Estudo de moagem de alta energia e de tratamento térmico de cerâmicas dos sistemas à base de Al2O3-Nb2O5-Ta2O5

Abstract

Given the economic and environmental measures that relate global warming and the continuous use of contaminating energy matrices, it is necessary to develop technologies that contribute to a reduction of pollutant emissions and sustainable energy generation. In this context, the CLC process (Chemical-Looping Combustion) is suggested as one alternative to CO2 capture that allows the generation of sustainable energy. The key issues on the viability of this technique are in the efficiency and cost of oxygen charger, which is a solid generally composed by metal oxide, and depending on the composition and microstructure, the use of bimetal oxides in a porous structure can be potentially attractive for CLC and CLR processes. The present work aimed to understand the effect of chemical composition, high-energy ball milling and heat-treatment temperature on the microstructure and physical properties of the α-Al2O3, Nb2O5 e Ta2O5 powder mixtures. Two kind of ball mills were utilized adopting: a planetary Fritsch P-7 mill (vial and balls of ZrO2) and a SPEX 8000M mill (vial of WC-Co, using hardened steel and alumina balls). Following, green bodies with 10 mm diameter were prepared by axial pressing from the milled powders, which were heated in air at 600, 800 and 1000°C. Aiming to obtain desired characteristics for oxygen carriers, were added high-density polyethylene (HDPE) or graphite in different amounts on the bodies green. The produced materials were characterized by means of X-ray diffraction (XRD), thermal analyses (DSC/TG), optical microscopy (OM), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), volumetric (BET), He pycnometry and wavelength dispersive X-ray fluorescence (XRF). The results showed that the increase in the milling time provided reduction on intensity in the XRD peaks of the α-Al2O3, Nb2O5 and Ta2O5 phases, there is no formation of AlNbO4 or AlNb(Ta)O4 during milling of Al2O3+Nb2O5 e Al2O3+Nb2O5+Ta2O5 powders, respectively. However, these phases were formed in powders heated at 800 and 1000°C. Analysis showed that the HDPE addition has resulted in the formation of surface and internal pores into the cylinders, which no notice in samples containing graphite addition was achieved. The 95Al2O3-5Nb2O5 cylinders presented higher surface area due to higher alpha alumina amount in starting powders. For ceramic powders processed with steel balls, the acid lixiviation step has contributed for an iron removal of 98.4% from the sample with highest Al2O3 content.