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Metal oxide nanoparticles, both magnetic and nonmagnetic, have a multitude of applications in gas sensors, catalysts and catalyst supports, airborne trapping agents, biomedicines and drug delivery systems, fuel cells, laser diodes, and magnetic microwaves. Over the past decade, an inexpensive, simple, recyclable, and environmentally friendly large, scale synthesis method for the synthesis of these metal oxide nanoparticles has been sought. Many of the current techniques in use today, while good on the small, laboratory bench scale, suffer from drawbacks that make them unsuitable for the industrial scale. The aminolytic method, developed by Dr. Man Han while working for Dr. Zhang, fits industrial scale-up requirements. The aminolytic method involves a reaction between metal carboxylate(s) and oleylamine in a non-coordinating solvent. This system was shown to produce a range of spinel ferrites. Dr. Lisa Vaughan showed that this method can be recycled multiple times without degrading the quality of the produced nanoparticles. The purpose of this thesis is to test the versatility of the aminolytic method in the production of a wide range of metal oxides as well as various core/shell systems. Chapter 2 explores the effect of precursor carboxylates chain length on the aminolytic synthesis of cobalt ferrite, and manganese ferrite nanoparticles. In Chapter 3, a series of CuxMn1-xFe₂O₄, (x ranges from 0.0 to 0.2), nanoparticles were synthesized via the aminolytic method. This series allows for the investigation of the effects of orbital Jahn-Teller distortion as well as orbital angular momentum on the magnetic properties of this ferrite. The quantum couplings of magnetic ions in spinel ferrites govern their magnetic properties and responses. An understanding of the couplings between these metal ions allows for tailoring magnetic properties to obtain the desired response needed for various applications. Chapter 4 investigates the synthesis of MnO and Mn₃O₄ nanoparticles in pure single phase with high monodispersity. To the best of our knowledge, the range of sizes produced for MnO and Mn₃O₄ is the most extensive, and therefore a magnetic study of these systems shows some intriguing size dependent properties. The final part of this chapter investigates the applicability of the aminolytic method for building a MnO shell on a CoFe₂O₄ core. Chapter 5 explores the synthesis of another metal oxide, ZrO₂ in both the cubic and monoclinic phases with no impurities. The use of the aminolytic method here removes the need for dangerous/expensive precursors or equipment and eliminates the need for extensive high temperature heat treatments that destroy monodispersity which is required for most techniques. The creation of a core/shell system between CoFe₂O₄ and ZrO₂ using the aminolytic method was also tested. This core/shell system adds magnetic manipulation which is especially useful for the recovery of zirconia based photocatalyst. Chapter 6 studies the application of the aminolytic method in the synthesis of yttrium iron garnet (YIG) and yttrium iron perovskite (YIP) nanoparticles. Current synthesis techniques used to produce YIG and YIP nanoparticles often requires high temperatures, sensitive to contamination, which could be eliminated through the use of our method

The ionic conductivity of the lithium ionic conductor, Li5La3Ta2O12, is studied in an attempt to better understand the intrinsic bulk ionic conductivity and extrinsic sample dependent contributions to the ionic conductivity, such as grain boundary effects and the electrode-electrolyte interface. To characterize the material, traditional AC impedance spectroscopy studies were performed as well novel in-situ nanoscale transport measurements. To perform the nanoscale measurements, higher quality samples were required and new synthesis techniques developed. The results of these new synthesis techniques was samples with higher densities, up to 96% of theoretical, and slightly higher room temperature ionic conductivity, 2x10^−5 S/cm. By combining the AC impedance spectroscopy results and in-situ nanoscale transport measurements from this study and prior reported results, as well as introducing models traditionally used to analyze supercapacitor systems, a new interpretation of the features seen in the AC impedance spectroscopy studies is presented. This new interpretation challenges the presence of Warburg Diffusion at low frequencies and the offers a new interpretation for the features that have been traditionally associated with grain boundary effects.

The North Caribou Greenstone Belt (NCGB) lies at the core the granitoid-dominant North Caribou Terrane (NCT). Two sedimentary assemblages; the Eyapamikama (ELS) and Zeemal-Heaton Lake (ZHA) form the core of the NCGB. Geochemistry of garnets from the orogenic Au deposit at Musselwhite suggest that the auriferous fluids have a contribution of metamorphic fluids and mineralization consisted of prolonged, multi-stage periods. Chemical zoning suggests changes in the influx of chalcophile and lithophile elements and that Au/sulphide ratios during nucleation were lower relative to later growth events. Zircons from the ELS and ZHA suggest a c. 100 My hiatus in the onset of sedimentation, with the ZHA showing younger, “Timiskaming-type” ages. Age distributions from each assemblage reflect proximal, igneous sources. Nd isotopic compositions of the ZHA suggest a mixture of ancient and contemporaneous sources which are similar to external TTG rocks. Deplete mantle model ages of the ZHA rocks indicate a Mesoarchean inheritance.

Nuo 1926-ųjų metų, kai pirmą kartą buvo ištirta preliminari natūralių silikatinių mineralų, turinčių kubinę kristalinę gardelę, struktūra, granatų šeimai priskiriami junginiai tapo viena labiausiai tyrinėjamų medžiagų grupių. Granatai, kuriuose yra pereinamųjų metalų bei retųjų žemių metalų, pasižymi ypatingu technologiniu pritaikymu. Kaip šviečiančios medžiagos jie naudojami kietafaziuose lazeriuose, televizorių ekranuose ar dioduose. Europiu arba chromu legiruoti junginiai galėtų būti pritaikyti optiniam vaizdavimui medicinoje, kas iki šiol nebuvo daryta. Galimybė pagerinti granatų optines ir mechanines savybes bei naujos pritaikymo sritys suteikia stiprią motyvaciją tyrinėjimams. Pagrindinis disertacijos tikslas buvo naujų mišrių metalų granatų sintezė bei jų optinių savybių tyrimas. Taip pat siekta ištirti europį supančios aplinkos įtaką jo liuminescencinėms savybėms tiek milteliuose, tiek kristaluose. Milteliai buvo sintetinti zolių-gelių arba kietafazės reakcijos metodu. Kristalai auginti keliaujančio lydalo slankioje zonoje būdu. Medžiagų faziniai virsmai tirti Rentgeno spindulių difrakcijos metodu. Neutronų difrakcijos duomenys bei Rietveldo tikslinimas buvo panaudoti granatų struktūrinei analizei. Junginių optinės savybės įvertintos išmatavus atspindžio, sužadinimo ir emisijos spektrus. / Since 1926 when the preliminary structure of natural silicate minerals having cubic structure was determined, the family of garnets became one of the most extensively studied group of compounds. Garnets containing transition metals and rare-earths carry many important technological uses as magnetic materials, as phosphor materials employed in solid state lasers, television screens and light-emitting diodes, as computer memories, as near UV and near IR radiation up/down-converting compounds in Si solar cells and in other devices as microwave optical elements. The europium or chromium doped garnets also could be applied in the new field as optical imaging. The improvements in mechanical and optical properties, the new areas of applications provide a strong motivation for studying garnets in general. To synthesize and to characterize new mixed-metal garnets was the main aim of the present thesis. The investigation of the dependence of europium optical properties on the local environment in different garnets was also in the field of interest. Therefore, powders of the new mixed-metal garnets were synthesized by sol-gel route, while traveling solvent floating zone method was used for crystal growth. X-ray diffraction was used for phase identification. The neutrons diffractions and Rietveld refinement gave information of the crystal structure. Finally, reflection, excitation and emission spectra were recorded for the investigation of the optical properties.

Since 1926 when the preliminary structure of natural silicate minerals having cubic structure was determined, the family of garnets became one of the most extensively studied group of compounds. Garnets containing transition metals and rare-earths carry many important technological uses as magnetic materials, as phosphor materials employed in solid state lasers, television screens and light-emitting diodes, as computer memories, as near UV and near IR radiation up/down-converting compounds in Si solar cells and in other devices as microwave optical elements. The europium or chromium doped garnets also could be applied in the new field as optical imaging. The improvements in mechanical and optical properties, the new areas of applications provide a strong motivation for studying garnets in general. To synthesize and to characterize new mixed-metal garnets was the main aim of the present thesis. The investigation of the dependence of europium optical properties on the local environment in different garnets was also in the field of interest. Therefore, powders of the new mixed-metal garnets were synthesized by sol-gel route, while traveling solvent floating zone method was used for crystal growth. X-ray diffraction was used for phase identification. The neutrons diffractions and Rietveld refinement gave information of the crystal structure. Finally, reflection, excitation and emission spectra were recorded for the investigation of the optical properties. / Nuo 1926-ųjų metų, kai pirmą kartą buvo ištirta preliminari natūralių silikatinių mineralų, turinčių kubinę kristalinę gardelę, struktūra, granatų šeimai priskiriami junginiai tapo viena labiausiai tyrinėjamų medžiagų grupių. Granatai, kuriuose yra pereinamųjų metalų bei retųjų žemių metalų, pasižymi ypatingu technologiniu pritaikymu. Kaip šviečiančios medžiagos jie naudojami kietafaziuose lazeriuose, televizorių ekranuose ar dioduose. Europiu arba chromu legiruoti junginiai galėtų būti pritaikyti optiniam vaizdavimui medicinoje, kas iki šiol nebuvo daryta. Galimybė pagerinti granatų optines ir mechanines savybes bei naujos pritaikymo sritys suteikia stiprią motyvaciją tyrinėjimams. Pagrindinis disertacijos tikslas buvo naujų mišrių metalų granatų sintezė bei jų optinių savybių tyrimas. Taip pat siekta ištirti europį supančios aplinkos įtaką jo liuminescencinėms savybėms tiek milteliuose, tiek kristaluose. Milteliai buvo sintetinti zolių-gelių arba kietafazės reakcijos metodu. Kristalai auginti keliaujančio lydalo slankioje zonoje būdu. Medžiagų faziniai virsmai tirti Rentgeno spindulių difrakcijos metodu. Neutronų difrakcijos duomenys bei Rietveldo tikslinimas buvo panaudoti granatų struktūrinei analizei. Junginių optinės savybės įvertintos išmatavus atspindžio, sužadinimo ir emisijos spektrus.

The procedure for milling micrometre scale cantilevers of lutetium iron garnet using a focused ion beam microscope was developed. The infrastructure to study these cantilevers using rotational hysteresis loops and ferromagnetic resonance experiments was set up. The cantilevers were shown to remain magnetic after milling, and the origin of their hysteresis loops investigated with a variant of the Stoner-Wohlfarth model. Ferromagnetic resonance in the cantilevers was demonstrated as the first step towards studying magnetomechanical coupling.

Thesis (Ph. D.)--University of Washington, 2007. / Vita. Includes bibliographical references (leaves 122-125).

A composição da granada possui relação direta com as condições físico-químicas de seu ambiente de geração e consequentemente com a rocha em que se formou. Assim, pode-se relacionar a composição química da granada com a rocha hospedeira, dentro de certas limitações. Este trabalho focaliza a análise varietal da granada para a identificação das principais rochas-fonte envolvidas na proveniência dos arenitos da Bacia de Campos (Andar Alagoas), no estado do Rio de Janeiro. Nas análises obtidas por microssonda eletrônica, dos 17 poços do segmento offshore do estudo, verifica-se a contribuição de diferentes rochas-fonte portadoras de granadas, identificadas como dos tipos A, B e C, e dentre essas, a que predomina são as granadas do tipo B. Uma individualização dessa classificação nos permitiu categorizá-las em granadas do tipo Bi, que são granadas derivadas de rochas ígneas ácidas e intermediárias, notadamente granitóides. A identificação precisa da rocha-fonte possui algumas limitações, devido a superposição nas composições mostradas nos diagramas ternários discriminantes das granadas. Entretanto, a ausência ou pequena incidência de zonações composicionais e de inclusões, embora não excluam totalmente as outras categorias, apontam para essa classificação. Granadas do tipo D e E não aparecem em nenhuma das amostras analisadas. A interpretação dos resultados de aproximadamente 4000 análises das 65 amostras indica duas contribuições principais para a proveniência desses arenitos: no setor sul da bacia, terrenos derivados do Domínio Cabo Frio, (rochas metamórficas da fácies granulito a anfibolito superior, meta-pelitos aluminosos e secundariamente metabasitos, além de granitos), e na porção norte da bacia, uma derivação dos terrenos orientais do orógeno Ribeira (terrenos de alto grau e granitóides associados). A direção de suplemento sedimentar principal é de sudoeste para nordeste, interpretada como resultado da identificação dessa maior contribuição dos terrenos fonte. As areias localizadas no setor norte, com granadas derivadas do tipo B e Bi, principalmente, indicam a presença de rochas granitóides na área-fonte. Tais rochas fonte geram areias de composição mais quartzosa e/ou quartzofeldspática, com maior potencial para produzirem arenitos-reservatórios de melhor qualidade. / Garnet composition have direct relationship with the physic-chemical environment of formation and because of this with the host rock composition. Hence, it is possible to establish a linking between the host rock type and garnet composition, despite some limitations. This work focus on the garnet varietal analysis to identify the provenance of sandstones, Campos Basin (Alagoas Stage), Rio de Janeiro. In the performed analyzes of seventeen offshore boreholes, it is remarkable the presence of garnets which plot into the fields A, B and C; and that among these, the predominant type belongs to the B field. The individualization of source-rock types in this classification allowed us to classify the garnets in the type Bi, which are derived from acidic and intermediate igneous rocks, mainly granitoids. Accurate identification of the source rock has some limitations due to overlap in the compositions shown in discriminating ternary diagrams of garnets. Despite the difficulty in distinguishing between the fields shown in the ternary diagram, we can say that the absence or minor incidence of inclusion and zonation in the samples support this separation. D-type garnets and E-type do not appear. Interpretation of the results of approximately 4000 analysis of the 65 samples indicates two main contributions to the provenance of these sandstones: the wells placed in the basin southern region derived from the Cabo Frio Domain (metamorphic rocks of amphibolite to medium granulite facies, mainly aluminous metapelites and secondarily metabasites and granites); the wells in the basin northern region, where there is substantially more analyzes and samples, derived from the eastern terrains of the Ribeira orogen (high degree terrains and granitoids). The main direction of sedimentary supplement is from southwest to northeast, interpreted as a result of identification of this major contribution of sediments supply. The sands located in the northern wells, with garnets derived from B and Bi fields, indicate mainly the presence of granitoids in the source-area. This sourcerock produce quartzor quartz-feldspathic sands which may be potential high quality sandstone reservoirs.

A composição da granada possui relação direta com as condições físico-químicas de seu ambiente de geração e consequentemente com a rocha em que se formou. Assim, pode-se relacionar a composição química da granada com a rocha hospedeira, dentro de certas limitações. Este trabalho focaliza a análise varietal da granada para a identificação das principais rochas-fonte envolvidas na proveniência dos arenitos da Bacia de Campos (Andar Alagoas), no estado do Rio de Janeiro. Nas análises obtidas por microssonda eletrônica, dos 17 poços do segmento offshore do estudo, verifica-se a contribuição de diferentes rochas-fonte portadoras de granadas, identificadas como dos tipos A, B e C, e dentre essas, a que predomina são as granadas do tipo B. Uma individualização dessa classificação nos permitiu categorizá-las em granadas do tipo Bi, que são granadas derivadas de rochas ígneas ácidas e intermediárias, notadamente granitóides. A identificação precisa da rocha-fonte possui algumas limitações, devido a superposição nas composições mostradas nos diagramas ternários discriminantes das granadas. Entretanto, a ausência ou pequena incidência de zonações composicionais e de inclusões, embora não excluam totalmente as outras categorias, apontam para essa classificação. Granadas do tipo D e E não aparecem em nenhuma das amostras analisadas. A interpretação dos resultados de aproximadamente 4000 análises das 65 amostras indica duas contribuições principais para a proveniência desses arenitos: no setor sul da bacia, terrenos derivados do Domínio Cabo Frio, (rochas metamórficas da fácies granulito a anfibolito superior, meta-pelitos aluminosos e secundariamente metabasitos, além de granitos), e na porção norte da bacia, uma derivação dos terrenos orientais do orógeno Ribeira (terrenos de alto grau e granitóides associados). A direção de suplemento sedimentar principal é de sudoeste para nordeste, interpretada como resultado da identificação dessa maior contribuição dos terrenos fonte. As areias localizadas no setor norte, com granadas derivadas do tipo B e Bi, principalmente, indicam a presença de rochas granitóides na área-fonte. Tais rochas fonte geram areias de composição mais quartzosa e/ou quartzofeldspática, com maior potencial para produzirem arenitos-reservatórios de melhor qualidade. / Garnet composition have direct relationship with the physic-chemical environment of formation and because of this with the host rock composition. Hence, it is possible to establish a linking between the host rock type and garnet composition, despite some limitations. This work focus on the garnet varietal analysis to identify the provenance of sandstones, Campos Basin (Alagoas Stage), Rio de Janeiro. In the performed analyzes of seventeen offshore boreholes, it is remarkable the presence of garnets which plot into the fields A, B and C; and that among these, the predominant type belongs to the B field. The individualization of source-rock types in this classification allowed us to classify the garnets in the type Bi, which are derived from acidic and intermediate igneous rocks, mainly granitoids. Accurate identification of the source rock has some limitations due to overlap in the compositions shown in discriminating ternary diagrams of garnets. Despite the difficulty in distinguishing between the fields shown in the ternary diagram, we can say that the absence or minor incidence of inclusion and zonation in the samples support this separation. D-type garnets and E-type do not appear. Interpretation of the results of approximately 4000 analysis of the 65 samples indicates two main contributions to the provenance of these sandstones: the wells placed in the basin southern region derived from the Cabo Frio Domain (metamorphic rocks of amphibolite to medium granulite facies, mainly aluminous metapelites and secondarily metabasites and granites); the wells in the basin northern region, where there is substantially more analyzes and samples, derived from the eastern terrains of the Ribeira orogen (high degree terrains and granitoids). The main direction of sedimentary supplement is from southwest to northeast, interpreted as a result of identification of this major contribution of sediments supply. The sands located in the northern wells, with garnets derived from B and Bi fields, indicate mainly the presence of granitoids in the source-area. This sourcerock produce quartzor quartz-feldspathic sands which may be potential high quality sandstone reservoirs.