the absence of any cytotoxicity in vitro and excellent MRI contrasting property (r2=186.44 mMs-1, higher than commercial contrast agents Ferridex® and Clio®), both in vitro and in vivo on mice. They were cleared out from the mice bodies in month without affecting their health. Due to the high density of core (8.3 g/cm3) they demonstrated ability to be contrast materials also for X-Ray CT diagnostic modality, increasing the tumor detection and visualization probability in combination with MRI. In addition to it’s diagnostic and drug-delivery modalities, PDFC was evaluated also for microwave-induced cytotoxicity as a novel concept in cancer treatment. As low as 10 μg/ml concentration of PDFCs in human cervical cancer cells caused extensive death above 73% upon exposure to 2,45 GHz of microwaves for one minute. Laser irradiation (808 nm, 15 minutes) of cancer cells with internalized PDFCs caused cell death above 60%. The specific absorption rate of PDFCs at 470 MHz frequency and 20 mT of the alternating magnetic field power was 180 W/g, which is nearly 100 W higher than for commercial nanoparticles (Ferridex®).

Iron-cobalt alloys have been extensively studied as potential hard disk drive write head materials due to their potentially high saturation flux densities (~2.4T), low coercivities and ease of deposition. Iron-cobalt plating solutions have, however, been shown to have stability issues, necessitating that they be used at low pH or that a stabilizing agent be added to the solution. The purpose of this thesis is to evaluate the stability of a dibasic ammonium citrate plating solution and to characterize the deposits which result from its use. The plating solutions are found to be less stable than previously claimed. The solutions are oxidized by dissolved oxygen, which leads to a valence change in the iron ions and eventually the formation of iron oxide/hydroxide precipitates. These effects are exacerbated by heating or the application of a voltage across the solution. Deposits plated from the solution are fine grained (<40nm) and compact through their thickness. While normally deposited as the equilibrium BCC phase, metastable phases are deposited at elevated temperatures, high pH or in the absence of a stabilizing agent. A metastable phase which is isomorphous to α-Mn is deposited at elevated temperatures. This phase transforms to the BCC phase when annealed at >174ºC and is highly textured. Its presence is detrimental to deposit coercivity. / Materials Engineering

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Thesis (Ph. D.)--Materials Science and Engineering, Georgia Institute of Technology, 2006. / Tannenbaum, Rina, Committee Chair ; Rosario Gerhardt, Committee Member ; Hamid Garmestani, Committee Member ; Karl Jacob, Committee Member Vita. Includes bibliographical references.

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Nanoalloys are an exciting new class of materials in the growing field of nanotechnology. Nanoalloys consist of the nanoscale co-aggregation of two or more metals with a potential to form compositionally-ordered phases or superstructures that have properties unlike those of the individual metal clusters or of bulk alloys of the constituent metals. This research seizes the opportunity that the nanoscale domain has to offer, and focuses on the synthesis of iron and cobalt nanoalloys via the simultaneous decomposition of iron cobalt organometallic precursors in a stabilizing environment, accompanied by the thorough characterization of the resulting nanoclusters. Zero-valent FeCo nanoalloys may potentially have interesting uses as magnetic materials. Since these clusters have sizes less than the size of their magnetic domain, the clusters will exhibit single domain magnetism. This magnetism may be observed by the presence of chain structures of FeCo nanoclusters due to the alignment of their single magnetic domains. In order to create a near-atomically homogeneous nanoalloy without preferential aggregation of its metal atom constituents, no clustering and phase separation should take place. In the bulk, alloys of iron and cobalt phase separate over most of the compositional range. Conversely, at the nanoscale, it may be possible to synthesize nanoalloy structures that are not normally favorable at given compositions, by the manipulation of reaction kinetics. In order to produce an atomically mixed nanoalloy, the transformation reactions of the organometallic precursors should display similar kinetic features, i.e. similar reaction rates. Therefore, the reaction kinetics of all the species in the reaction must be similar to avoid competition between them. As a result, kinetic control of the individual transformation reaction rates of each species may be used to modulate the aggregation and phase separation of the different species, and consequently control cluster morphology. This work has provided the framework for the design of synthesis methods that enable the control of the structure of FeCo nanoalloys with careful attention to precursor decomposition kinetics and the correlation between reaction kinetics and nanoalloy morphology.

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The purpose of this research project was to study the αᵧ phase in Alnico 6. Other phases were studies for comparison. Also the effect of an applied magnetic field on the formation of the αᵧ phase was investigated. Three single crystals of Alnico 6 were heat treated for one hour—one at 1250°C, one at 1000°C, and one at 800°C—and water-quenched. The microstructure of each sample was observed with the optical microscope, and X-ray diffraction patterns were taken to determine the crystal structure of the phases present. Several single crystal samples of Alnico 6 were heat treated at 1000°C and furnace-cooled. Some of the samples were heat treated and furnace-cooled in the presence of an applied magnetic field of about 5000Oe, and the others were heat treated and furnace-cooled without an applied magnetic field. Each set of samples were electrothinned, and the microstructure of the αᵧ and α₁ ₊ α₂ phases was studied using the electron microscope. Electron diffraction patterns and electron micrographs were taken from αᵧ regions and α₁ ₊ α₂ regions of each sample. By a combination of X-ray and electron diffraction, it was determined that the crystal structure of the α, α₁, α₂ and αᵧ phases is body-centered cubic, with a lattice parameter of 2.87 Å. Electron diffraction showed that the crystal structure of the combined α₁ ₊ α₂ phases is ordered body-centered cubic, and that the lattices of these two phases are coherent. Other investigators have found that only the α₁ phase is ordered in Alnico 5 and Alnico 8 and thus is believed be the case in Alnico 6 also. Electron diffraction showed the αᵧ phase to be ordered, with the degree of ordering less than that in the α₁ phase. Some difference was noted between the αᵧ phase formed with a magnetic field and that formed without a magnetic field. The αᵧ formed with a magnetic field showed twinning and some small lattice rotations, while stat formed without a field did not. The reason for this is not known.

Dans ce travail, nous nous sommes intéressés aux propriétés magnétiques intrinsèques (moments et anisotropie magnétiques) de nanoparticules bimétalliques fer-cobalt. Pour cela, des agrégats FeCo dans la gamme de taille 2-6 nm ont été préparés en utilisant la technique MS-LECBD (Mass Selected Low Energy Cluster Beam Deposition) et enrobés en matrice in − situ afin de les séparer, d'éviter leur coalescence pendant les recuits et de les protéger à leur sortie à l'air. Dans un premier temps, les propriétés structurales (dispersion de taille, morphologie, composition, structure cristallographique) ont été étudiées en vue de corréler directement les modifications des caractéristiques magnétiques des nanoparticules, à leur structure et à l'ordre chimique obtenu après traitement thermique haute température. D'autre part, pour mettre en évidence les effets d'alliages à cette échelle, des références d'agrégats purs de fer et de cobalt ont été fabriquées et étudiées en utilisant les mêmes techniques. Par microscopie électronique en transmission à haute résolution, diffraction anomale et absorption de rayons X (high resolution transmission electron microscopy (HRTEM), anomalous x-ray diffraction (AXD) and extended x-ray absorption fine structure (EXAFS), nous avons mis en évidence un changement structural depuis une phase A2 chimiquement désordonnée vers une phase B2 type CsCl chimiquement ordonnée. Cette transition a été validée par nos résultats obtenus par magnétomètrie SQUID et dichroïsme magnétique circulaire (x-ray magnetic circular dichroism (XMCD)) / Over the past few decades, use of nanostructures has become widely popular in the different field of science. Nanoparticles, in particular, are situated between the molecular level and bulk matter size. This size range gave rise to a wide variety physical phenomena that are still not quite understood. Magnetic nanoparticles are at their hype due to their applications in medical field, as a catalyst in a wide number of chemical reactions, in addition to their use for information storage devices and spintronics. In this work, we are interested in studying the intrinsic magnetic properties (magnetic moments and anisotropy) of FeCo nanoparticles. Thus, in order to completely understand their properties, mass-selected FeCo nanoparticles were prepared using the MS-LECBD (Mass Selected Low Energy Cluster Beam Deposition) technique in the sizes range of 2-6 nm and in − situ embedded in a matrix in order to separate them, to avoid coalescence during the annealing and to protect during transfer in air. From a first time, the structural properties (size, morphology, composition, crystallographic structure) of these nanopar- ticles were investigated in order to directly correlate the modification of the magnetic properties to the structure and chemical ordering of the nanoparticles after high temperature treatment. In addition to the bimetallic FeCo nanoparticles, reference Fe and Co systems were also fabricated and studied using the same techniques. The structural properties were investigated using high resolution transmission electron microscopy (HRTEM), anomalous x-ray diffraction (AXD) and extended x-ray absorption fine structure (EXAFS) where a phase transition from a disordered A2 phase to a chemically ordered CsCl B2 phase was observed and further validated from the magnetic findings using SQUID magnetometry and x-ray magnetic circular dichroism (XMCD)