Este trabalho investiga a obtenção de nanopartículas (NP) de óxido de ferro por coprecipitação, sua estabilização com surfactantes e caracterização quanto à morfologia e comportamento magnético. Atualmente, as NP estão sendo amplamente utilizadas para aplicações biomédicas, tais como contraste em imagens médicas e sistema de distribuição de drogas. Na síntese das NP foram investigados, parâmetros como a temperatura da reação, o pH da solução e a velocidade de agitação. O estudo da estabilidade comparou dois diferentes surfactantes: o ácido oleico (AO) e o polietileno glicol (PEG). As NP obtidas foram caracterizadas por difração de raios X (DRX), e quanto à sua morfologia por microscopia eletrônica por varredura (MEV) e microscopia eletrônica de transmissão (MET), a qual também proporcionou uma distribuição de tamanho de partículas, com variação entre 5 nm e 10,23 nm. A interação entre o óxido de ferro e seus revestimentos foi caracterizada por espectrocopia no infravermelho (FTIR) e espectrocopia Raman. O comportamento magnético das NP foi caracterizado por magnetometria de gradiente de força alternada (AGFM) e espectroscopia Mössbauer. Os resultados revelaram que as NP de óxido de ferro são tipicamente constituídas por magnetita ( ) revestida com AO e PEG e com um tamanho médio de cristalito entre 4,6 e 19,2 nm, calculado através da equação de Scherrer. O AGFM mostrou que as propriedades magnéticas das partículas foram mais eficientes para as NP com revestimento, do que com as NP sem revestimento, e o valor de magnetização de saturação (M) para a revestida com PEG foi maior quando comparado com a revestida com AO. A espectroscopia Mössbauer foi utilizada para confirmação do óxido de ferro como , para estimar tamanho de partícula quando os espectros são medidos a baixa temperatura e para análise do comportamento superparamagnético das partículas. / This work investigates the obtained nanoparticles (NP) iron oxide by coprecipitation stabilization with surfactants and characterize the morphology and magnetic behavior. Currently, the NP are being widely used for biomedical applications such as contrast in medical imaging and drug delivery system. In the synthesis of NP were investigated parameters such as the reaction temperature, the pH and stirring speed. The stability study compared two different surfactants: oleic acid (OA) and polyethylene glycol (PEG). The NP were characterized by X-ray diffraction (XRD), and morphologically by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), which also provided a distribution of particle size, ranging from 5 nm and 10.23 nm. The interaction between the iron oxide and their coatings was characterized by infrared spectroscopy (FTIR) and Raman spectroscopy. The magnetic behavior of NP was characterized by magnetometry alternating gradient force (AGFM) and Mössbauer spectroscopy. The results show that the NP iron oxide are typically comprised of magnetite ( ) coated with PEG and AO and a crystallite size between 4.6 and 19.2 nm calculated by the Scherrer equation. The AGFM showed that the magnetic properties of the particles were more efficient for the NP uncoated than to NP coated, and the value of saturation magnetization (M) to coated with PEG was higher when compared to coated AO. Mössbauer spectroscopy was used to confirm the iron oxide as , to estimate the size of particle where the spectra are measured at low temperature and to analyze the behavior of superparamagnetic particles.

Orientador: Marco Antonio Bica de Moraes / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Fisica Gleb Wataghin / Made available in DSpace on 2018-08-06T01:12:05Z (GMT). No. of bitstreams: 1 Gadioli_GiovanaZanini_M.pdf: 816711 bytes, checksum: 5d38a2c08f13049d8af5fd4659ded22e (MD5) Previous issue date: 2006 / Resumo: As propriedades de filmes obtidos por co-deposição de um material ferromagnético e um não-magnético são objetos de intensa investigação. Neste trabalho, foram investigadas as propriedades de filmes Gdx W1-x, com x variando de 0 a 1. Os filmes foram depositados por magnetron-sputtering a partir de alvos de Gd e W. Para a análises dos filmes foram usadas as técnicas EPMA (microanálise eletrônica) e difratometria de raio-x de baixo ângulo para determinar a composição atômica e a estrutura cristalina, respectivamente. O momento magnético, m , de cada filme foi medido em função da temperatura, T, e do campo magnético aplicado, H, usando um magnetômetro SQUID (superconducting quantum interference device). Os filmes são amorfos para para 0,15 < x < 0,85, mas a coercividade foi observada em todos as amostras. A partir das curvas m vs T, foi observado um forte ordenamento magnético para T < TB. Para T > T B as amostras se mostram paramagnéticas. Os valores de T B foram observados em baixa temperatura (entre 5 e 50 K). A temperatura de Curie-Weiss, deduzida a partir das curvas x -1 vs T, onde x é a suscetibilidade, aumentaram com x. O efeito magnetocalórico foi estudado a partir das isotermas de magnetização, M vs H, das quais a variação de entropia magnética, D S M, foi obtida. As curvas D SM vs T exibiram máximos que variam entre 5 K e temperatura ambiente, dependendo da proporção de Gd / Abstract: The magnetic properties of films obtained by the co-deposition of a ferromagnetic and a non-magnetic components are the subject of intense investigation. In this work, the magnetic properties of Gdx W1-x, with x ranging from 0 to 1, were investigated. The films were deposited by magnetron sputtering from Gd and W targets. EPMA (electron probe microanalysis) and low-angle XRD (x-ray diffraction) were used to determine the film atomic composition and structure, respectively. The magnetic moment, m , of the films was measured as a function of temperature, T, and applied field H, using a SQUID (superconducting quantum device) magnetometer. The films were amorphous for 0.15 < x < 0.85 but coercivity was observed in all samples. From plots of m vs T, a strong magnetic ordering was observed for T < TB. For T > T B the samples were paramagnetic. TB-values occurred at low temperatures (between 5 K and 50 K). The Curie paramagnetic temperature, deduced from the x -1 vs T plots, where x is the susceptibility, was observed to increase with increasing x. The magnetocaloric effect was investigated from the magnetization isotherms, M vs H, from which the magnetic entropy change, D SM, caused by the application and removal of a 50 kOe field, was deduced. The D SM vs T curves exhibited maxima which varied from 5 K to about room temperature, depending on the Gd concentration / Mestrado / Física da Matéria Condensada / Mestre em Física

Made available in DSpace on 2014-07-29T15:12:45Z (GMT). No. of bitstreams: 1 Dissertacao Frederico Costa e Silva.pdf: 3291815 bytes, checksum: 2ee5afa45a0edf1283c63ca3496727b8 (MD5) Previous issue date: 2011-04-15 / The nanoscience and nanotechnology exhibited an outstanding development, which have been caused by the unusual properties featured by materials in the nanometric regime. Because of this, many magnetic materials with sizes smaller than before have been studied; among these materials, the ferrites have been extensively researched in new applications as drug carriers and ferrofluid components. In this work cobalt magnesium mixed ferrites, Co1-xMgxFe2O4 where 0 &#8804; x &#8804; 0.6, were synthesized by the forced hydrolysis method, which involves the hydrolysis of precursor salts mixed in a organic medium under mild heating. The structural characterization of the obtained materials was done by X-Ray Diffraction (DRX) and Transmission Electron Microscopy (MET); beyond these, the materials were characterized by Infrared Spectroscopy (FTIR), Thermogravimetry (TG) and Differential Thermal Analysis (DTA). The magnetic characterization was done in a Vibrating Sample Magnetometer (VSM), in applied fields varying from -2 to +2 Tesla and at 273, 323 and 373 K temperatures, and in a Physical Properties Measuring System (PPMS) operating in a temperature range of 4 to 300 K. The synthesized materials featured the characteristic spinel structure from ferrites, low crystallinity and average crystallite diameter below 5 nm. The presence of organic residues from the synthetic step was detected and quantified in the samples; beyond this, an increase of crystallinity of the material was observed when this is thermally treated. Using the room temperature and above room temperature magnetization curves of the samples, the superparamagnetic behavior was detected and confirmed. The saturation magnetization of the samples at room temperature were 260.29, 237.42, 198,27, 191.25 e 161.49 emu/cm3 to the samples with x =0, 0.2, 0.4, 0.5 e 0.6, respectively; then, the substitution of Co2+ with Mg2+ caused the decrease of saturation magnetization of the synthesized samples. The samples Blocking Temperature (TB) were obtained of the Zero Field Cooling (ZFC) and Field Cooling (FC) curves, and, with those values, the Effective Anisotropy Constants (Kef) of each sample were calculated; the obtained values were 196 K and 1.41 x 107 ergs/cm3 to the x = 0 sample; 178 K and 1.28 x 107 ergs/cm3 to the x = 0.2 sample; 172 K and vi 1.24 x 107 ergs/cm3 to the x = 0.4 sample; 172 K and 1.24 x 107 ergs/cm3 to the x = 0.5 sample and 146 K and 1.05 x 107 ergs/cm3 to the x = 0.6 sample. The trend featured by the obtained TB and Kef values was directly associated with the Ms trend. A comparison of the Anisotropy Constants between the x = 0 sample, a bulk and a 8.5 nm diameter cobalt ferrite were also done; among these, the x = 0 sample featured a higher value of Kef, therefore, the x = 0 sample anisotropy energy seems to be composed by superficial and interparticle magnetic effects contributions besides the magnetocrystalline energy contribution. / A nanociência e a nanotecnologia têm apresentado um grande crescimento devido às novas propriedades exibidas por materiais em regime nanométrico. Por isso, materiais magnéticos com tamanhos cada vez menores têm sido estudados; dentre estes materiais, as ferritas têm sido extensivamente pesquisadas em novas aplicações como carreadoras de fármacos e composição de ferrofluidos. Neste trabalho ferritas mistas de cobalto e magnésio, Co1-xMgxFe2O4 onde 0 &#8804; x &#8804; 0,6, foram sintetizadas através do método de hidrólise forçada, que envolve a hidrólise de uma mistura de sais precursores em um meio orgânico a médias temperaturas. A caracterização estrutural dos materiais obtidos foi realizada por Difração de Raios-X (DRX) e Microscopia Eletrônica de Transmissão (MET); ainda foram realizadas análises de Espectroscopia de Infravermelho (FTIR), de Termogravimetria (TG) e de Análise Térmica Diferencial (DTA). A caracterização magnética destes materiais foi realizada em um Magnetômetro de Amostra Vibrante (VSM), com campos aplicados de -2 a +2 Tesla e temperaturas de 273, 323 e 373 K, e em um Sistema de Medidas de Propriedades Físicas (PPMS), em temperaturas de 4 a 300 K. Os materiais sintetizados apresentaram estrutura de espinélio com baixa cristalinidade e diâmetros médios de cristalito menores que 5 nm. A presença de resíduos orgânicos provenientes da etapa de síntese foi detectada e quantificada nas amostras; além disso, observou-se um aumento da cristalinidade das mesmas quando tratadas termicamente. Através das curvas de magnetização a temperatura ambiente das amostras, observou-se que as mesmas apresentavam superparamagnetismo. Os valores de Magnetização de Saturação (Ms) a temperatura ambiente foram de 260,29, 237,42, 198,27, 191,25 e 161,49 emu/cm3 para as amostras com x =0, 0,2, 0,4, 0,5 e 0,6, respectivamente; logo a substituição de íons Co2+ por Mg2+ causa a diminuição da magnetização de saturação das amostras. Através de curvas de Zero Field Cooling (ZFC) e Field Cooling (FC) os valores das Temperaturas de Bloqueio (TB) e, consequentemente, das Constantes de Anisotropia Efetiva (Kef) das amostras foram obtidos; estes valores foram de, respectivamente, 196 K e 1,41 x 107 ergs/cm3 para a amostra com x = 0; 178 K e 1,28 x 107 ergs/cm3 iv para a amostra com x = 0,2; 172 K e 1,24 x 107 ergs/cm3 para a amostra com x = 0,4; 172 K e 1,24 x 107 ergs/cm3 para a amostra com x = 0,5 e 146 K e 1,05 x 107 ergs/cm3 para a amostra com x = 0,6. Todos os valores de TB e de Kef obtidos decresceram frente ao aumento da concentração de Mg2+, o que foi explicado em termos da diminuição de Ms ao longo da série de amostras. Uma comparação entre os valores de constante de anisotropia foi feita para a amostra x = 0, a ferrita de cobalto no estado bulk e nanopartículas de ferrita de cobalto com 8,5 nm de diâmetro; visto que o valor desta constante é consideravelmente maior para a amostra x = 0 conjecturou-se que as contribuições de superfície e de interações magnéticas entre partículas à energia de anisotropia sejam maiores para a amostra x= 0 do que para as nanopartículas de CoFe2O4 usadas na comparação.

Orientador: Marcelo Knobel / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Fisica Gleb Wataghin. / Made available in DSpace on 2018-08-12T12:15:41Z (GMT). No. of bitstreams: 1 LeonVanegas_AlvaroAugusto_M.pdf: 1938062 bytes, checksum: c09af0b2555e73ce9f9d903c4094424c (MD5) Previous issue date: 2008 / Resumo: Neste trabalho estudamos o comportamento magnético de uma amostra de nanopartículas de níquel com alto grau de desordem estrutural com uma distribuição estreita de diâmetros. Encontramos que o sistema apresenta duas fases magnéticas, uma paramagnética, que segue uma lei tipo Curie-Weiss com constante de Curie C = 3, 36 × 10-3emuK/gOe e temperatura crítica de TC = 8, 5 K e outra ferromagnética que não segue o comportamento superparamagnético clássico a altas temperaturas e provavelmente é originada pela formação de pequenos clusters que são os responsáveis pela irreversibilidade observada por baixo dos 23 K nos dados de magnetização FC-ZFC a 50 Oe. Os dados obtidos de Magnetização FC mostram um aumento abrupto da magnetização em 23 K relacionada com o crescimento e criação de novos clusters e estes, devido a interações de tipo dipolar e de troca e a uma forte anisotropia superficial, geram estados frustrados tipo vidro de spin que se refletem na queda na magnetização em 17 K. Em 7 K os restantes spins superficiais que não haviam se incorporado aos clusters ferromagnéticos da partícula tentam-se ordenar. Os dados dos ciclos de histereses confirmam a forte anisotropia superficial e a presença de uma grande porcentagem de spins não ordenados na superfície. / Abstract: We have studied the magnetic behavior of amorphous nickel nanoparticles sample with size narrow distributions. We find that the system have two magnetic phases, one paramagnetic, that follows the Curie-Weiss law with C = 3.36×10-3emuK/gOe and TC= 8.5 K and other ferromagnetic that not follows the classic superparamagnetic behavior to high temperatures and is probably result of small clusters formation, who are the responsibles of observed irreversibility in the Field Cooled magnetization data with magnetic field of 50 Oe. The obtained data of MFC shows a strong increase in the magnetization in 23 K related with the growth and the appearance of new clusters, and these, due to dipolar and exchange interactions and strong surface anisotropy, generates frustrate spin-glass-like states that lead up to a decrease in magnetization at 17 K . At 7 K the system begins to order the remaining superficial spins that are outside the ferromagnetic part of the particle. The histeresis data confirm a strong surface anisotropy and a considerable part of no ordered spins on the surface. / Mestrado / Materiais Magneticos e Propriedades Magneticas / Mestre em Física

Les travaux effectués dans cette thèse concernent la mécanique des gels d'actine branchés in vitro ainsi que leur processus de génération de forces contre des parois. Pour étudier ces effets, nous avons développé un nouveau montage expérimental, basé sur des mesures via l'auto assemblage de microcylindres superparamagnétiques sous un champ magnétique. Cela nous permet d'en déduire les relations entre force et vitesse des réseaux d'actine branchés, ainsi que de faire le lien entre force et mécanique, des sujets cruciaux en mécanique et en migration cellulaire. / The work done during this tesis concerns the mechanics and force generation processes of branched actin networks reconstructed in vitro. To study these effects, we’ve developped a new experimental setup, based on self assembly of supermaramagnetic microcylinders under a magnetic force. This allows us to obtain relations between force and growth velocity of branched actin networks, as well as linking force generation with mechanics, which are crucial to understand cell mechanics and migration.

Orientador: Marcelo Knobel / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Física Gleb Wataghin / Made available in DSpace on 2018-08-30T18:13:51Z (GMT). No. of bitstreams: 1 OrozcoHenao_JuanManuel_M.pdf: 7687296 bytes, checksum: d9aecf2d118aed0c43ab747d0dcff34c (MD5) Previous issue date: 2016 / Resumo: Nanopartículas de magnetita com diâmetros entre 5nm e 19nm sintetizadas mediante um método de decomposição térmica são apresentadas. A caracterização estrutural é feita usando diferentes técnicas experimentais como a microscopia eletrônica de transmissão (TEM), difração de raios-X e espalhamento de raios-X a baixos ângulos (SAXS) de onde são obtidos os tamanhos e a forma das nanopartículas. As propriedades magnéticas e de magneto-hipertermia das nanopartículas são estudadas para diferentes parâmetros de produção como concentração dos surfactantes, temperaturas de refluxo e atmostfera de crescimento. A dependência com a temperatura das propriedades magnéticas são analisadas dentro do marco do modelo usual do superparamagnetismo e o modelo de interação superparamagnética (ISP), de onde os parâmetros magnéticos dependentes do tamanho como anisotropia magnética (1.06x10^4 J/m^3 até 9.91x10^4 J/m^3), momento magnético por partícula (2618?B até 11500?B), temperatura de bloqueio (18K até mais de 300K) e energia de ineração dipolar magnética (0.55x10^-21 J até 5.5x10^-21 J) são inferidos. Os resultados de magneto-hipertermia foram obtidos mediante a medição da resposta térmica das nanopartículas de magnetita suspendidas em tolueno. Valores da taxa de absorção específica (SAR) são calculados experimental e teoricamente utilizando a teoria de resposta linear para um sistema superparamagnético não interagente. Valores de SAR entre 3.0W/g e 40.3W/g e a sua dependência com a frequência e o campo aplicado são apresentados. Como resultado interessante, a resposta de magneto-hipertermia para as nanopartículas de 19nm preparadas na presença de oxigênio e mais de 10 vezes maior do que nanopartículas similares mas obtidas na ausência da atmosfera de oxigênio. Também é destacada a possibilidade de prever a resposta de magneto-hipertermia num sistema de nanopartículas magnéticas mediante a obtenção dos parâmetros de caracterização magnetica e estrutural / Abstract: Magnetite nanoparticles with diameters between 5nm and 19nm synthesized by means of a thermal decomposition method are presented. Structural characterization is made by different experimental techniques such as transmission electron microscopy (TEM), X-ray diffraction and Small Angle X-ray Scattering (SAXS) from where nanoparticles size and shape are obtained. Magnetic and magneto-hyperthermia properties of the nanoparticles are studied for different production parameters, such as surfactant concentrations, refluxing temperature and growth atmosphere. Temperature dependence of the magnetic properties are analyzed in the framework of the standard superparamagnetism model and the interacting superparamagnetic model (ISP), from where size dependent magnetic parameters for each sample such as anisotropy (1.06×10^4 J/m^3 to 9.91x10^4 J/m^3) magnetic moment per particle (2618?B to 11500?B), blocking temperature (18K to above 300K) and magnetic dipolar interaction energy on dried nanoparticle samples (0.55 × 10^?21 J to 5.5 × 10^?21 J) are inferred. Magneto-hyperthermia results are obtained by measuring the thermal response of magnetite nanoparticles dissolved in toluene. Specific absorption rate (SAR) values are theoretically and experimentally calculated by means of a linear response theory approach of a non-interacting superparamagnetic system. SAR values between 5.8W/g and 40.3W/g are reported; interestingly, the magneto-hyperthermia response for 19nm nanoparticles prepared in presence of an oxygen atmosphere is more than 10 times larger than similar particles obtained in absence of oxygen atmosphere. Also it is important to highlight the possibility to obtain the magneto-hyperthermia behavior of a magnetic nanoparticles system by knowing a priori its structural and magnetic characterization parameters / Mestrado / Física / Mestre em Física / 1247647/2013 / CAPES

The aim of the work is characterization of structure and magnetic properties of various CoFe2O4/SiO2 nanocomposites. Emphasis was put on the corelation of the magnetic properties with particle size (samples with different annealing temperature) and with strenght of the interparticle interactions (samples with different Fe/Si ratio or without silica matrix). Structure properties of all samples were determinated by powder x-ray diffraction, scanning and transmission electron microscopy. Magnetic properties were determinated by standard (temperature dependence of magnetization, magnetization isotherms) and advanced (a.c. susceptibility, memory effects) magnetic measurements. A sharp increase of the values of blocking temperature and coercivity with increase of strenght of the interparticle interactions and with increase of particle size was observed. Particle size determines the maximum value of coercivity and blocking temperature and strengh of the interparticle interactions shift this values in the interval determined by particle size.

Title: NMR in magnetic systems Author: Petr Křišťan Department: Department of Low Temperature Physics Supervisor: prof. RNDr. Helena Štěpánková, CSc. Abstract: Magnetically ordered iron oxides, namely magnetite, maghemite, hexagonal ferrite M or system Fe-B, with nano or submicron dimensions of particles are the main subject of study of the presented thesis. The materials were investigated mainly by 57 Fe nuclear magnetic resonance (NMR). The results were thoroughly analyzed and compared with the results obtained by other methods (Mössbauer spectroscopy, ZFC/FC magnetic measurement, X-ray diffraction or TEM). In case of the maghemite nanoparticles a regular distribution of vacancies in octahedral positions was verified by the help of NMR in external magnetic fields and at various temperatures. The experi- mental results were also compared with ab-initio calculations. In thin layers of barium M type hexaferrite, effects of reduced particle size on 57 Fe NMR spectra were observed. The NMR methods were also successfully applied to investigation of system FeMoCuB of amorphous and nanocrystalline ribbons, where 57 Fe NMR was able to resolve formation of different phases in depen- dence on the process of preparation. Due to different NMR excitation condi- tions of signal from strontium M type hexaferrite and maghemite,...

Fe3O4 magnetic nanoparticles of 5 to 11 nm in size were prepared by organic methods. Particle size was analyzed by both X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM) techniques. Zero Field Cooling (ZFC) / Field Cooling (FC) and magnetization loop measurements were recorded by VSM, and they confirmed superparamagnetic behavior in the sample. The blocking temperature is found to be in the range of 30 K ~ 170 K. It has a dependence on the particle size. ZFC / FC curves also indicate the presence of magnetic coupling between particles. X-ray Magnetic Circular Dichroism (XMCD) measurements of these nanoparticles were measured at 80 K and 300 K. By using the sum rules, spin and orbital magnetic moments were calculated from the XMCD signal. The results confirm a quenching orbital moment and a large spin moment. The calculated total magnetic moments are somewhat smaller than in bulk Fe3O4. Also, the spin moment at 80 K was found to be larger than at 300 K. X-ray Resonant Magnetic Scattering (XRMS) measurements at different temperatures, polarizations and fields were carried out. The intensity profile gives information on the interparticle distance between nanoparticles which is consistent with TEM results. A magnetic signal was extracted by calculating the dichoroic term, when the energy is tuned to resonant edges. This magnetic signal is confirmed by comparing the dichroic terms at different conditions.

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