Characterization of iron ore green pellets by scanning electron microscopy and X-ray microtomography

Sammanfattning: Cryogenic scanning electron microscopy (cryo-SEM), image analysis (IA) of SEM micrographs and X-ray microtomography (XMT) were used to obtain new information about the morphology of iron ore green pellets in this work. Cryo-SEM and freeze fracturing was used to observe entrapped air bubbles and arrangement of particles around the bubbles and in the matrix of wet green pellets. The observations of samples prepared by plunge and unidirectional freezing indicate that unidirectional freezing facilitates the observation of entrapped bubbles with minimum formation of artifacts, whereas plunge freezing enables observation of the degree of water filling at the outer surface of wet pellets with minimum amount of artifacts. It was also observed in the wet pellets that the size of the water domains in the matrix is quite small and the finer grains are mixed with coarser grains resulting in a denser matrix, whereas no fine grains were observed in the vicinity of the air bubbles. Two types of pellets prepared with and without addition of extra flotation reagent prior to balling were studied using IA and XMT. IA of scanning electron micrographs of epoxy impregnated pellets was used to separate bubble porosity from packing porosity and to quantify the former. The individual SEM micrographs acquired by a backscattered electron detector were reconstructed to provide the entire two-dimensional (2D) sections of the pellets. The 2D data obtained by IA were unfolded to three-dimensional (3D) by stereology and relatively good agreement with XMT data was observed. The size and amount of air bubbles could be quantified with both techniques. The addition of extra flotation reagent was found to increase the number of entrapped air bubbles and slightly decrease the median bubble diameter. The additional entrapped air bubbles due to the addition of extra flotation reagent was shown to be responsible for the difference in total porosity observed by mercury porosimetry between the two types of pellets. Mercury intrusion porosimetry (MIP) is shown in this work to produce inappropriate results with regard to the porosity due to bubble entrapment, it only provides values for total porosity and the throat size distribution of the porosity. In summary, this work has shown that cryo-SEM, IA of SEM micrographs and XMT are powerful and very useful methods for characterization of the morphology of iron ore green pellets.