Particle shape is evaluated on three scales corresponding to form, roundness and roughness. Shape at each of these scales uniquely influences material behavior. The shape of sand grains is largely formed as magma cools. Subsequent cleavage and abrasion change the roundness and roughness of particles. Published results indicate that particle shape influences several aspects of granular systems behavior including stiffness, strength, the evolution of strength anisotropy, dilation, and the development of strain localization. The crushing of granite creates a particulate material with a unique angular shape. A wide range of experimental studies implemented as part of this research permit assembling a unique database of material parameters and comparing the behavior of several crushed and natural sands. In general, the low roundness of crushed sands leads to higher maximum void ratios, lower small strain stiffnesses, and higher critical state friction angles than more rounded natural sands. It also impacts mortar strength and workability. Previous studies have emphasized size-controlled segregation. New experimental results show that differences in particle shape can also lead to segregation in a binary granular material. Round or spherical particles are more mobile than angular or flat particles. Then, the greater motion of round or spherical particles in a binary mixture subjected to horizontal or vertical vibration results in their segregation from their angular or flat neighbors. Particle shape may change significantly with stress in the case of soft particles. Therefore, the presence of shape-deformable particles decreases the stiffness of binary rigid-soft particle mixtures. However, macro-scale measurements with rigid-soft mixtures show higher stiffness than would be expected by volume averaging techniques. A subsequent microscale study shows the formation of backbone chains made of the rigid particles, partially supported by the soft particles which prevent the buckling of the load-carrying chains.

A numerical model based on the discrete element (DE) method, for modelling the flow of irregularly shaped, smooth-surfaced particles in a 3-D system is presented. An existing DE program for modelling the contact between spherical particles in periodic space (without real walls or boundaries) was modified to model non-spherical particles in a system with containing walls. The new model was validated against analytical calculations of single particle movements and also experimentally against data from physical experiments using synthetic non-spherical particles at both a particle and bulk scale. It was then used to study the effect of particle shape on the flow behaviour of assemblies of particles with various aspect ratios discharging from a flat-bottomed hopper. The particles were modelled using the Multi-Sphere Method (MSM) which is based on the CSG (Constructive Solid Geometry) technique for construction of complex solids by combining primitive shapes. In this method particle geometry is approximated using overlapping spheres of arbitrary diameter which are fixed in position relative to each other. The contact mechanics and contact detection method are the same as those used for spheres, except that translation and rotation of element spheres are calculated with respect to the motion of the whole particle. Numerical simulations of packing and flow of particles from a flat-bottomed hopper with a range of aspect ratios were performed to investigate the effect of particle shape on packing and flow behaviour of a particulate assembly. It was found that the particle shape influenced both bed structure and flow characteristics such as flow pattern, shear band strength and the occurrence of bridging. The flow of the bed of spherical particles was smoother than the flow of beds of elongated particles in which flow was fluctuating and there was more resistance to shear.

The entrainment rate of Ferrosilicone (FeSi) particles was measured in a 140 mm perspex column with air as the fluidising medium. Two different types of FeSi were used, namely atomised FeSi, which is mostly spherical in shape with smooth surfaces, and milled FeSi, which is irregular with rough surfaces. Both the FeSi mixtures had the same solid density and the similar average particle diameters ranging from 38 µm to 50 µm. The size and density of these particles put them on the border between Geldart A and Geldart B powders, similar to the high temperature Fischer-Tropsch catalyst. The atomised FeSi had a slightly higher concentration in fines (8.6% vs 1.8%), but except for the difference in particle shape, the two mixtures had otherwise very similar physical properties. A substantial difference in entrainment rate was measured between the atomised and milled FeSi, where the atomised had an entrainment rate of about six times higher than the milled FeSi throughout the range of superficial velocities tested. It was shown that the higher entrainment rate cannot be attributed only to the higher fines concentration, but that the difference in particle shape had a significant effect on the entrainment rate. Several two dimensional shape characterisation techniques were used in attempt to quantify the difference between the atomised and the milled FeSi. Of these the particle circularity managed to differentiate the best between the two particle mixtures. The circularities of the atomised and the milled FeSi were found to be 0.782 and 0.711 respectively. The measured circularity was used instead of a sphericity to adjust for the effect of particle shape on the terminal velocity of the particles. The adjusted terminal velocity was then used in the elutriation rate constant correlations to see which of the popular correlations in literature predicts the entrainment rate of the FeSi the best. All of the correlations gave a poor performance in predicting the measured entrainment rates. The two correlations that performed the best were that of Choi et al. (1999) (AARE = 72.6%) and Geldart et al. (1979) (AARE = 79%). It was concluded that single particle drag and single particle terminal velocities are not adequate to incorporate the effect of particle shape on entrainment rate. The method i by which shape affects entrainment rate therefore deserves further investigation. Further studies should also be done to develop a three dimensional shape descriptor that predicts bulk behaviour better. / Dissertation (MEng)--University of Pretoria, 2008. / Chemical Engineering / unrestricted

Approximately 80% of pharmaceutical products and the ingredients required for their manufacture are in powder form. The solid dosage form (tablets and capsules) is manufactured by either dry-blending of fine powder ingredients or combining the ingredients in a wet granulation step, followed by drying. Arching, ratholing, caking, segregation and flooding are some of the commonly encountered flow problems in the handling of fine powders. These problems lead to losses worth thousands of dollars at production scale. Poor powder flowability is a consequence of the combined effects of many variables, including improper equipment design, particle size, size distribution, shape, moisture content and surface texture. In the present work, a systematic study has been performed to determine the relationship between the flowability of fine powders and their physical properties of mean size and size distribution, density and shape.<p> Flowability studies were done on six different powders: the NutraSweet® Brand sweetener (aspartame), Respitose ML001, Alpha-D-Lactose monohydrate, the pharmaceutical binder Methocel (R) F50 Premium Hydroxypropyl methylcellulose- HPMC, a placebo pharmaceutical granulate, and common pastry flour. Scanning electron microscopy (SEM) and stereomicroscopy were used for particle shape and size analysis. Particle size distribution was determined using the laser light scattering technique. Powder flowability was measured using shear strength, angle of repose, and tapped-to-bulk density measurements. A novel method of measuring the dynamic angle of repose using electrical capacitance tomography (ECT) was developed. <p> Analysis of the images from microscopy revealed that the particles of aspartame and HPMC powders were elongated, the particles of ML001, pastry flour and lactose monohydrate powders were irregular, and the particles of placebo granulate were nearly spherical. Particle size was found to be the most reliable indicator of powder flowability, with decreasing particle size corresponding to lower flowability; however other parameters such as particle elongation and irregularity, were also found to have an influence on powder flowability. Although HPMC and pastry flour had similar particle sizes, they exhibited differences in flowability. This can be explained by the greater irregularity of the flour particles. Particle irregularity may cause mechanical interlocking between the particles, thus reducing powder flowability. ECT was found to be a promising non-intrusive tool for the measurement of the dynamic angle of repose. Unlike other methods for the measurement of dynamic angle of repose, the results obtained from ECT were not influenced by the effect of end caps. The present technique could be used by pharmaceutical industries in process analytical technology (PAT) for the detection and elimination of potential flow problems early in the manufacturing process.

Approximately 80% of pharmaceutical products and the ingredients required for their manufacture are in powder form. The solid dosage form (tablets and capsules) is manufactured by either dry-blending of fine powder ingredients or combining the ingredients in a wet granulation step, followed by drying. Arching, ratholing, caking, segregation and flooding are some of the commonly encountered flow problems in the handling of fine powders. These problems lead to losses worth thousands of dollars at production scale. Poor powder flowability is a consequence of the combined effects of many variables, including improper equipment design, particle size, size distribution, shape, moisture content and surface texture. In the present work, a systematic study has been performed to determine the relationship between the flowability of fine powders and their physical properties of mean size and size distribution, density and shape.<p> Flowability studies were done on six different powders: the NutraSweet® Brand sweetener (aspartame), Respitose ML001, Alpha-D-Lactose monohydrate, the pharmaceutical binder Methocel (R) F50 Premium Hydroxypropyl methylcellulose- HPMC, a placebo pharmaceutical granulate, and common pastry flour. Scanning electron microscopy (SEM) and stereomicroscopy were used for particle shape and size analysis. Particle size distribution was determined using the laser light scattering technique. Powder flowability was measured using shear strength, angle of repose, and tapped-to-bulk density measurements. A novel method of measuring the dynamic angle of repose using electrical capacitance tomography (ECT) was developed. <p> Analysis of the images from microscopy revealed that the particles of aspartame and HPMC powders were elongated, the particles of ML001, pastry flour and lactose monohydrate powders were irregular, and the particles of placebo granulate were nearly spherical. Particle size was found to be the most reliable indicator of powder flowability, with decreasing particle size corresponding to lower flowability; however other parameters such as particle elongation and irregularity, were also found to have an influence on powder flowability. Although HPMC and pastry flour had similar particle sizes, they exhibited differences in flowability. This can be explained by the greater irregularity of the flour particles. Particle irregularity may cause mechanical interlocking between the particles, thus reducing powder flowability. ECT was found to be a promising non-intrusive tool for the measurement of the dynamic angle of repose. Unlike other methods for the measurement of dynamic angle of repose, the results obtained from ECT were not influenced by the effect of end caps. The present technique could be used by pharmaceutical industries in process analytical technology (PAT) for the detection and elimination of potential flow problems early in the manufacturing process.

Particle size and shape are important characteristics of the sediment which affects the adsorption of sediment-associate contaminants and nutrients onto the surface of sediment. This thesis characterized the spatial and temporal variation in size and shape of sediment particles in the Tobacco Creek Watershed. A strong correlation between the particle size of suspended sediment and stream discharge was observed. Spatial and temporal variation in size of suspended and channel bed sediment showed that particle size was significantly coarser at the upper reaches and following the rainfall events, but finer at the lower reaches and following the snowmelt events. Image analysis of coarser particles showed that rock fragments are not becoming rounded in short distances, but they reduced in size. The coarser materials from bedrock outcrops can be sources of fine-sized particle during transport. These findings have important implications for understanding suspended sediment dynamics transport in the study watershed.

Granular soils with different sizes and shapes are often used in many civil engineering structures. In different contexts, several researchers have emphasized that shape of particles play a pivotal role in influencing several engineering properties such as maximum and minimum packing densities, shear strength, permeability and compressibility. However, the complexities involved in obtaining the geometrical parameters necessary to adequately compute particle shape have hampered the clear understanding of the contribution of particle shape to such properties. Researchers have attempted to characterize the shape of the particles by many conventional and advanced image based methods in the past. However, these methods suffer from many criticisms; conventional methods of shape characterization include ocular inspection of particles based on visual reference charts, which are more prone to user dependent interpretations. The recently developed image based methods deviate from the conventional and most well accepted definitions formulated by researchers in the past due to the difficulties involved in automating them. The aim of this thesis is to address this shortcoming by developing a robust methodology for accurate and precise determination of particle shape in accordance with the most widely accepted formulae in literature, which can replace the existing methods based on manual measurements, approximate visual charts and non-robust imaging techniques. For this purpose, several computational algorithms are written and implemented in MATLAB and operations are performed on particle images. These methods are developed to precisely characterize the particles shape parameters observed at three levels of scales, which are adequate for complete shape characterization. According to Barrett (1980) the particle shape features can be observed independently at three different scales, viz. macro-scale, meso-scale and micro-scale, the shape parameters such as form, roundness and surface texture falls into these three scales respectively. The macro-scale component of form (sphericity) is quantified as per the formula used in the visual chart proposed by Krumbein & Sloss (1951). In light of its continuing popularity and wide usage, the roundness concept proposed by Wadell (1932) is chosen to be the appropriate parameter for meso-scale shape representation. The micro-scale component of surface texture or roughness is measured by the conventional and widely used root mean square definition, by incorporating the use of digital filtering techniques. The distinct concept of angularity as proposed by Lees (1964) is used for effective shape representation of crushed particles. Kinematic behaviour of particles such as sliding, rolling and interlocking are dependent on the geometrical features observed at meso-scale present along their boundaries, which consequently govern the material strength and deformation characteristics. Based on precise identification of such features (concavo-convex regions along particle boundary), a new classification chart is proposed in this thesis to comprehend the kinematics of particles. The effects of critical parameters such as scale, resolution and user defined cutoff values on the quantification of shape parameters are analyzed and eliminated. The proposed methodology is compared with standard visual charts provided by earlier researchers and is demonstrated on real soil particles falling across a wide range of sizes and shapes. Finally, the role of particle shape in governing packing behaviour of aggregates is quantified based on the precise particle shape characterization.

The theoretical and experimental investigation of the novel in-line CMOS image sensor was performed. This sensor is aimed to investigate particle size distribution, particle concentration and shape in hydraulic liquid in order to implement the proactive maintenance of hydraulic equipment. The existing instruments such as automatic particle counters and techniques are not sufficiently enough to address this task because of their restricted sensitivity, limit of concentration to be measured and they cannot determine particle shape. Other instruments cannot be used as inline sensors because they are not resistant to the arduous conditions such as high pressure and vibration. The novel mathematical model was proposed as it is not possible to use previously developed techniques based on using optical system and complicated algorithms. This model gives the output signal of the image sensor depending on the particle size, its distance from the light source (LED) and image sensor. Additionally, the model takes into account the limited exposure time and particle track simulation. The results of simulation based on the model are also performed in thesis. On the basis of the mathematical model the image processing algorithms were suggested in order to determine particle size even when this size is lower than pixel size. There are different approaches depending on the relation between the size of the particle and the pixel size. The approach to the volume of liquid sample estimation was suggested in order to address the problem of low accuracy of concentration measurement by the conventional automatic particle counters based on the single photodiode. Proposed technique makes corrections on the basis of particle velocity estimation. Approach to the accuracy estimation of the sensor was proposed and simulation results are shown. Generally, the accuracy of particle size and concentration measurement was considered. Ultimately, the experimental setup was used in order to test suggested techniques. The mathematical model was tested and the results showed sufficient correlation with the experiment. The zinc dust was used as a reference object as there are the particles within the range from 1 to 25 microns which is appropriate to check the sensitivity. The results of experiments using reference instrument showed the improved sensitivity and accuracy of volume measured compared to the reference one.

Self-assembly of colloidal particles into ordered structures is hailed as the preferred route to production of functional devices on the nanometre and micron length scales. The shape of a colloidal particle is one of the most influential factors determining the type of ordered structure that is assembled. Thus this thesis is devoted to understanding the role of particle shape on phase behaviour of colloidal systems. The effect of particle shape is isolated by using computer simulations to model particles as hard, anisotropic bodies which interact via purely repulsive interactions. Two particle models are studied which are representative of real colloids: non-convex wireframe polyhedra, and convex spherical caps. This thesis investigates the densest packings of several wireframe polyhedra. By comparing packings of six distinct polyhedra some general conclusions are drawn regarding the effects of rounded polyhedra edges, and a new shape descriptor is given which can suggest whether a wireframe polyhedron is likely to form new interpenetrating crystal structures. Wireframe cubes were studied in more detail, where the full phase behaviour was mapped out. A curious phenomenon was found whereby crystals formed by cubic wireframes exhibit plastic fluctuations. This unusual behaviour, if reproduced experimentally, may lead to useful optical properties. A systematic study of spherical caps demonstrates the effect of shape on collective behaviour as the particle model interpolates between a sphere and a thin platelet. Purely repulsive interactions are responsible for a range of different crystal structures, but the nucleation of these structures is challenging due to slow dynamics. Furthermore, there are often many ways for a spherical cap to pack in a given volume, which leads to multiple metastable states. The self-assembly of spherical caps was directed by sedimentation on a solid template which resulted in increased nucleation rates and more stable crystals. However, there is still a lack of control over the exact crystal structure due to the degeneracy in ways to pack.

Characterization of micron and sub-micron size particles requires the simultaneous measurement of the joint particle property distribution (JPPD). The JPPD is comprised of particle size, shape, orientation, composition, optical properties, and surface properties. Measurement of each of the particle properties independently is a difficult task and it has been only partially successful. To determine as many particle properties as possible using optical methods it is necessary to simultaneously measure all aspects of the interaction of the incident light with the particles of interest. This approach leads to the concept of multidimensional spectroscopy suggested by Prof. Garcia-Rubio. Dr. Bacon proved the proposition by developing and testing a prototype multianglemultiwavelength (MAMW) spectrometer proposed by Prof. Garcia-Rubio. However, the prototype MAMW spectrometer has limitations in the amount of information it can obtain because of strong absorption of deep UV light and detector saturation due to the use of optical fibers and single integration time for the CCD detector. The Integrated UV-VIS MAMW spectrometer has been developed to overcome the limitations of the prototype MAMW spectrometer. Improvements have become possible through the use of UV lenses and integration time multiplexing (ITM). The Integrated UV-VIS MAMW spectrometer has the capabilities to perform low angle scattering measurements starting from 4o with simultaneous detection of multiwavelength light from 200 nm to 820 nm, UV-VIS transmission spectroscopy, and frequency domain fluorescence spectroscopy. Following the development, possible sources of errors were analyzed and data calibration procedures have been established to ensure the validity and reproducibility of the measurement results. The capabilities of the Integrated UV-VIS MAMW spectrometer were tested by measuring UV-VIS MAMW spectra of polystyrene standards. The measured UV-VIS MAMW spectra clearly show differences due to particle size, shape, and compositional changes. Measurements of the UV-VIS MAMW spectra of sickled whole blood samples demonstrate that particle shape and compositional changes can be detected simultaneously. These results confirmed that the Integrated UV-VIS MAMW spectrometer could be a powerful tool for the characterization of micron and sub-micron size particles. Alternate approaches to enhance these capabilities further, i.e., the development of a new multidimensional MAMW spectrometer, are also described.