Síntese e caracterização de TaC e óxido misto de tântalo e cobre nanoestruturados a partir do precursor oxálico de tântalo através de reações gás-sólido e sólido-sólido a baixa temperatura

The research and development of nanostructured materials have been growing significantly in the last years. These materials have properties that were significantly modified as compared to conventional materials due to the extremely small dimensions of the crystallites. The tantalum carbide (TaC) is an extremely hard material that has high hardness, high melting point, high chemical stability, good resistance to chemical attack and thermal shock and excellent resistance to oxidation and corrosion. The Compounds of Tantalum impregnated with copper also have excellent dielectric and magnetic properties. Therefore, this study aimed to obtain TaC and mixed tantalum oxide and nanostructured copper from the precursor of tris (oxalate) hydrate ammonium oxitantalato, through gas-solid reaction and solid-solid respectively at low temperature (1000 ° C) and short reaction time. The materials obtained were characterized by X-ray diffraction (XRD), Rietveld refinement, Scanning Electron Microscopy (SEM), Spectroscopy X-Ray Fluorescence (XRF), infrared spectroscopy (IR), thermogravimetric (TG), thermal analysis (DTA) and BET. Through the XRD analyses and the Reitiveld refinement of the TaC with S = 1.1584, we observed the formation of pure tantalum carbide and cubic structure with average crystallite size on the order of 12.5 nanometers. From the synthesis made of mixed oxide of tantalum and copper were formed two distinct phases: CuTa10O26 and Ta2O5, although the latter has been formed in lesser amounts

Síntese e caracterização de CuNb2O6 e CuNbC através de reação sólido- sólido e gás- sólido a baixa temperatura

The refractory metal carbides have proven important in the development of engineering materials due to their properties such as high hardness, high melting point, high thermal conductivity and high chemical stability. The niobium carbide presents these characteristics. The compounds of niobium impregnated with copper also have excellent dielectric and magnetic properties, and furthermore, the Cu doping increases the catalytic activity in the oxidation processes of hydrogen. This study aimed to the synthesis of nanostructured materials CuNbC and niobium and copper oxide from precursor tris(oxalate) oxiniobate ammonium hydrate through gas-solid and solid-solid reaction, respectively. Both reactions were carried out at low temperature (1000°C) and short reaction time (2 hours). The niobium carbide was produced with 5 % and 11% of copper, and the niobium oxide with 5% of copper. The materials were characterized by X-Ray Diffraction (XRD), Rietveld refinement, Scanning Electron Microscopy (SEM), X-Ray Fluorescence Spectroscopy (XRF), infrared spectroscopy (IR), thermogravimetric (TG) and differential thermal analysis (DTA , BET and particle size Laser. From the XRD analysis and Rietveld refinement of CuNbC with S = 1.23, we observed the formation of niobium carbide and metallic copper with cubic structure. For the synthesis of mixed oxide made of niobium and copper, the formation of two distinct phases was observed: CuNb2O6 and Nb2O5, although the latter was present in small amounts

Síntese e caracterização do carbeto de molibdênio nanoestruturado para fins catalíticos na reação de oxidação parcial do metano

The nanostructures materials are characterized to have particle size smaller than 100 nm and could reach 1 nm. Due to the extremely reduced dimensions of the grains, the properties of these materials are significantly modified relatively when compared with the conventional materials. In the present work was accomplished a study and characterization of the molybdenum carbide, seeking obtain it with particles size in the nanometers order and evaluate its potential as catalyst in the reaction of partial methane oxidation. The method used for obtaining the molybdenum carbide was starting from the precursor ammonium heptamolybdate of that was developed in split into two oven, in reactor of fixed bed, with at a heating rate of 5ºC/min, in a flow of methane and hydrogen whose flow was of 15L/h with 5% of methane for all of the samples. The studied temperatures were 350, 500, 600, 650, 660, 675 and 700ºC and were conducted for 0, 60, 120 and 180 minutes, and the percent amount and the crystallite size of the intermediate phases were determined by the Rietveld refinement method. The carbide obtained at 660ºC for 3 hours of reaction showed the best results, 24 nm. Certain the best synthesis condition, a passivating study was accomplished, in these conditions, to verify the stability of the carbide when exposed to the air. The molybdenum carbide was characterized by SEM, TEM, elemental analysis, ICP-AES, TG in atmosphere of hydrogen and TPR. Through the elemental analysis and ICP-AES the presence carbon load was verified. TG in atmosphere of hydrogen proved that is necessary the passivating of the molybdenum carbide, because occur oxidation in room temperature. The catalytic test was accomplished in the plant of Fischer-Tropsch of CTGAS, that is composed of a reactor of fixed bed. Already the catalytic test showed that the carbide presents activity for partial oxidation, but the operational conditions should be adjusted to improve the conversion

Nitrificação de efluentes de reatores anaeróbicos em filtros submersos aerados

Although the good performance in organic matter and suspended solids removal, the anaerobic reactors are unable to remove ammonia nitrogen from sewage, which makes indispensable to include a step of post-treatment for removal of ammonia or nitrate as necessary. This paper presents the performance of a new variant technology, where the nitrification unit, preceded by anaerobic units, is a submerged aerated biological filter, without continuous sludge discharge in their daily operation. The oxygenation system is very simple and inexpensive, consisting of perforated hoses and compressors. The anaerobic reactors are a septic tank with two chambers followed (8.82 m³) and two parallel anaerobic filters (36 m³ each) filled with ceramic bricks and conics plastic parts. Both followed aerated filters were filled with cut corrugated conduit. The study evaluated the behavior of the system with constant domestic sewage flow (10 m³/d) and different aeration conditions, are these: stage 01, when applied air flow of 0.01 m³ air/min in both aerated filter; stage 02, remained in the initial air flow rate in the second aerated filter and increased at the first to 0.05 m³ air/min; at last, at last, in stage 03, the air flow rate of first aerated filter was 0.10 m³ air/min and on the second remained at 0.01 m³ air/min. The filter FA1 received load of 0.41 kg COD/m³.d, 0.37 kg COD/m³.d and 0.26 kg COD/m³.d on phases 01, 02 and 03, respectively. The FA2 received loads of 0.25 kg COD/m³.d, 0.18 kg COD/m³.d and 0.14 kg COD/m³.d on phases 01, 02 and 03, respectively. During stage 01, were found the following results: 98% removals of BODtotal and 92% of CODtotal, with effluent presenting 9 mg/L of BODtotal final average and 53 mg/L of CODtotal average; suspended solids removals of 93%, with a mean concentration of 10 mg/L in the final effluent; 47% reduction of ammonia of FA2 to FAN 's, presenting average of 28 mg NNH3/ L of ammonia in the effluent with; the dissolved oxygen levels always remained around 2.0 mg/L. During stage 02, were found removals of 97% and 95% to BODtotal and suspended solids, respectively, with average final concentrations of 8 and 7 mg/L, respectively; was removed 60% of ammonia, whose final concentration was 16.3 mg NNH3/ L, and nitrate was increased to a final average concentration of 16.55 mg N-NO3/L. Finally, the stage 03 provided 6 mg/L of DBOtotal (98% removal) and 23 mg/L of CODtotal (95% removal) of final effluent concentrations average. At this stage was identified the higher ammonia oxidation (86%), with final effluent showing average concentration of 6.1 mg N-NH3/L, reaching a minimum of 1.70 mg N-NH3/L. In some moments, during stage 03, there was a moderate denitrification process in the last aerated filter. The average turbidity in the effluent showed around 1.5 NTU, proving the good biomass physical stability. Therefore, the results demonstrate the submerged biological filters potential, filled with high void ratio material (98%), and aerated with hoses and compressor adoption, in the carbonaceous and nitrogenous matter oxidation, also generating an effluent with low concentration of solids