Measurement, modelling, and closed-loop control of crystal shape distribution: Literature review and future perspectives

Crystal morphology is known to be of great importance to the end-use properties of crystal products, and to affect down-stream processing such as filtration and drying. However, it has been previously regarded as too challenging to achieve automatic closed-loop control. Previous work has focused on controlling the crystal size distribution, where the size of a crystal is often defined as the diameter of a sphere that has the same volume as the crystal. This paper reviews the new advances in morphological population balance models for modelling and simulating the crystal shape distribution (CShD), measuring and estimating crystal facet growth kinetics, and two- and three-dimensional imaging for on-line characterisation of the crystal morphology and CShD. A framework is presented that integrates the various components to achieve the ultimate objective of model-based closed-loop control of the CShD. The knowledge gaps and challenges that require further research are also identified

Stereo Imaging Camera Model for 3D Shape Reconstruction of Complex Crystals and Estimation of Facet Growth Kinetics

The principle that the 3D shape of crystals that grow from a solution can be characterised in real-time using stereo imaging has been demonstrated previously. It uses the 2D images of a crystal that are obtained from two or more cameras arranged in defined angles as well as a mathematical reconstruction algorithm. Here attention is given to the development of a new and more robust 3D shape reconstruction method for complicated crystal structures. The proposed stereo imaging camera model for 3D crystal shape reconstruction firstly rotates a digitised crystal in the three-dimensional space and varies the size dimensions in all face directions. At each size and orientation, 2D projections of the crystal, according to the angles between the 2D cameras, are recorded. The contour information of the 2D images is processed to calculate Fourier descriptors and radius-based signature that are stored in a database. When the stereo imaging instrument mounted on a crystalliser captures 2D images, the images are segmented to obtain the contour information and processed to obtain Fourier descriptors and radius-based information. The calculated Fourier descriptors and radius-based signature are used to find the best matching in the database. The corresponding 3D crystal shape is thus found. Potash alum crystals that each has 26 habit faces were used as a case study. The result shows that the new approach for 3D shape reconstruction is more accurate and significantly robust than previous methods. In addition, the growth rates of {111}, {110} and {100} faces were correlated with relative supersaturation to derive models of facet growth kinetics

Image analysis framework with focus evaluation for in situ characterisation of particle size and shape attributes

Particle processing industries, such as pharmaceutical, food processing and consumer goods sectors, increasingly require strategies to control and engineer particle attributes. In both traditional batch and continuous processes, particle size and shape need to be effectively monitored through in-line measurements from Process Analytical Technologies. However, obtaining quantitative information from these measurements has proven to be challenging and in-line imaging techniques are primarily used for qualitative purposes. Two key challenges are: (1) the presence of out-of-focus objects and (2) images only represent 2D projections of three-dimensional objects. In this work, a novel framework to process frames from in-line imaging probes incorporates a focus evaluation step in order to extract meaningful quantitative shape and size information through rejection of out-of-focus particles. Furthermore, a model is proposed that simulates the 2D projection of three-dimensional particles onto the focal plane and computes the corresponding size and shape distributions. The framework is quantified and evaluated against standard particles of well-defined size and shape such as polystyrene microspheres and needle-like cuboid silicon particles

Application of ultraviolet, visible, and infrared light imaging in protein-based biopharmaceutical formulation characterization and development studies

Imaging is increasingly more utilized as analytical technology in biopharmaceutical formulation research, with applications ranging from subvisible particle characterization to thermal stability screening and residual moisture analysis. This review offers a comprehensive overview of analytical imaging for scientists active in biopharmaceutical formulation research and development, where it presents the unique information provided by the ultraviolet (UV), visible (Vis), and infrared (IR) sections in the electromagnetic spectrum. The main body of this review consists of an outline of UV, Vis, and IR imaging techniques for several (bio)physical properties that are commonly determined during protein-based biopharmaceutical formulation characterization and development studies. The review concludes with a future perspective of applied imaging within the field of biopharmaceutical formulation research

Simulation and characterisation of electroplated micro-copper columns for electronic interconnection

Growth mechanism of electroplated copper columns has been systematically studied by simulations and characterizations. A two-dimensional cross-sectional kinetic Monte Carlo (2DCS-KMC) model has been developed to simulate the electrodeposition of single crystal copper. The evolution of the microstructure has been visualized. The cluster density, average cluster size, variance of the cluster size and average aspect ratio were obtained from the simulations. The growth history of the deposition from the first atom to an equivalent of 100 monolayers was reconstructed. Following the single-lattice 2DCS-KMC model for a single crystal, a two-dimensional cross-sectional poly-lattice kinetic Monte Carlo (2DCSP-KMC) model has been developed for simulation of the electrodeposition of polycrystalline copper on both a copper and a gold substrate. With this model, the early-stage nucleation and the grain growth after impingement of nuclei can be simulated; as such the entire growth history is reconstructed in terms of the evolution of microstructure, grain statistics and grain boundary misorientation. The model is capable of capturing some key aspects of nucleation and growth mechanisms including the nucleation type (e.g. homogeneous or heterogeneous), texture development, the growth of grains and higher energetic state of grain boundaries. The model has also proven capable of capturing the effects of deposition parameters including applied electrode potential, concentration of cupric ions and temperature. Their effects are largely dependent on the substrates. The early-stage electrocrystallization of Cu on polycrystalline Au has been studied by ex-situ AFM observations. The evolution of surface morphology of the electrodeposited copper on a sputtered Au seed layer from 16ms to 1000s was observed and their formation mechanism discussed. The heterogeneous nucleation phenomenon, the competitive growth both longitudinally and laterally, and the dominant growth of some nuclei were experimentally observed, which are also visualized by the relevant KMC simulation results at a smaller size scale and a shorter time scale. A heuristic model is therefore proposed to describe the mechanism of the early-stage electrocrystallization of Cu on a polycrystalline Au seed layer. Electroplated copper columns plated for different times have been characterized in terms of the evolution of their external morphology, cross-sectional microstructure and crystal structure. The microstructure of electroplated copper columns is characteristic of bi-modal or tri-modal grain size distribution. The results indicate that recrystallization has occurred during or after the plating, top-down and laterally. Slight changes of the crystal structure were observed by in-situ XRD and it was found that the changes of the (111) and (200) planes occurred at different stages of self-annealing. Finally, the results indicate the presence of organic additives is not essential for self-annealing of a copper column to occur

Simulation and characterisation of electroplated micro-copper columns for electronic interconnection

Growth mechanism of electroplated copper columns has been systematically studied by simulations and characterizations. A two-dimensional cross-sectional kinetic Monte Carlo (2DCS-KMC) model has been developed to simulate the electrodeposition of single crystal copper. The evolution of the microstructure has been visualized. The cluster density, average cluster size, variance of the cluster size and average aspect ratio were obtained from the simulations. The growth history of the deposition from the first atom to an equivalent of 100 monolayers was reconstructed. Following the single-lattice 2DCS-KMC model for a single crystal, a two-dimensional cross-sectional poly-lattice kinetic Monte Carlo (2DCSP-KMC) model has been developed for simulation of the electrodeposition of polycrystalline copper on both a copper and a gold substrate. With this model, the early-stage nucleation and the grain growth after impingement of nuclei can be simulated; as such the entire growth history is reconstructed in terms of the evolution of microstructure, grain statistics and grain boundary misorientation. The model is capable of capturing some key aspects of nucleation and growth mechanisms including the nucleation type (e.g. homogeneous or heterogeneous), texture development, the growth of grains and higher energetic state of grain boundaries. The model has also proven capable of capturing the effects of deposition parameters including applied electrode potential, concentration of cupric ions and temperature. Their effects are largely dependent on the substrates. The early-stage electrocrystallization of Cu on polycrystalline Au has been studied by ex-situ AFM observations. The evolution of surface morphology of the electrodeposited copper on a sputtered Au seed layer from 16ms to 1000s was observed and their formation mechanism discussed. The heterogeneous nucleation phenomenon, the competitive growth both longitudinally and laterally, and the dominant growth of some nuclei were experimentally observed, which are also visualized by the relevant KMC simulation results at a smaller size scale and a shorter time scale. A heuristic model is therefore proposed to describe the mechanism of the early-stage electrocrystallization of Cu on a polycrystalline Au seed layer. Electroplated copper columns plated for different times have been characterized in terms of the evolution of their external morphology, cross-sectional microstructure and crystal structure. The microstructure of electroplated copper columns is characteristic of bi-modal or tri-modal grain size distribution. The results indicate that recrystallization has occurred during or after the plating, top-down and laterally. Slight changes of the crystal structure were observed by in-situ XRD and it was found that the changes of the (111) and (200) planes occurred at different stages of self-annealing. Finally, the results indicate the presence of organic additives is not essential for self-annealing of a copper column to occur.EThOS - Electronic Theses Online ServiceGBUnited Kingdo

Head Tracked Multi User Autostereoscopic 3D Display Investigations

The research covered in this thesis encompasses a consideration of 3D television requirements and a survey of stereoscopic and autostereoscopic methods. This confirms that although there is a lot of activity in this area, very little of this work could be considered suitable for television. The principle of operation, design of the components of the optical system and evaluation of two EU-funded (MUTED & HELIUM3D projects) glasses-free (autostereoscopic) displays is described. Four iterations of the display were built in MUTED, with the results of the first used in designing the second, third and fourth versions. The first three versions of the display use two-49 element arrays, one for the left eye and one for the right. A pattern of spots is projected onto the back of the arrays and these are converted into a series of collimated beams that form exit pupils after passing through the LCD. An exit pupil is a region in the viewing field where either a left or a right image is seen across the complete area of the screen; the positions of these are controlled by a multi-user head tracker. A laser projector was used in the first two versions and, although this projector operated on holographic principles in order to obtain the spot pattern required to produce the exit pupils, it should be noted that images seen by the viewers are not produced holographically so the overall display cannot be described as holographic. In the third version, the laser projector is replaced with a conventional LCOS projector to address the stability and brightness issues discovered in the second version. In 2009, true 120Hz displays became available; this led to the development of a fourth version of the MUTED display that uses 120Hz projector and LCD to overcome the problems of projector instability, produces full-resolution images and simplifies the display hardware. HELIUM3D: A multi-user autostereoscopic display based on laser scanning is also described in this thesis. This display also operates by providing head-tracked exit pupils. It incorporates a red, green and blue (RGB) laser illumination source that illuminates a light engine. Light directions are controlled by a spatial light modulator and are directed to the users’ eyes via a front screen assembly incorporating a novel Gabor superlens. In this work is described that covered the development of demonstrators that showed the principle of temporal multiplexing and a version of the final display that had limited functionality; the reason for this was the delivery of components required for a display with full functionality

Research Reports: 1997 NASA/ASEE Summer Faculty Fellowship Program

For the 33rd consecutive year, a NASA/ASEE Summer Faculty Fellowship Program was conducted at the Marshall Space Flight Center (MSFC). The program was conducted by the University of Alabama in Huntsville and MSFC during the period June 2, 1997 through August 8, 1997. Operated under the auspices of the American Society for Engineering Education, the MSFC program was sponsored by the Higher Education Branch, Education Division, NASA Headquarters, Washington, D.C. The basic objectives of the program, which are in the 34th year of operation nationally, are: (1) to further the professional knowledge of qualified engineering and science faculty members; (2) to stimulate an exchange of ideas between participants and NASA; (3) to enrich and refresh the research and teaching activities of the participants' institutions; and (4) to contribute to the research objectives of the NASA centers. The Faculty Fellows spent 10 weeks at MSFC engaged in a research project compatible with their interests and background and worked in collaboration with a NASA/MSFC colleague. This document is a compilation of Fellows' reports on their research during the summer of 1997. The University of Alabama in Huntsville presents the Co-Directors' report on the administrative operations of the program. Further information can be obtained by contacting any of the editors

Spatial integration in computer-augmented realities

In contrast to virtual reality, which immerses the user in a wholly computergenerated perceptual environment, augmented reality systems superimpose virtual entities on the user's view of the real world. This concept promises to fulfil new applications in a wide range of fields, but there are some challenging issues to be resolved. One issue relates to achieving accurate registration of virtual and real worlds. Accurate spatial registration is not only required with respect to lateral positioning, but also in depth. A limiting problem with existing optical-see-through displays, typically used for augmenting reality, is that they are incapable of displaying a full range of depth cues. Most significantly, they are unable to occlude real background and hence cannot produce interposition depth cueing. Neither are they able to modify the real-world view in the ways required to produce convincing common illumination effects such as virtual shadows across real surfaces. Also, at present, there are no wholly satisfactory ways of determining suitable common illumination models with which to determine the real-virtual light interactions necessary for producing such depth cues. This thesis establishes that interpositioning is essential for appropriate estimation of depth in augmented realities, and that the presence of shadows provides an important refining cue. It also extends the concept of a transparency alpha-channel to allow optical-see-through systems to display appropriate depth cues. The generalised theory of the approach is described mathematically and algorithms developed to automate generation of display-surface images. Three practical physical display strategies are presented; using a transmissive mask, selective lighting using digital projection, and selective reflection using digital micromirror devices. With respect to obtaining a common illumination model, all current approaches require either . prior knowledge of the light sources illuminating the real scene, or involve inserting some kind of probe into the scene with which to determine real light source position, shape, and intensity. This thesis presents an alternative approach that infers a plausible illumination from a limited view of the scene.EThOS - Electronic Theses Online ServiceGBUnited Kingdo