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xxv, 207 p. ; ill. (some col.) A print copy of this title is available from the UO Libraries, under the call number: SCIENCE QD172.T6 T87 2008 / A growing interest in the physics of complex systems such as in the transition-metal oxide family has exploded recently, especially in the last 20 years or so. One notable effect is the change in electrical resistivity of a system by orders of magnitude in an applied magnetic field, coined the "colossal magnetoresistance effect". In efforts to understand these types of effects, there has been an unveiling of a rich variety of phenomena in the field of strongly correlated electron physics that has come to dominate the current scientific times. Most notable is the competition of myriad types of order: magnetic, lattice, charge and orbital all self-organize to display a fascinating array of phases on a variety of length scales. Furthermore, it has become apparent that new probes are needed to grasp some of this physics that transcends current condensed matter theory, where much of the behavior of these types of systems has remained unexplored. We have developed a new technique to gain more information about the system than with conventional x-ray diffraction. By scattering highly coherent, low energy x-rays, we can measure manganite speckle: a "fingerprint' of the microscopic structure in the bulk. The coherence of the x-rays can further be used to elucidate new insight into the dynamics of these phases. We describe here a number of novel effects near the orbital order phase transition in a half-doped manganite. We observe a small fluctuating component in the scattered signal that is correlated with three effects: both a rapidly decreasing total signal and orbital domain size, as well as an abrupt onset of a broad background intensity that we attribute to the thermal production of correlated polarons. Our results suggest that the transition is characterized by a competition between a pinned orbital domain topology that remains static, and mobile domain boundaries that exhibit slow, spatiotemporal fluctuations. This study opens up a new chapter to the study of manganite physics as coherent x-ray scattering offers a new direction to understand the strange and exotic behavior demonstrated in the multifaceted manganites. / Adviser: Stephen Kevan

Orientadora: Profa. Dra Márcia T. Escote / Dissertação (mestrado) - Universidade Federal do ABC, Programa de Pós-Graduação em Física, 2014. / Este trabalho mostra um estudo sistemático da síntese e caracterização da manganita mista La1..xSrxMnO3 (com x = 0, 4; 0, 5 e 0, 6) e os estudos iniciais de síntese e caracterização da manganita mista La1..xBaxMnO3 ( com x = 0, 4; 0, 5 e 0, 6). As amostras foram produzidas a partir de soluções precursoras contendo sais de La, Ba, Sr e Mn misturadas em quantidades estequiométricas em uma solução de hidróxido de potássio (KOH) para a obtenção de manganitas na forma de pós cristalinos utilizando o método de síntese hidrotermal usando um reator de microondas. No trabalho são estudados os parâmetros da reação necessários para a produção destes compostos. Esses parâmetros foram: temperatura de síntese, concentração da solução mineralizadora (KOH), tempo de síntese e porcentagem de preenchimento do vaso reacional. As amostras foram caracterizadas pelas técnicas de difração de raios-X (DRX), microscopia eletrônica de varredura (MEV) e medidas de magnetização em função da temperatura e campo magnético aplicado. A partir dos resultados experimentais foram determinadas as condições adequadas para a síntese dessas manganitas, essas condições foram: temperatura do forno de 250C, 30 minutos de síntese, um preenchimento de 50% da capacidade do vaso reacional usado para a síntese de ambas manganitas e concentrações molares na faixa de 9-12 mol/L de KOH na solução para a o caso da síntese da manganita dopada com estrôncio e concentrações 10-14 mol/L de KOH para as manganitas dopadas com bário. As caracterizações mostraram que as manganitas La1..xSrxMnO3 (com x = 0, 4; 0, 5 e 0, 6) obtidas neste estudo cristalizam-se em uma estrutura perovskita distorcida tetragonalmente com tamanho de partículas na faixa de 0, 2 - 8 mm e com uma morfologia irregular. Foi encontrado que o aumento na concentração do mineralizador KOH resulta na obtenção de partículas menores reduzindo a faixa de tamanhos de 3 - 8 mm a 0, 2 - 1 mm no caso das manganitas de lantânio estrôncio manganês preparadas com concentrações molares na faixa de 9 a 12 mol/L de KOH. O aumento da concentração de KOH no caso das manganitas de bário favoreceu a cristalização de microcubos. Os fatores como tempo de síntese e porcentagem de preenchimento do vaso reacional não tiveram um efeito significativo no tamanho ou morfologia dos produtos obtidos neste estudo. Os compostos La0,6Sr0,4MnO3, La0,5Sr0,5MnO3 e La0,4Sr0,6MnO3 tiveram comportamentos típicos ferromagnético abaixo da temperatura de transição e o composto La0,4Sr0,6MnO3 apresentou um comportamento anti-ferromagnético a temperaturas menores a 200K. / This work shows a systematic study for the synthesis and characterization of mixed valence manganites La1..xAxMnO3 (A = Sr and Ba with x = 0.4, 0.5 and 0.6). The samples were produced from precursor solutions containing La, Ba, Sr and Mn salts in stoichiometric amounts in KOH alkaline medium in order to obtain the manganites in the form of crystalline powders using the microwave hydrothermal synthesis technique. In this work we evaluate the necessary parameters for the production of these compounds, these parameters were: temperature synthesis, concentration of mineralizer agent (KOH), synthesis time and the filling percentage of the reaction vessel. The obtained samples were characterized using X-ray diffraction technique (XRD), scanning electron microscopy (SEM) and magnetic measurements as a function of temperature and applied magnetic field. The results show that the suitable conditions for the synthesis were a temperature of 250C for A = Sr and Ba with KOH concentration in the range of 9 - 12 mol/L for the stronium based manganite and from 10-14 mol/L for de barium based manganite. 30 minutes of hydrothermal synthesis were found sufficient to obtain the manganites and with a filling percentagem of 50% of capacity of the reaction vessel. Were found that the La1..xSrxMnO3 manganites had a tetragonal perovskite structure with particle sizes in the range of 0.2 - 8 mm with irregular morphology. The size of this particles were dependent of the KOH concentration used in the synthesis, It was found that the enhancement of the KOH concentration results in smaller size particles. Others factors as synthesis time and filling percentage have not a significative effect on the manganite morphology. The magnetic measurements of the compounds La0.6Sr0.4MnO3, La0.5Sr0.5MnO3 and La0.4Sr0.6MnO3 show that these compounds present a typical ferromagnetic behavior below their Tc and the compound La0.4Sr0.6MnO3 has an antiferromagnetic behavior below 200K.

Made available in DSpace on 2014-06-11T19:23:26Z (GMT). No. of bitstreams: 0 Previous issue date: 2009-08-24Bitstream added on 2014-06-13T19:29:24Z : No. of bitstreams: 1 silva_ca_me_bauru.pdf: 3461984 bytes, checksum: 726a1953418403989a2dac8b2bceb4e3 (MD5) / As manganitas óxidas apresentam um complexo diagrama de fases magnéticas e muitos dos seus mecanismos fundamentais de interação magnética ainda precisam ser explorados. A nível cristalográfico, as manganitas óxidas de terras-raras têm suas propriedades magnéticas fortemente afetadas pela variação do íon de terra na estrutura cristalina do composto, pela natureza do elemento de transição presente na composição e pela possibilidade deste metal sofrer flutuações de valência. Além disso, a natural ocorrência de vacâncias de oxigênio também presentes nesses materiais cerâmicos são responsáveis por respostas magnéticas distintas. Este trabalho teve como objetivo a síntese, a caracterização estrutural e a caracterização magnética de dois conjuntos de amostras policristalinas da família Er'Co IND. x''Mn IND. 1-x''O IND> 3+ou - δ' preparados pelo Método dos Precursores Poliméricos. O primeiro conjunto apresenta diferentes valores das composições relativas de manganês e cobalto e um segundo conjunto apresenta variações na estequiometria de oxigênio, além dos compostos base ErMn'O POT. 3' e ErCo'O POT. 3'. Para a caracterização cristalográfica, as amostras foram estudadas por difração de Raios X e analisadas através do método de refinamento Rietveld, e a caracterização magnética foi feita por medidas de magnetização em função da temperatura e em função do campo magnético aplicado. Da análise estrutural, tem-se que as amostras produzidas possuíam frações muito pequenas de fases secundárias, sendo que as fases foram quantificadas através do método Rietveld. As medidas magnéticas mostraram a extensa coexistência de diferentes respostas magnéticas para as amostras com composição relativa Co/Mn. / Manganese based oxides present a very complex magnetic phase diagram and still have many of their basic physical properties and magnetic interaction to be better explored. At crystallographic level, rare-earth oxide manganites have their magnetic properties strongly effected by tchanges in the rare-earth ion present in the structure, the nature of the transition element in the structure and also by the possibility of electronic valence fluctuations. Furthermore, the occurrence of oxygen vacancies are also responsible for a sort of different magnetic responses. In this work it was studied the synthesis procedure, structural and magnetic characterization of polycrystalline samples of the ErMn'O POT. 3' e ErCo'O POT. 3' family prepared by a polymeric precursors method. A first group of samples presents different manganese and cobalt contents ratio and a second group of the analized samples presents variations in the oxygen stoichiometric. The structural and crystalographic characterization were performed by X ray powder diffraction and further analyzed by the Rietveld refinement method, and the magnetic characteristic were studied by measurements of magnetization as a function of temperature at different values of applied magnetic field. From structural analysis, the produced sample have a small piece of secondary phase, that were quantifity using the Rietveld method. The magnetic measures showed a larger coexistence of differents magnetics interactions to sample with relative composition Co/Mn.

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Orientador: Sergio Gama / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Fisica Gleb Wataghin / Made available in DSpace on 2018-08-09T01:21:06Z (GMT). No. of bitstreams: 1 Rocco_DanielLeandro_D.pdf: 7791593 bytes, checksum: 4428135e865b15fec8e5338713adba04 (MD5) Previous issue date: 2006 / Resumo: No presente trabalho são apresentados os resultados da avaliação do Efeito Magnetocalórico (EMC) das cerâmicas manganitas e do intermetálico La(Fe,Si)13. Para as manganitas foram produzidas amostras do tipo Tr1-x Mx MnO3(com Tr = terra-rara e M = alcalino-terroso). Em alguns conjuntos de amostras variou-se a quantidade x, ou seja, mudou-se a relação entre o Mn3+ e Mn 4+. Em outro conjunto a quantidade x era fixada em 0,4 e fazia a substituição da terra-rara pelo alcalino-terroso. Isto tinha como efeito a alteração do valor do raio iônico médio do sítio A <rA>. As amostras obtidas foram caracterizadas por difração de raios-X com refinamento Rietveld, metalografia óptica, e medidas magnéticas. Estas últimas permitiram o cálculo do EMC, que foi avaliado em função de x e de <rA>. Chegou-se a conclusão que à medida que < rA> diminuí há um aumento do acoplamento spin-rede que promove uma mudança do caráter da transição magnética de segunda para primeira ordem, provocando, portanto, um aumento do EMC. O outro material estudado foi o sistema metálico La(Fe,Si)13, cujo método de obtenção é por meio de fusão em forno a arco. Na verdade, é assim que todos os trabalhos da literatura sugerem preparar esta liga. Porém, descobriu-se neste trabalho de doutorado um intervalo de imiscibilidade, ainda não reportado na literatura, que origina-se no sistema binário La-Fe, e se expande para a liga ternária. Este fato tem implicações importantíssimas, pois comprova que apenas pelo processo de fusão da liga não é possível a obtenção deste material de forma monofásica. Então, se propõe uma nova forma de preparação do material que consiste na fusão em forno a arco com uma posterior pulverização das amostras e um tratamento térmico por longos períodos em atmosfera inerte / Abstract: In the present work we show the results of the Magnetocaloric effect evaluation for ceramics manganites and for La(Fe,Si)13 intermetallic. The manganites sample produced were of Tr1-x Mx Mn O3 (Tr = rare-earth and M = alkaline earth) type. In one sample group it was changed the quantity x, or equivalently, the relation between the Mn3+ and Mn4+. On the other sample set, the x amount was fixed in 0.4 and the replacement was from the rare-earth to alkaline earth. This had as effect the variation of the value of the average ionic radius (<rA>) of site A. The samples that obtained were characterised by x-Rays diffraction with Rietveld analyses, optic metallographic and magnetic measurements. The latter made possible the calculation of the MCE, which was evaluated as a function of x and < rA>. We conclude that as soon as <rA> diminishes there is an increase of the spin-lattice coupling that promotes a change in the magnetic transition order, causing, than, an increase of MCE. The second material studied was the metallic system La(Fe,Si )13, which preparation method is by arc-melting. In fact, in other works this material was obtained using this technic, but it was discovered in this Ph. D. work an immiscibility interval, until now not reported. This miscibility gap has its origin in the binary La-Fe phase diagram, and it extends for ternary alloy. This fact has an important implication, because it shows that with only the fusion process of the alloy it is impossible to obtain a single phase material. So, we propose a new way for material preparation that consists in the arc-melting with followed by sample milling and heat-treatment for a long time in an inert atmosphere / Doutorado / Física da Matéria Condensada / Doutor em Ciências

Complex magnetic oxides represent a unique intersection of immense technological importance and fascinating physical phenomena originating from interwoven structural, electronic and magnetic degrees of freedom. The resulting energetically close competing orders can be controllably selected through external fields. Competing interactions and disorder represent an additional opportunity to systematically manipulate the properties of pure magnetic systems, leading to frustration, glassiness, and other novel phenomena while finite sample dimension plays a similar role in systems with long-range cooperative effects or large correlation lengths. A rigorous understanding of these effects in strongly correlated oxides is key to manipulating their functionality and device performance, but remains a challenging task. In this dissertation, we examine a number of problems related to intrinsic and extrinsic low dimensionality, disorder, and competing interactions in magnetic oxides by applying a unique combination of standard magnetometry techniques and unconventional magnetocaloric effect and transverse susceptibility measurements. The influence of dimensionality and disorder on the nature and critical properties of phase transitions in manganites is illustrated in La0.7Ca0.3MnO3, in which both size reduction to the nanoscale and chemically-controlled quenched disorder are observed to induce a progressive weakening of the first-order nature of the transition, despite acting through the distinct mechanisms of surface effects and site dilution. In the second-order material La0.8Ca0.2MnO3, a strong magnetic field is found to drive the system toward its tricritical point as competition between exchange interactions in the inhomogeneous ground state is suppressed. In the presence of large phase separation stabilized by chemical disorder and long-range strain, dimensionality has a profound effect. With the systematic reduction of particle size in microscale-phase-separated (La, Pr, Ca)MnO3 we observe a disruption of the long-range glassy strains associated with the charge-ordered phase in the bulk, lowering the field and pressure threshold for charge-order melting and increasing the ferromagnetic volume fraction as particle size is decreased. The long-range charge-ordered phase becomes completely suppressed when the particle size falls below 100 nm. In contrast, low dimensionality in the geometrically frustrated pseudo-1D spin chain compound Ca3Co2O6 is intrinsic, arising from the crystal lattice. We establish a comprehensive phase diagram for this exotic system consistent with recent reports of an incommensurate ground state and identify new sub-features of the ferrimagnetic phase. When defects in the form of grain boundaries are incorporated into the system the low-temperature slow-dynamic state is weakened, and new crossover phenomena emerge in the spin relaxation behavior along with an increased distribution of relaxation times. The presence of both disorder and randomness leads to a spin-glass-like state, as observed in γFe2O3 hollow nanoparticles, where freezing of surface spins at low temperature generates an irreversible magnetization component and an associated exchange-biasing effect. Our results point to distinct dynamic behaviors on the inner and outer surfaces of the hollow structures. Overall, these studies yield new physical insights into the role of dimensionality and disorder in these complex oxide systems and highlight the sensitivity of their manifested magnetic ground states to extrinsic factors, leading in many cases to crossover behaviors where the balance between competing phases is altered, or to the emergence of entirely new magnetic phenomena.

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