Síntese in situ da liga de FeCo altamente estável encapsulada em carbono a partir do etanol
This research proposed to develop a FeCo magnetic alloy encapsulated in carbon, using ethanol as a carbon precursor, through the CVD route, for the photocatalytic degradation of organic contaminants. Initially, a CoxFeyO4 oxide in a 1:1 ratio was synthesized using the Pechini method. The material was subjected to in situ reduction, by the CVD method, using ethanol as the initial reagent at temperatures of 400, 500, 600 and 700ºC. The reactions were studied by Gas Chromatography (GC), from gas aliquots collected at predetermined times. From the ethanol dehydrogenation and dehydration reactions, it is transformed into an encapsulated binder and, for comparative purposes, it is reduced to oxide in the pure FeCo binder using only H2. You are materialized by a characterized and interpreted result. From the analysis of XRD and Rietveld Refinement, it is possible to identify the phases present without CoxFeyO4 oxide, as well as the presence of crystalline carbon and FeCo phases in reduced materials via CVD, whose peak intensity increases with the synthesis temperature. Thus, we show FeCo-400 and FeCo-700 were treated in acidic and alkaline medium and we verified the importance of encapsulation for the stability of the FeCo bond. TGA profiles indicate an increase in the thermal stability of the bond as the local temperature is raised. Magnetic measurements performed for the FeCo, FeCo-400 and FeCo-700 samples reveal a reduction in the more values due to the presence of the carbon phase, as well as showing high Hc values compared to the FeCo Bond, especially for an It presents FeCo-400, which may be associated with the existence of a fraction of the oxide phase that was not reduced. Mössbauer spectroscopy confirms the presence of the BCC structure of the FeCo magnetic bond in FeCo, FeCo-400 and FeCo-700 materials and indicates values of isomeric displacement and Bhf coefficient with literature for the FeCo phase. The H2-TPR profile shows a complete reduction of the oxide in the bond at approximately 470°C, or which justifies the presence of the mixture of oxide and bonding phases in presenting FeCo-400. The profiles of NH3-TPD and CO2-TPD revealed the presence of Lewis acid sites and basic sites (O2- ). The Raman spectra will show that a higher and lower degree of graphitization is respectively FeCo-700 and FeCo-500, which uses TEM analysis to confirm the presence of more organized CNTs for FeCo-700. The SEM-FEG analysis shows the uniformity of the oxide surface and the prediction of the presence of CNTs, which was confirmed by the TEM images. Adsorption tests prove or encapsulate two materials as the synthesis temperature increases and indicate a less encapsulated FeCo-400 that synergizes with Fe-Co oxide as an adsorbent. Proposal is a mechanism to explain the formation of carbon-based encapsulated binding material in ethanol dehydration and dehydration reactions. The band-gap energy of two materials indicates that they are promising for photocatalytic applications, where the photodegradation of methylene blue (MB) is studied, which obtains the best removal for the FeCo-400 sample through a photo-processing process. Fenton with in situ H2O2 generation, which also has its mechanism of synergism between the encapsulated bond and the oxide phase, together with the small diameter of the crystallite of the FeCo bond, favors MB photodegradation.
Liga FeCo, Encapsulamento em carbono, Nanotubos de carbono, Aplicações fotocatalíticas, Separação magnética
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Universidade Federal do Rio Grande do Norte