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Building crystals out of crystals : Synthesis, structure and magnetic properties of iron oxide nanoparticles and self-assembled mesocrystalsWetterskog, Erik January 2013 (has links)
This thesis is focused on the fabrication and characterization of self-assembled arrays of magnetic iron oxide (Fe3O4, γ-Fe2O3 and Fe1-xO) nanoparticles. The synthesis of spherical and cubic iron oxide nanocrystals, with sizes between 5 and 30 nm and narrow size distributions, is demonstrated, along with a rigorous morphological characterization of the cubic nanoparticles. The transformation of core|shell Fe1-xO|Fe3-δO4 particles into single-phase Fe3-δO4 particles is studied in detail. It is found that anti-phase boundaries in the particles result in the emergence of anomalous magnetic properties i.e. exchange bias, and a reduced saturation magnetization compared to that of bulk Fe3O4. Cubic nanocrystals are assembled into arrays possessing an exceptionally high degree of translational ordering and a high degree of crystallographic alignment. A combination of electron microscopy and small-angle X-ray scattering is used in the characterization of the 3D nanostructures. The directional (anisotropic) interactions in the 3D structures are modeled in an attempt to find a link between the nanocrystal morphology and the corresponding mesostructure. Here, the cohesive van der Waals energy is estimated for a system of nanocubes with a variable truncation. The assembly of nanocubes in magnetic fields of various strengths is systematically investigated. A perturbed mesocrystal growth habit is observed at intermediate fields, whereas at high field strengths, the assembly is dominated by ferrohydrodynamic instabilities. Last, magnetometry is used to study the collective magnetic properties of self-assembled nanocrystals. The magnetic susceptibility in a weak magnetic field is studied as a function of film thickness and particle size. An increase in the tendency to form ferromagnetic couplings with decreasing film thickness can be established. This 2D to 3D crossover of the magnetic properties of the nanoparticle arrays can be related to a change in the magnetic vortex states.
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SYNTHESIS AND CHARACTERIZATION OF MAGNETIC HYDROGEL NANOCOMPOSITES FOR CANCER THERAPY APPLICATIONSMeenach, Samantha Ann 01 January 2010 (has links)
Currently, cancer is the second leading cause of death in the United States. Conventional cancer treatment includes chemotherapy, radiation, and surgical resection, but unfortunately, all of these methods have significant drawbacks. Hyperthermia, the heating of cancerous tissues to between 41 and 45°C, has been shown to improve the efficacy of cancer therapy when used in conjunction with irradiation and/or chemotherapy. In this work, a novel method for remotely administering heat is presented. This method involves heating of tumor tissue using hydrogel nanocomposites containing magnetic nanoparticles which can be remotely heated upon exposure to an external alternating magnetic field (AMF). The iron oxide nanoparticles contained in the hydrogel nanocomposites are able to heat via an AMF due to Brownian and Neel relaxation processes. The administration of hyperthermia via hydrogel nanocomposites allows for local delivery of heat to tumor tissue while also providing a drug depot to deliver chemotherapeutic agents. Both in vivo and in vitro studies have demonstrated that numerous chemotherapeutic agents, when used in conjunction with hyperthermia, show improved efficacy in treating cancer
Various magnetic hydrogel nanocomposites were synthesized and characterized for this work including poly(ethylene glycol) (PEG)-based hydrogels, which were studied due to their inherent biocompatibility and “stealth” properties, as well as, poly(β-amino ester) (PBAE)-based hydrogels which have tailorable degradation properties. The PEG hydrogels were investigated for their temperature-responsiveness swelling, mechanical strength, heating capabilities, biocompatibility, ability to kill M059K glioblastoma cells via thermoablation, and the ability to deliver paclitaxel, a chemotherapeutic agent. PBAE hydrogels were also characterized for their degradation and swelling properties, ability to heat upon exposure to an AMF, biocompatibility, mechanical strength, and ability to deliver paclitaxel in a controlled fashion. Additionally, multiple cancer cell lines were exposed to a combination of paclitaxel and heat (at 42.5 °C) in vitro and it was shown that A539 lung carcinoma cells exhibit higher cytotoxicity when exposed to both heat and paclitaxel than either treatment alone. Overall, magnetic hydrogel nanocomposites are promising materials that can be utilized for the multi-modality treatment of cancer through the synergistic delivery of both heat and chemotherapeutic agents.
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Raman Spectroscopy and Hyperspectral Analysis of Living Cells Exposed to NanoparticlesAhlinder, Linnea January 2015 (has links)
Nanoparticles, i.e. particles with at least one dimension smaller than 100 nm, are present in large quantities in ambient air and can also be found in an increasing amount of consumer products. It is known that many nanomaterials have physicochemical properties that differ from physicochemical properties of the same material in bulk size. It is therefore important to characterize nanoparticles and to evaluate their toxicity. To understand mechanisms behind nanotoxicity, it is important to study the uptake of nanoparticles, and how they are accumulated. For these purposes model studies of cellular uptake are useful. In this thesis metal oxide and carbon-based nanoparticles have been studied in living cells using Raman spectroscopy. Raman spectroscopy is a method that facilitates a non-destructive analysis without using any fluorescent labels, or any other specific sample preparation. It is possible to collect Raman images, i.e. images where each pixel corresponds to a Raman spectrum, and to use the spectral information to detect nanoparticles, and to identify organelles in cells. In this thesis the question whether or not nanoparticles can enter the cell nucleus of lung epithelial cells has been addressed using hyperspectral analysis. It is shown that titanium dioxide nanoparticles and iron oxide nanoparticles are taken up by cells, and also in the cell nucleus. In contrast, graphene oxide nanoparticles are mainly found attached on the outside of the cell membrane and very few nanoparticles are found in the cell, and none have been detected in the nucleus. It is concluded that graphene oxide nanoparticles are not cytotoxic. However, a comparison of Raman spectra of biomolecules in cells exposed to graphene oxide, unexposed cells and apoptotic cells, shows that the graphene oxide nanoparticles do affect lipid and protein structures. In this thesis, several multivariate data analysis methods have been used to analyze Raman spectra and Raman images. In addition, super-resolution algorithms, which originally have been developed to improve the resolution in photographic images, were optimized and applied to Raman images of cells exposed to submicron polystyrene particles in living cells.
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Engineering behavior and characterization of physical-chemical particulate mixtures using geophysical measurement techniquesChoo, Hyunwook 27 August 2014 (has links)
Natural geomaterials exhibit a wide range in size, physical properties, chemical properties, and mechanical behaviors. Soils that are composed of mixtures of particles with different physical and chemical properties pose a challenge to characterization and quantification of the engineering properties. This study examined the behavior of particulate mixtures composed of differently sized silica particles, mixtures composed of aluminosilicate and organic carbon particles, and mixtures composed of particles with approximately three orders of magnitude difference in particle size. This experimental investigation used elastic, electromagnetic, and thermal waves to characterize and to quantify the small to intermediate strain behavior of the mixtures.
The mechanical property of stiffness of mixed materials (e.g. binary mixtures of silica particles and fly ashes with various carbon and biomass contents) was evaluated through the stiffness of active grain contacts, and the stiffness of particles which carry applied load, using the physical concepts of intergranular void ratio and interfine void ratio. Additionally, the change in both contact mode/stiffness and electrical property due to the presence of nano-sized particles (i.e., iron oxides) on the surface of soil grains was evaluated according to applied stress, packing density, iron coating density, and substrate sand particle size. Finally, the biomass fraction and total organic carbon content of mixtures was used to quantify the electrical and thermal conductivities when particulate organic was mixed with aluminosilicate particles.
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Investigation of Nanoparticles for Use in Microwave Systems in BiomedicineTaghavi, Houra 03 October 2013 (has links)
This research focuses on the microwave properties of nanoparticles for use as contrast and hyperthermia agents. Currently, visible light is used for irradiation of nanoparticles as hyperthermia agents. Additionally, visible/Near-infrared light is used for photoacoustic tomography (PAT) imaging. Compared to optical wavelengths, frequencies in microwave range transmit through tissue with high penetration depth . Thus, deep cancerous cells and malignant tissue may be treated and imaged. These nanoparticles could enable the use of a hybrid microwave/acoustic technique known as thermoacoustic tomography.
Here, quantitative measurements of the heat generation in super paramagnetic iron oxide nanoparticle (SPIONs), gold nanoparticles (AuNPs), and gold nanoclusters (AuNCs) induced by microwave energy at 3 GHz, are presented and compared. Based on our experiments, SPIONs are the most efficient nanoparticles for microwave heating. Very high concentrations of SPIONs are able to convert microwave energy into heat about 22° C more than DI-water. AuNPs, which support plasmon resonances, do not provide heat under microwave irradiation as predicted by our computational analysis based on Mie Theory. AuNCs are a new form of ultra-small (<2.5 nm) AuNPs which do not support plasmonic resonances and have supra-molecular properties such as sub-conduction band transitions. Interestingly, AuNCs have the potential to absorb microwave energy and may provide an alternative to SPIONs. These nanoparticles had not yet been studied before in this frequency region. In addition, the absorption coefficient of nanoparticles were calculated using complex permittivity data from a dip probe kit and a Vector Network Analyzer (VNA) in a broad band range from 500 MHZ to 10 GHz. This method allows identification of best frequency region with highest penetration depth. In the last step, the nanoparticles with different concentrations were tested as exogenous contrast agents in a Thermoacoustic Tomography (TAT) system. TAT utilizes the penetration depth of microwave energy while producing high resolution images through acoustic waves. The addition of an exogenous contrast agent improves image quality by more effectively converting microwave energy to heat. The experiment reveals that the time resolved thermoacoustic signal (TA) from SPIONs is stronger than AuNPs and AuNCs and thus, the image contrast produced by SPIONs is stronger than the two other aforementioned nanoparticles.
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Soldering in High Pressure Die Casting and its Prevention by Lubricant and Oxide LayersFraser, Darren Timothy Unknown Date (has links)
Soldering results from the interfacial interactions between the die and the casting alloy during high pressure die casting and is one of the major die failure modes. To prevent this occurring, lubricant layers and surface coatings are used to act as a barrier between the die and the casting alloy. The microstructures of a series of soldered layers on H13 tool steel core pins were examined after conducting high pressure die casting experiments with a specially designed die using removable core pins and Al-11Si-3Cu casting alloy. This showed that first, a casting alloy build-up layer formed, and then intermetallic phases nucleated at the die steel interface and grew to cover the entire surface in subsequent casting cycles. The structures of intermetallic layers formed during immersion of H13 tool steel into an Al-11Si-3Cu casting alloy melt were studied by X-ray diffraction and energy dispersive spectroscopy (EDS). A thick composite layer away from the H13 steel substrate consisted of irregular intermetallic phases and solidified casting alloy. A thin intermetallic layer was present between the composite layer and an inner compact layer next to the steel substrate. The irregular intermetallic phase in the thick composite layer away from the H13 steel substrate was identified to have a body centre cubic (bcc) structure, abcc-( FeSiAlCrMnCu). The thin and continuous intermetallic layer between the composite layer and the inner compact layer was found to be structurally isomorphous with aH-Fe2SiAl8. The compositional differences observed between aH and abcc phases indicated that the latter consisted of a higher amount of chromium, manganese, copper, and a lower amount of iron. It was likely that the presence of chromium, manganese and copper in the H13 tool steel caused the transformation of aH®abcc. The inner compact layer next to the steel substrate was identified to be orthorhombic h-Fe2Al5 containing silicon and chromium. An examination of lubricants to prevent soldering in high pressure die casting in conjunction with Nissan Casting Australia Pty Ltd. found that soldering was reduced by using a suitable lubricant. The chemistry of the lubricant, spray parameters, and die surface temperature were important factors in producing a protective lubricant layer. It was found that lubricant containing polypropylene waxes prevented soldering significantly better than lubricant containing polyethylene waxes. It was also found that the lubricant containing polypropylene waxes had lower surface tension. An examination of the use of iron oxide layers to prevent soldering in high pressure die casting was performed. H13 tool steel was oxidised in air and produced porous iron oxide with a mixture of haematite (Fe2O3) and magnetite (Fe3O4). These porous iron oxides did not completely prevent the H13 steel from soldering in immersion tests as intermetallic cones formed at the surface of the steel. Commercial steam tempering of H13 steel produced more compact iron oxide layers with magnetite (Fe3O4) and haematite (Fe2O3) structures. It was found that these compact iron oxide layers offered better protection against soldering than the porous layers created in air. Pure iron oxidised in a CO2/H2 gas mixture at a ratio of 95:5 at 550°C produced structurally pure, compact magnetite (Fe3O4) layers. H13 steel oxidised in a CO2/H2 gas mixture at a ratio of 95:5 at 550°C produced compact iron oxide layers that showed only magnetite (Fe3O4) structure. The magnetite (Fe3O4) layer containing chromium, manganese, silicon and vanadium formed next to the H13 substrate was found to be a very adherent layer and protected H13 steel from soldering in high pressure die casting experiments with a specially designed die using removable core pins and Al-11Si-3Cu casting alloy. An examination of aluminium oxide layers to prevent soldering in high pressure die casting was performed. Incoloy MA956 containing 4.5 wt.% aluminium, oxidised in air at 1100°C, produced a single, compact, adherent oxide layer with a-alumina (Al2O3) structure, that prevented the formation of intermetallic phases between aluminium alloy and Incoloy MA956 during high pressure die casting. However, non-reactive casting alloy build-up formed on the oxide coatings, similarly to physical vapour deposition (PVD) and vanadium carbide coatings. It was found that the thickness of the non-reactive casting alloy build-up was reduced by decreasing the roughness of the oxide coatings by lightly grinding of the surface of the coatings. The industrial application of these findings are discussed and directions for further research are presented.
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Anaerobic ammonium oxidation (Anammox) coupled with extracellular electron transfer to semiconductive minerals by anammox bacteriaBibiano Guadarrama, Carlos 03 1900 (has links)
No description available.
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Influência do método de preparação nas propriedades do óxido de ferro suportadoMonteiro, Ana Paula de Melo January 2005 (has links)
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Previous issue date: 2005 / O estireno é uma das substâncias químicas básicas mais importantes para produção de valiosos artigos como poliestireno, acrilonitrila-butadieno-estireno e estireno-butadieno-estireno. É produzido comercialmente pela desidrogenação do etilbenzeno com excesso de vapor d’água a temperaturas altas de 600-700ºC. Este processo é termodinamicamente limitado e consome energia. O uso de um oxidante, tal como oxigênio, permite superar as limitações termodinâmicas e por conseguinte operar a temperaturas mais baixas com reação exotérmica. Porém, há uma perda significantiva de seletividade a estireno, assim se buscou outro oxidante por muito tempo. O uso de gás carbônico surge como um potencial oxidante, além da conveniência do uso do gás causador do efeito estufa. Na busca de um catalisador alternativo para esta reação, neste trabalho estudou-se o efeito do método de preparação nas propriedades de óxido de ferro. As amostras foram preparadas incorporando óxido de ferro em lantânia, nióbia, titânia, magnésia e zircônia através de dois métodos: a impregnação de nitrato férrico e a deposição de nanoparticulas de óxido de ferro previamente preparadas. Os sólidos foram calcinados a 600ºC por 4 h e caracterizados por análise química, termogravimetria, análise térmica diferencial, difração de raios X, área de superfície específica e medidas de porosidade e redução a temperatura-programada. Os catalisadores foram avaliados na desidrogenação do etilbenzeno na presença de dióxido de carbono, usando um microreator que opera a 1 atm e a 600ºC e uma relação molar gás carbônico/etilbenzeno de 10. Depois dos testes, as amostras foram caracterizadas por difração de raios X e área de superfície específica. Observou-se que a concentração do óxido de ferro incorporado depende do tipo do suporte e do método de preparação. A hematita foi observada nos catalisadores novos. Durante a desidrogenação do etilbenzeno, os suportes não se alteraram, mas a hematita se transformou em magnetita. Os suportes e os catalisadores são sólidos macroporosos com pequena contribuição de mesoporos. A área específica mudou devido à adição de óxido de ferro e foi influenciada pelo método de preparação. A incorporação das nanoparticulas conduziu a um aumento da área superficial específica, indiferentemente do tipo do suporte, fato que foi atribuído ao tamanho pequeno das partículas. As áreas específicas não se alteraram durante a reação. Os sólidos mostraram diferentes resistência contra redução que se deve ao suporte e ao método de incorporação do óxido de ferro. A impregnação de nitrato férrico produziu sólidos menos redutíveis. Os suportes foram cataliticamente ativos na desidrogenação do etilbenzeno na presença de gás carbônico e também eram seletivos a estireno. A adição de compostos de ferro melhorou estas propriedades e a deposição de nanoparticulas melhoraram ainda mais. O óxido ferro suportado em magnésia, preparado pela deposição de nanoparticulas, foi o mais ativo (2,8 x 10-3 mol.g-1.h-1) e catalisador seletivo a estireno (96%) na desidrogenação do etilbenzeno na presença de gás carbônico. A atividade e a seletividade foram mais altos do que um catalisador comercial à base de óxido de ferro, cromo e potássio (a=1,2 x 10-3 mol. g-1. h-1 e S=90%) , sendo o catalisador promissor na reação. / Salvador
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Incorporação de impurezas pelo método do complexo polimerizado em nanoestruturas de óxido de ferroAguilar, Daniel Angel Bellido January 2015 (has links)
Orientador: Prof. Dr. Flavio Leandro de Souza / Dissertação (mestrado) - Universidade Federal do ABC, Programa de Pós-Graduação em Nanociências e Materiais Avançados, 2015. / Iron oxide is one of the most promising semiconductors for applications as photoanodes in photoelectrochemical cells. A simple and cheap route to prepare hematite photoelectrodes is the sol-gel method. Hematite thin films can be also prepared by using the polymerized complex (PC) method that is a sol-gel method derived technique. This methodology involves the formation of complexes of metal ions that then undergo polymerization. In addition, the PC method allows an optimal control of stoichiometry and of the incorporation of impurities during the process. In this work, pure and doped hematite thin films were prepared by using the PC method at two different heat treatments (500°C and 800°C). The á-Fe2O3 thin films were modified with two differently charged dopants (Zn2+ and Sn4+), and their photoelectrochemical properties were studied in comparison with the pure hematite films. Hematite electrodes prepared at 800°C exhibited the best photocatalytic response in comparison with 500°C-treated hematite films. This effect was attributed to the higher roughness and surface area of films synthesized at higher temperatures. Furthermore, the modification of á-Fe2O3 with Zn2+ and Sn4+ ions resulted in a better photoresponse and stability as showed by the linear sweep voltammetry and chronoamperometry results. Dopants influenced differently on the photocurrent onset potential and the potential for the electrocatalytic oxygen evolution. In addition, results suggested that impurities were incorporated more efficiently into the hematite films prepared at 800°C. Nevertheless, the photocatalytic properties of the undoped and modified hematite films was poor, and two plausible hypothesis are proposed to explain the poor performance of hematite electrodes. First, most of dopants may have segregated, and, according to the previous reports in the literature, they may have acted as recombination sites that reduced the efficiency of the charge separation (photogenerated electron-hole pair). Second, poor contact between the hematite and F-SnO2 layer (from substrate) may have formed that severely hindered the harvesting of the photogenerated charges. The overall consequence of these two effects is the reduction in the activity of hematite films under illumination conditions. / O oxido de ferro e um dos semicondutores mais promissores para aplicacoes como fotoanodos em celulas fotoeletroquimicas. Uma rota simples e barata para preparar fotoeletrodos de hematita e o metodo sol-gel. Filmes finos de hematita podem tambem ser preparados utilizando o metodo do complexo polimerizado (CP) que e um metodo derivado da tecnica sol-gel. Esta metodologia envolve a formacao de complexos de ions metalicos que em seguida se polimerizam. Alem disso, o metodo do CP permite um controle optimo da estequiometria e da incorporacao de impurezas durante o processo. Neste trabalho, filmes finos de hematita pura e dopada foram preparados utilizando o metodo do CP em dois tratamentos termicos diferentes (500¿C e 800¿C). Os filmes finos de ¿¿-Fe2O3 foram modificados com dois dopantes de cargas diferentes (Zn2+ e Sn4+) e as suas propriedades fotoeletroquimicas foram estudadas em comparacao com os filmes de hematita pura. Os eletrodos de hematita preparados a 800¿C apresentaram a melhor resposta fotocatalitica em comparacao com os filmes de hematita preparados a 500¿C. Este efeito foi atribuido a maior rugosidade e area superficial dos filmes sintetizados a temperaturas mais elevadas. Alem disso, a modificacao de ¿¿-Fe2O3 com os ions Zn2+ e Sn4+ resultou em uma melhor fotoresposta e estabilidade como demonstrado pelos resultados da voltametria linear e cronoamperometria. Os dopantes influenciaram de forma diferente no potencial do comeco da fotocorrente e no potencial da evolucao de oxigenio eletrocatalitica. Alem disso, os resultados sugeriram que as impurezas foram incorporadas de forma mais eficiente nos filmes de hematita preparados a 800¿C. Porem, as propriedades fotocataliticas dos filmes de hematita nao dopada e modificada nao foram significativas, e duas hipoteses plausiveis sao propostas para explicar o baixo desempenho dos eletrodos de hematita. Em primeiro lugar, a maioria dos dopantes podem ter segregado, e, de acordo com o reportado na literatura, eles podem estar atuando como sitios de recombinacao que reduziram a eficiencia da separacao das cargas (par eletron-buraco fotogerado). Em segundo lugar, mau contato entre a camada de hematita e F-SnO2 (do substrato) pode ter sido formado que impediu severamente a colheita das cargas fotogeradas. A consequencia global destes dois efeitos e a reducao da atividade fotocatalitica dos filmes de hematita.
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Preparação, caracterização e estudo da eficiência na fotodegradação e adsorção de Rodamina B de heteroestruturas de TiO2/α-Fe2O3 / Preparation, characterization and study of the efficiency of Rhodamine B photodegradation and adsorption of the TiO2/α-Fe2O3 heterostructuresMaluf, Nágila El Chamy [UNESP] 18 April 2016 (has links)
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Previous issue date: 2016-04-18 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / A fotocatálise heterogênea, utilizando dióxido de titânio com estrutura do tipo anatase, tem se mostrado uma alternativa promissora para a remediação de sistemas aquáticos contaminados. Com o intuito de aumentar a eficiência do fotocatalisador, estudos científicos têm reportado a heterojunção deste óxido com estruturas do tipo hematita do óxido de ferro, α-Fe2O3. Neste estudo, foi investigada a síntese de nanoestruturas de TiO2 puro, α-Fe2O3 pura e heteroestruturas de TiO2/α-Fe2O3 em diferentes proporções dos óxidos a fim de testá-los como fotocatalisadores na degradação de um corante com elevada toxicidade, a Rodamina B. Os materiais foram sintetizados por rotas híbridas, utilizando o Metódo do Peróxido Oxidante com posterior tratamento hidrotérmico, totalizando a produção de 8 amostras. Foram empregadas três rotas de síntese: a rota (a) foi responsável pela síntese de TiO2 puro variando-se o pH do meio reacional na etapa de tratamento hidrotérmico, a rota (b) foi utilizada para a preparação de α-Fe2O3 pura e a rota (c) foi empregada na produção das heteroestruturas de TiO2/α-Fe2O3 nas concentrações de 0,1, 0,5, 1,0 e 5,0% p/p de hematita. As amostras foram caracterizadas quanto a sua estrutura, microestrutura e propriedades superficiais com o auxílio das técnicas de DRX, FT-Raman, método de BET, MEV/FEG, MET, TG e FT-IR. A análise dos resultados de caracterização estrutural mostrou que a rota (a) é eficiente para a síntese de TiO2 anatase quando realizada em meio básico, produzindo uma mistura de fases anatase/rutilo quando procedida em meio ácido. Sendo assim, na rota (c) foi utilizado o meio sintético básico para a síntese de TiO2 anatase e hematita. Em resumo, foi produzida pela rota (a) em meio básico a amostra HTTI1, que degradou a molécula de RhB em 95,0% e os materiais HTTI2 e HTTI3, produzidos em meio ácido, os quais degradaram a solução do corante em 70,9 e 24,4%, respectivamente, em 90 minutos de ensaio fotocatalítico, o que evidencia a importância em se obter nanomateriais com estrutura anatase do TiO2. Com o estudo da atividade fotocatalítica dos materiais produzidos, notou-se que alguns dos semicondutores apresentavam elevada taxa de adsorção no decorrer do processo. Devido a isso, a cinética de adsorção de RhB pelos materiais produzidos foi também estudada no período de 14 horas, cujos resultados mostraram que o óxido de ferro com estrutura hematita é um excelente adsorvente para o corante. Os resultados dos ensaios fotocatalíticos e de adsorção de RhB evidenciaram, principalmente, a elevada eficiência do TiO2 anatase como fotocatalisador e, em contrapartida, a elevada capacidade da hematita em adsorver as moléculas do corante. As heteroestruturas produzidas apresentaram o efeito de reduzir a eficiência na fotodegradação da RhB em relação a amostra HTTI1 com o aumento da concentração do óxido de ferro, porém as mesmas heterojunções se mostraram favoráveis para as propriedades adsortivas dos compostos quanto maior a concentração de α-Fe2O3. / The heterogeneous photocatalysis using titanium dioxide with anatase type structure, has proved to be a promising alternative for the remediation of contaminated aquatic systems. In order to increase the efficiency of this photocatalyst, scientific studies have reported the heterojunction of this oxide with hematite structures of iron oxide, α-Fe2O3. In this study, it was investigated the synthesis of pure TiO2 nanostructures, pure α-Fe2O3 and TiO2/α-Fe2O3 heterostructures in different proportions in order to test them as photocatalysts in the degradation of a dye having high toxicity, the Rhodamine B. The materials were synthesized by hybrid routes, using the Oxidant Peroxo Method with subsequent hydrothermal treatment, producing a total of 8 samples. Three synthesis routes were employed: the route (a) was responsible for the pure TiO2 synthesis by varying the pH of the reaction medium in the hydrothermal treatment step, route (b) was used for the preparation of pure α-Fe2O3 and route (c) was employed in the production of TiO2/α-Fe2O3 heterostructures in concentrations of 0.1, 0.5, 1.0 and 5.0% w/w of hematite. The samples were characterized as their structure, microstructure and surface properties with XRD, FT-Raman, BET method, SEM/FEG, TEM, TG and FT-IR techniques. The results of the structural characterization showed that route (a) is effective for the synthesis of anatase TiO2 when carried out in basic medium, producing a mixture of phases anatase/rutile when performed in an acid medium. Thus, in route (c) it was used the basic synthetic medium for the synthesis of anatase TiO2 and hematite. In summary, it was produced by route (a) in a basic medium the HTTI1 sample, that degraded RhB molecule in 95.0%, HTTI2 and HTTI3 materials, produced in acid medium, which degraded dye solution in 70.9 and 24.4%, respectively, in 90 minutes of the photocatalytic test, which highlights the importance of obtaining nanomaterials with anatase TiO2 structure. With the study of the photocatalytic activity of the materials, it was noted that some of the semiconductor had high adsorption rate during the process. Because of this, the RhB adsorption kinetics by the materials produced was also studied within 14 hours. The results showed that the iron oxide with hematite structure is an excellent adsorbent for the dye. Especially, the results of the photocatalytic tests and RhB adsorption showed high efficiency of anatase TiO2 as a photocatalyst and, conversely, high capacity of hematite to adsorb dye molecules. The heterostructures produced had the effect of reducing the efficiency in photodegradation of RhB comparing with HTTI1 sample with increasing concentration of iron oxide, however the same heterojunctions demonstrated favorable for adsorptive properties of the compounds the greater the concentration of α-Fe2O3.
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