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- Bhuiyan, Iftekhar Uddin
(författare)
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Characterization of iron ore green pellets by scanning electron microscopy and X-ray microtomography
- 2011
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Licentiatavhandling (övrigt vetenskapligt/konstnärligt)abstract
- 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.
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- Bhuiyan, Iftekhar Uddin, et al.
(författare)
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Consideration of X-ray microtomography to quantitatively determine the size distribution of bubble cavities in iron ore pellets
- 2013
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Ingår i: Powder Technology. - : Elsevier BV. - 0032-5910 .- 1873-328X. ; 233, s. 312-318
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Tidskriftsartikel (refereegranskat)abstract
- X-ray microtomography data of iron ore green pellets of approx. 12 mm in diameter were recorded using a commercial instrument. The reconstructed volume after thresholding represented a unique dataset consisting of a three-dimensional distribution of equiaxed objects corresponding to bubble cavities. This dataset was used to successfully validate a stereological method to determine the size distribution of spherical objects dispersed in a volume. This was achieved by investigating only a few cross-sectional images of this volume and measuring the profiles left by these objects in the cross-sectional images. Excellent agreement was observed between the size distribution of the bubble cavities obtained by directly classifying their size in the reconstructed volume and that estimated by applying the aforementioned stereological method to eight cross-sectional images of the reconstructed volume. Subsequently, we discuss the possibility of calibrating X-ray tomography data quantitatively using the size distribution of the bubble cavities as a figure of merit and the results obtained by applying the stereological method to SEM images as reference data. This was justified by considering the validity of the stereological method demonstrated by tomography, the accurate thresholding made possible by back-scattered electron imaging and the solid reproducibility of the results obtained by SEM. Using different threshold values for binarization of the X-ray microtomography data and comparing the results to those obtained by SEM, we found that X-ray microtomography can be used after proper calibration against SEM data to measure the total porosity of the bubble cavities but can only provide a rough estimate of the median diameter because of the limited resolution achieved in this study.
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- Bhuiyan, Iftekhar Uddin
(författare)
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Microstructural characterization of iron ore green pellets
- 2013
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Doktorsavhandling (övrigt vetenskapligt/konstnärligt)abstract
- The aim of this thesis work was to develop new methodologies to characterize iron ore green pellets, in wet and dry state. The new characterization methods applied and developed in this work were mainly based on scanning electron microscopy (SEM) to gather both qualitative and quantitative data on different components of the pellets, i.e. mineral particles, water, bentonite and entrapped bubbles.In a first attempt to preserve the structure of wet iron ore green pellets by freezing before investigation by cryogenic SEM, wet pellets were frozen in liquid nitrogen by direct plunging or a new method developed in the present work denoted unidirectional freezing. The former method was found useful to study the degree of water filling at the outer surface of the pellet but led to artifacts in the interior of the pellet. The latter method was developed to confirm that the spherical cavities observed in dry pellets were related to entrapped bubbles in wet pellets. Capillaries were observed at the outer surface of the pellets and fine particles were lacking within a layer of approximately 100 µm from the outer surface and also in the direct vicinity of the air bubbles in the interior of the pellets.More advanced freezing methods were subsequently employed to reveal the artifact free microstructure of bentonite in wet pellets. In order to verify the observations made on a slice of a wet pellet frozen by plunging in liquid ethane, SEM investigations were also carried out on a bentonite suspension and a bentonite-iron ore slurry, which could be cryo-fixed by the most reliable freezing method, i.e. high pressure freezing. All microstructures were comparable and consisted in a voluminous network of well-dispersed clay platelets. This network was found to collapse upon drying. Bentonite was drawn to the contact points between the particles and formed what appeared as bridges, which may impart strength to the dry pellets. A combination of energy dispersive spectroscopy (EDS) and imaging by low-loss backscattered electrons at low voltage evidenced the presence of very finely divided silicate species on the magnetite particles. In order to visualize the three dimensional structure of dispersed bentonite clay with unprecedented resolution, a method based on SEM imaging with a monochromatic and decelerated beam was used for the first time. The recorded images showed very well-dispersed clay platelets forming a fine network of Y shaped contacts, which is quite different from earlier reports of much coarser structures formed as a result of poor sample preparation. Finally, in order to gain quantitative data about the porosity due to bubble entrapment in dry pellets, the entire cross-section of dry epoxy embedded and polished pellets were recorded by SEM. The three-dimensional bubble size distribution was unfolded from 2D SEM data using image processing, image analysis and stereological principles. The same type of pellets was also investigated by X-ray micro-tomography (XMT). The resulting three-dimensional dataset allowed the validation of the unfolding procedure based on stereology. However, the lack of resolution obtained by XMT was shown to lead to slight discrepancies with the SEM data for small bubble sizes. Entrapped air bubbles due to the addition of extra flotation reagent in pellets were shown to be responsible for additional porosity observed by mercury intrusion porosimetry (MIP). In summary, useful characterization methods for iron ore pellets based on SEM have been developed in this work, which opens up new possibilities to for instance study agglomeration processes in more detail.
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- Bhuiyan, Iftekhar Uddin, et al.
(författare)
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Microstructure of Bentonite in Iron Ore Green Pellets
- 2014
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Ingår i: Microscopy and Microanalysis. - 1431-9276 .- 1435-8115. ; 20:1, s. 33-41
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Tidskriftsartikel (refereegranskat)abstract
- Sodium-activated calcium bentonite is used as a binder in iron ore pellets and is known to increase strength of both wet and dry iron ore green pellets. In this article, the microstructure of bentonite in magnetite pellets is revealed for the first time using scanning electron microscopy. The microstructure of bentonite in wet and dry iron ore pellets, as well as in distilled water, was imaged by various imaging techniques (e.g., imaging at low voltage with monochromatic and decelerated beam or low loss backscattered electrons) and cryogenic methods (i.e., high pressure freezing and plunge freezing in liquid ethane). In wet iron ore green pellets, clay tactoids (stacks of parallel primary clay platelets) were very well dispersed and formed a voluminous network occupying the space available between mineral particles. When the pellet was dried, bentonite was drawn to the contact points between the particles and formed solid bridges, which impart strength to the solid compact.
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| 8. |
- Bhuiyan, Iftekhar Uddin, et al.
(författare)
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Quantitative image analysis of bubble cavities in iron ore green pellets
- 2011
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Ingår i: Powder Technology. - : Elsevier BV. - 0032-5910 .- 1873-328X. ; 214:3, s. 306-312
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Tidskriftsartikel (refereegranskat)abstract
- Scanning electron microscopy and image analysis was used for quantitative analysis of bubble cavities in iron ore green pellets. Two types of pellets prepared with and without addition of flotation reagent prior to balling were studied. The bubble cavity porosity amounted to 2.8% in the pellets prepared without addition of flotation reagent prior to balling. When flotation reagent was added prior to balling, the bubble cavity porosity increased by a factor of 2.4 and the median bubble diameter was decreased slightly. It was also shown that mercury intrusion porosimetry is not suitable for determination of the distribution of bubble cavities. Finally, our data suggested that the difference in total porosity determined by mercury intrusion porosimetry and pycnometry between the two types of pellets was due to the bubble cavities.
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| 9. |
- Mouzon, Johanne, et al.
(författare)
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Cryo-SEM method for the observation of entrapped bubbles and degree of water filling in large wet powder compacts
- 2011
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Ingår i: Journal of Microscopy. - : Wiley. - 0022-2720 .- 1365-2818. ; 242:2, s. 189-196
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Tidskriftsartikel (refereegranskat)abstract
- There are generally two problems associated with cryogenic scanning electron microscopy (cryo-SEM) observations of large wet powder compacts. First, because water cannot be vitrified in such samples, formation of artefacts is unavoidable. Second, large frozen samples are difficult to fracture but also to machine into regular pieces which fit in standard holders, especially if made of hard materials like ceramics. In this article, we first describe a simple method for planning hard cryo-samples and a low-cost technique for cryo-fracture and transfer of large specimens. Subsequently, after applying the entire procedure to green pellets of iron ore produced by balling, we compare the influence of plunge- and unidirectional freezing on large entrapped bubbles throughout the samples as well as the degree of water filling at the outer surface of the pellets. By carefully investigating the presence of artefacts in large areas of the samples and by controlling the orientation of the sample during freezing and preparation, we demonstrate that unidirectional freezing enables the observation of large entrapped bubbles with minimum formation of artefacts, whereas plunge freezing is preferable for the characterization of the degree of water filling at the outer surface of wet powder compacts. The minimum formation of artefacts was due to the high packing density of the iron ore particles in the matrix
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- Mouzon, Johanne, et al.
(författare)
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The structure of montmorillonite gels revealed by sequential cryo-XHR-SEM imaging
- 2016
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Ingår i: Journal of Colloid and Interface Science. - : Elsevier BV. - 0021-9797 .- 1095-7103. ; 465, s. 58-66
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Tidskriftsartikel (refereegranskat)abstract
- Imaging by extreme high resolution-scanning electron microscopy (XHR-SEM) with a monochromated and decelerated beam was applied on 5% (wt/wt) Na and Ca-montmorillonite gels frozen by high pressure freezing (HPF). In order to visualize the three-dimensional structure and the contacts between clay platelets, a new approach was developed. It consists in recording a sequence of micrographs on a region of interest during controlled sublimation. This simple method allows to rewind and to relate the instantaneous configuration between several particles to their original position in the hydrated state. Consequently, aggregates of parallel platelets (i.e. curved tactoids) were present in the Ca-sample and the instantaneous position of these aggregates in the course of sedimentation was revealed. The Na-sample consisted of a continuous network of flexible platelets sharing mostly face-to-face (FF) contacts caused by jamming at the relatively high concentration of the suspension (5% (wt/wt)), which was above the gel transition. Yet individual platelets belonging to the smallest size fraction were observed to be fully dispersed within the entangled structure, which confirmed the repulsive character of the gel. Substructures consisting of several platelets connected by FF-associations were also evidenced. The origin and potential impact of such substructures on the occurrence of the sol–gel transition and birefringence are discussed.
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