X-ray MicroCT of electrospun polyacrylonitrile fiber mat with an average fiber diameters of 1 micron

In recent years, automated mineralogy has become an essential tool in geometallurgy. Automated mineralogical tools allow the acquisition of mineralogical and liberation data of ore particles in a sample. These particle data can then be used further for particle-based mineral processing simulation in the context of geometallurgy. However, most automated mineralogical tools currently in application are based on two-dimensional (2D) microscopy analysis, which are subject to stereological error when analyzing three-dimensional(3D) object such as ore particles. Recent advancements in X-ray microcomputed tomography (µCT) have indicated great potential of such system to be the next automated mineralogical tool. µCT's main advantage lies on its ability in monitoring 3D internal structure of the ore at resolutions down to few microns, eliminating stereological error obtained from 2D analysis. Aided with the continuous developments of computing capability of 3D data, it is only the question of time that µCT system becomes an interesting alternative in automated mineralogy system. This study aims to evaluate the potential of implementing µCT as an automated mineralogical tool in the context of geometallurgy. First, a brief introduction about the role of automated mineralogy in geometallurgy is presented. Then, the development of µCT system to become an automated mineralogical tool in the context of geometallurgy andprocess mineralogy is discussed (Paper 1). The discussion also reviews the available data analysis methods in extracting ore properties (size, mineralogy, texture) from the 3D µCT image (Paper 2). Based on the review, it was found that the main challenge inperforming µCT analysis of ore samples is the difficulties associated to the segmentation of the mineral phases in the dataset. This challenge is adressed through the implementation of machine learning techniques using Scanning Electron Microscope (SEM) data as a reference to differentiate the mineral phases in the µCT dataset (Paper 3).

Milling is a common unit operation in industry for the purpose of intentional size reduction. Considerable amount of energy is consumed during a grinding process and much of the energy is dissipated as heat and sound, which often makes grinding into an energy-intensive and highly inefficient operation. Despite many attempts to interpret particle breakage during a milling process, the grindability of a material in a milling operation remains aloof and the mechanisms of particle breakage are still poorly understood. Hence the optimisation and refinement in the design and operation of milling are in great need of an improved scientific understanding of the complex failure mechanisms. This thesis aims to provide an in-depth understanding of particle breakage associated with stressing events that occur during milling. A hybrid of experimental, theoretical and numerical methods has been adopted to elucidate the particle breakage mechanics. This study covers from single particle damage at micro-scale to bulk comminution during the whole milling process. The mechanical properties of two selected materials, i.e. alumina and zeolite were measured by indentation techniques. The breakage test of zeolite granules subjected to impact loading was carried out and it was found that tangential component velocity plays an increasingly important role in particle breakage with increasing impact velocity. Besides, single particle breakage via in-situ loading was conducted under X-ray microcomputed tomography (μCT) to study the microstructure of selected particles, visualize the progressive failure process and evaluate the progressive failure using the technique of digital image correlation (DIC). A new particle breakage model was proposed deploying a mechanical approach assuming that the subsurface lateral crack accounts for chipping mechanism. Considering the limitation of existing models in predicting breakage under oblique impact and the significance of tangential component velocity identified from experiment, the effect of impact angle is considered in the developed breakage model, which enables the contribution of the normal and tangential velocity component to be rationalized. The assessment of breakage models including chipping and fragmentation under oblique impact suggests that the equivalent normal velocity proposed in the new model is able to give close prediction with experimental results sourced from the public literature. Milling experiments were performed using the UPZ100 impact pin mill (courtesy by Hosokawa Micron Ltd. UK) to measure the comminution characteristics of the test solids. Several parameters were used to evaluate the milling performance including product size distribution, relative size span, grinding energy and size reduction ratio etc. The collective data from impact pin mill provides the basis for the validation of numerical simulation results. The Discrete Element Method (DEM) is first used to model single particle breakage subject to normal impact loading using a bonded contact model. A validation of the bonded contact model was conducted where the disparity with the experimental results is discussed. A parametric study of the most significant parameters e.g. bond Young’s modulus, the mean tensile bond strength, the coefficient of variation of the strength and particle & particle restitution coefficient in the DEM contact model was carried out to gain a further understanding of the effect of input parameters on the single particle breakage behavior. The upscaling from laboratory scale (single particle impact test) to industrial process scale (impact pin mill) is achieved using Population Balance Modelling (PBM). Two important functions in PBM, the selection function and breakage function are discussed based on the single particle impact from both experimental and numerical methods. An example of predicting product size reduction via PBM was given and compared to the milling results from impact pin mill. Finally, the DEM simulation of particle dynamics with emphasis on the impact energy distribution was presented and discussed, which sheds further insights into the coupling of PBM and DEM.

Im Rahmen der vorliegenden Dissertationsschrift „Semi-quantitative röntgentomographische Untersuchungen zur Biodistribution von magnetischen Nanopartikeln in biologischem Gewebe“ wurden tomographische Untersuchungen an biologischen Objekten durchgeführt. Bei diesen Objekten handelt es sich um Gewebeproben nach minimal-invasiven Krebstherapien wie zum Beispiel magnetischem Drug Targeting und magnetischer Wärmebehandlung. Der Erfolg dieser Therapien ist sowohl abhängig von der korrekten Verteilung der magnetischen Nanopartikel als auch von der Tatsache, dass diese in der Zielregion in einer ausreichenden Menge vorhanden sind. Das Vorliegen dieser beiden Voraussetzungen ist in der vorliegenden Arbeit untersucht worden. Dabei lag der Schwerpunkt der Arbeit auf der Quantifizierung von magnetischem Material in unterschiedlichen biologischen Gewebeproben mittels Röntgenmikrocomputertomographie (XµCT). Für diesen Zweck wurde ein Kalibrationssystem mit speziellen Phantomen entwickelt, mit dessen Hilfe eine Nanopartikelkonzentration einem Grauwert voxelweise zugewiesen werden kann. Mit Hilfe der Kalibration kann der Nanopartikelgehalt sowohl in monochromatischen als auch in polychromatischen tomographischen Daten im Vergleich zu magnetorelaxometrischen Ergebnissen mit wenigen Prozent Abweichung ermittelt werden. Trotz Polychromasie und damit einhergehenden Artefakten können 3-dimensionale röntgentomographische Datensätze mit einer geringfügigen Konzentrationsabweichung im Vergleich zur quantitativen Messmethode Magnetorelaxometrie semi-quantitativ ausgewertet werden. / The success of the minimal invasive cancer therapies, called magnetic drug targeting and magnetic heating treatment, depends strongly on the correct distribution of the magnetic nanoparticles on one side. On the other side it depends on the fact that a sufficient amount of magnetic nanoparticles carrying drugs is accumulated in the target region. To study whether these two requirements are fulfilled motivates this PhD thesis „Semi-quantitative X-ray-tomography examinations of biodistribution of magnetic nanoparticles in biological tissues“. The analysis of the distribution of the magnetic nanoparticles in tumours and other tissue examples is realized by means of X-ray-micro computer tomography (XμCT). The work focuses on the quantification of the magnetic nanoparticles in different biological tissue samples by means of XµCT. A calibration of the tomographic devices with adequate phantoms, developed in the frame of this work, opens now the possibility to analyze tomographic data in a semi-quantitative manner. Thus, the nanoparticle concentration can be allocated voxel-wise to the grey values of the three-dimensional tomographic data. With the help of calibration of the tomography equipments used, polychromatic as well as monochromatic three-dimensional representations of objects can be analyzed with regard to the biodistribution of magnetic nanoparticles as well as with regard to their quantity. The semi-quantitative results have been compared with results obtained with a quantitative measurement method magnetorelaxometry (MRX). Thereby a good agreement of the semi-quantitative and quantitative data has been figured out.

Im Rahmen der vorliegenden Dissertationsschrift „Semi-quantitative röntgentomographische Untersuchungen zur Biodistribution von magnetischen Nanopartikeln in biologischem Gewebe“ wurden tomographische Untersuchungen an biologischen Objekten durchgeführt. Bei diesen Objekten handelt es sich um Gewebeproben nach minimal-invasiven Krebstherapien wie zum Beispiel magnetischem Drug Targeting und magnetischer Wärmebehandlung. Der Erfolg dieser Therapien ist sowohl abhängig von der korrekten Verteilung der magnetischen Nanopartikel als auch von der Tatsache, dass diese in der Zielregion in einer ausreichenden Menge vorhanden sind. Das Vorliegen dieser beiden Voraussetzungen ist in der vorliegenden Arbeit untersucht worden. Dabei lag der Schwerpunkt der Arbeit auf der Quantifizierung von magnetischem Material in unterschiedlichen biologischen Gewebeproben mittels Röntgenmikrocomputertomographie (XµCT). Für diesen Zweck wurde ein Kalibrationssystem mit speziellen Phantomen entwickelt, mit dessen Hilfe eine Nanopartikelkonzentration einem Grauwert voxelweise zugewiesen werden kann. Mit Hilfe der Kalibration kann der Nanopartikelgehalt sowohl in monochromatischen als auch in polychromatischen tomographischen Daten im Vergleich zu magnetorelaxometrischen Ergebnissen mit wenigen Prozent Abweichung ermittelt werden. Trotz Polychromasie und damit einhergehenden Artefakten können 3-dimensionale röntgentomographische Datensätze mit einer geringfügigen Konzentrationsabweichung im Vergleich zur quantitativen Messmethode Magnetorelaxometrie semi-quantitativ ausgewertet werden. / The success of the minimal invasive cancer therapies, called magnetic drug targeting and magnetic heating treatment, depends strongly on the correct distribution of the magnetic nanoparticles on one side. On the other side it depends on the fact that a sufficient amount of magnetic nanoparticles carrying drugs is accumulated in the target region. To study whether these two requirements are fulfilled motivates this PhD thesis „Semi-quantitative X-ray-tomography examinations of biodistribution of magnetic nanoparticles in biological tissues“. The analysis of the distribution of the magnetic nanoparticles in tumours and other tissue examples is realized by means of X-ray-micro computer tomography (XμCT). The work focuses on the quantification of the magnetic nanoparticles in different biological tissue samples by means of XµCT. A calibration of the tomographic devices with adequate phantoms, developed in the frame of this work, opens now the possibility to analyze tomographic data in a semi-quantitative manner. Thus, the nanoparticle concentration can be allocated voxel-wise to the grey values of the three-dimensional tomographic data. With the help of calibration of the tomography equipments used, polychromatic as well as monochromatic three-dimensional representations of objects can be analyzed with regard to the biodistribution of magnetic nanoparticles as well as with regard to their quantity. The semi-quantitative results have been compared with results obtained with a quantitative measurement method magnetorelaxometry (MRX). Thereby a good agreement of the semi-quantitative and quantitative data has been figured out.