Dissertations / Theses on the topic 'Rheometal™ process'

Semi-Solid Metal (SSM) casting is a promising technology offering an opportunity to manufacture net-shape, complex geometry metal components in a single operation. However, the absence of foundry guidelines and limited design data for SSM casting makes it challenging to predict the performance of both process and components. The objective of this research was to develop and offer new solutions to material processing-related issues in the electronics industry. By investigating the opportunities afforded by the recently developed RheoMetalTM rheocasting process, a better understanding of the critical factors needed for an effective manufacturing process and optimised component characteristics was achieved. A study of the evolution of microstructure at different stages of the RheoMetalTM process demonstrated the influence of multistage solidification on the microstructural characteristics of the rheocast components. The microstructure of a slurry consists of the solute-lean and coarse globular α-Al particles with a uniform distribution of alloying elements, suspended in the liquid matrix. Additional solute-rich α-Al particles were identified as being a consequence of discrete nucleation events taking place after the initial slurry production. In the final components, macrosegregation was observed in the form of variations in the ratio of solute-lean coarse globular α-Al particles and solute-rich fine α-Al particles in both longitudinal and transverse directions. The relation between microstructural characteristics and material properties was established by determination of the local properties of a rheocast component. The fracture of a rheocast telecom component was strongly affected by microstructural inhomogeneity. In particular, macrosegregation in the form of liquid surface segregation bands and sub-surface pore bands strongly affected the fracture behaviour. Thermal conductivity measurements revealed that regions of the component with a high amount of solute-lean globular α-Al particles showed higher thermal conductivity. The effect of the local variation in thermal conductivity on the thermal performance of a large rheocast heatsink was evaluated by simulation. The results clearly show the importance of considering material inhomogeneity when creating a robust component design.

The vehicles industry is facing increasing demands for fuel efficiency and cost reduction due to environmental legislation, sustainability and customer demands. Therefore, there is a great need to develop and produce lightweight components by using materials and processes that offer higher specific strength and/or design optimization. Semi‐solid aluminium casting offers design freedom and castings with lower shrinkage and gas entrapment defects compared to high pressure die castings. The lack of understanding of microstructure and defect formation, and design data, for semi‐solid castings is a barrier for foundries and designers in the vehicles industry to use semi‐solid castings. In this study, the effect of two grain refiners on slurry formation and surface segregation of semi‐solid Al‐7Si‐0.3Mg castings produced by the Rheometal™ process was evaluated. The influence of grain refinement on primary α‐Al grain size, shape factor and solid fraction was analysed in addition to the solute content of the surface segregation layer. The influence of magnesium on the formation of intermetallic phases during solidification and the heat treatment response of Al‐7Si‐Mg semi‐solid castings was investigated. The magnesium content was varied from 0.3 to 0.6wt.% and the semi-solid castings were analysed in the T5 and T6 conditions. Energy dispersive spectroscopy was used to identify the intermetallic phases formed during solidification. Tensile testing was performed and the results were correlated to the magnesium and silicon concentration measured in the interior of the α‐Al globules formed during slurry preparation. The results suggest that the addition of grain refiner decreases the solid fraction obtained in the Rheometal™ process. However, no significant effect was observed on the α‐Al grain size and shape factor. A good correlation was obtained between the magnesium concentration in the interior of the α‐Al globules formed during slurry preparation and the offset yield strength for all alloys. The low magnesium solubility in α‐Al at temperatures in the solidification range of the Al‐7Si‐Mg alloys is suggested to be the reason for the low hardening response for the T5 heat treatment compared to the T6 condition.

A novel on-line capillary rheometer (OLR) was used to examine the shear and extensional characteristics of polyolefin melts during twin screw extrusion (TSE). Comparisons with off-line rheometry were made using a twin-bore capillary rheometer and a modular in-line slit die rheometer (ILR) provided in-line rheometry comparisons. Both capillary rheometers were controlled via PCs running dedicated software, and the extrusion line and ELR were fully instrumented allowing real-time process monitoring to be carried out by IBM compatible PCs via data acquisition hardware and software. The prototype OLR was developed by the re-design of several key features including an instrumented transfer section and capillary die block which facilitated the use of various die geometries. Shear and extensional on-line rheometry of three polyethylenes (linear and branched), and four molecular weight grades of polypropylene were examined, and a direct comparison with off-line capillary rheometry showed a good correlation. The effect of a high loading of filler on two of the polyethylenes was investigated. In-line shear stress and entry pressure measurements showed a reasonable correlation with on-line rheometry. A study of entry flows in the OLR using capillary dies approaching orifice showed non-linearities occurred at very low capillary length to diameter(L:D) ratios, and this was repeatable using off-line rheometry. Predicted zero length entry pressures (Po) were used to estimate apparent extensional viscosity using a number of standard models. Melt instability and capillary wall slip were also investigated using on-line rheometry. Melt pressure and temperature in the twin screw extruder and OLR were monitored at various process conditions to examine the ability of the OLR to condition melt during testing, and the effect of OLR testing on extrusion conditions. Pressure variation in the extruder, OLR and off-line rheometer were compared in order to quantify process noise. The effect of OLR testing on melt rheology and polymer molecular weight were examined using off-line rheometry and gel permeation chromatography(GPC).

An in-line process rheometer, employing a proven shear-stress transducer, was designed and built for polymer melts. The entire process stream runs through the rheometer, giving it a much faster response time than conventional side-stream models. The possibility of using the in-line rheometer for dynamic mechanical analysis was investigated and methods were developed to obtain the complex modulus over a wide range of frequencies with a single measurement. Measurement techniques for shear viscosity testing were also developed along with algorithms to compensate for the effects of process pressure and temperature.
The rheometer was used as a viscosity sensor to provide feedback control for a polypropylene visbreaking process. A first order plus dead time model was used to model the process and the rheometer together, and typically had dead times of less than 60 s and a first order time constant of 15 s. Gain scheduling was incorporated into minimum variance and proportional-integral controllers to achieve closed-loop settling times of 200 s for viscosity setpoint changes and process disturbances.

Innovative materials with novel properties are in great demand for use in the criticalcomponents of emerging technologies, which promise to be more cost-effective and energyefficient.A controversial issue with regard to manufacturing complex industrial products isto develop advanced materials with optimised manufacturability in addition to the requiredmechanical and physical properties. The objective of this research study was to develop andoffer new solutions in material-processing-related issues in the field of mechanical andelectrical engineering. This was achieved by investigating the new opportunities affordedby a recently developed rheocasting method, RheoMetalTM process, with the goal of comingto an understanding of the critical factors for effective manufacturing process. A study of the evolution of microstructure at different stages of the rheocasting process,demonstrated the influence of multistage solidification on the microstructural characteristicsof the rheocast components. The microstructural investigation onquench slurry showed itconsists of the solute-lean coarse globular α-Al particles with uniform distribution ofalloying elements, suspended in the solute-rich liquid matrix. Such inhomogeneous slurryin the sleeve seems to play a critical role in the inhomogeneity of final microstructure. Inthe rheocast component, the separation of the liquid and solid parts of slurry during fillinginfluenced on the microstructural inhomogeneity. The relationship between the microstructural characteristics and properties of the rheocastcomponents was investigated. The study on the fracture surfaces of the tensile-testedspecimens showed that the mechanical properties strongly affected by microstructuralinhomogeneity, in particular macrosegregation in the form of near surface liquid segregationbands and subsurface porosity. The thermal conductivity measurement showed variation ofthis property throughout the rheocast component due to variations in the ratio of solute-leanglobular α-Al particles and fine solute α-Al particles. The result showed silicon in solidsolution have a strong influence (negative) on thermal conductivity and precipitation ofsilicon by heat treatment process increase the thermal conductivity.
RheoCom

The quality of continuous fiber reinforced polymer matrix composite parts and structures depends strongly on the friction during the composite forming process. The two major types of friction that cause deformations during this process are ply-ply friction and tool-ply friction. One of the challenges in the composite forming process is the occurrence of wrinkling and shape distortion of the fabric caused by the surface differences between the forming tool and surface of the laminate. Frictional measurements of composites can vary widely depending on processing parameters, measurement technique, and instruments used. In this study, a commercial rheometer was used to evaluate tool-ply friction of unidirectional carbon fiber epoxy prepreg at various contact pressures, temperatures and sliding velocities. Viscoelastic properties such as the complex viscosity (η*), storage modulus (G'), loss modulus (G"), and loss factor (tan δ) were used to determine the critical transition events (such as gelation) during cure. An understanding of changes in viscoelastic properties as a function of time, temperature, and cure provides insight for establishing a suitable processing range for compression forming of prepreg systems. Surface imaging results were coupled with rheological results to qualitatively examine the effects of processing parameters on prepreg distortions. Changes in gap height over the measurement interval qualitatively describe the changes in contact area and contact mechanisms between the tool-ply surfaces. The results indicate that friction behavior of the prepreg system is a contribution of adhesive and frictional forces, where increase in viscosity, reduction in gap height, and cure of the sample correlate to higher friction values.
Master of Science
The quality of composite parts and structures depends strongly on the friction present during the composite forming process. One of the major challenges in the forming process is the occurrence of wrinkling and shape distortions of the fabric caused by the surface differences between the forming tool and material. The presence of these defects can compromise the final material property and lead to failure when in use. Frictional measurements of composites can vary widely depending on processing parameters, measurement technique, and instruments used. The extent of interaction between the tool and surface of the material depends on the tooling height, and by extension, contact area, which cannot easily be monitored with traditional test designs. A commercial rheometer was used in this study to evaluate tool-ply friction of unidirectional carbon fiber epoxy prepreg at various contact pressures, temperatures, and sliding velocities. Gap height and torque were monitored to provide information on the frictional dependence of processing parameters. In addition, surface-imaging results were coupled with rheological results to examine the relationship between friction and fiber distortions. The understanding of changes in material property with respect to the tooling process is the key to optimizing the composite forming process.

Additives, incorporated in film coating formulations, and their process parameters are generally selected using a trial-and-error approach. However, coating problems and defects, especially those associated with aqueous coating systems, indicate the necessity of embracing a quality-by-design approach to identify the optimum coating parameters. In this study, the feasibility of using thermal and rheological measurements to help evaluate and design novel coating formulations has been investigated. Hydroxypropyl methylcellulose acetate succinate (HPMCAS), an enteric coating polymer, was used as the film forming polymer. Differential Scanning Calorimetry (DSC), Dynamic Mechanical Analysis (DMA), and Parallel Plate Shear Rheometery (PPSR) were used to evaluate the effect of different plasticisers on the performance of HPMCAS. The results illustrate that, for identical formulations, the DSC and DMA methods yielded up to 40% differences in glass transition temperature (Tg) values. Moreover, Tg measured using loss modulus signals were always 20-30 oC less than those measured using tan delta results in DMA testing. Absolute and relative Tg values can significantly vary depending on the geometry of the samples, clamp size, temperature ramping rate and the frequency of the oscillations. Complex viscosity data for different formulations demonstrated a variable shear thinning behaviour and a Tg independent ranking. It is, therefore, insufficient to rely purely on Tg values to determine the relative performance of additives. In addition, complex viscosity results, obtained using both the DMA and PPSR techniques at similar temperatures, are shown to be comparable. The results from both techniques were therefore used to produce continuous master curves for the HPMCAS formulations. Additionally, step strain tests showed that HPMCAS chains do not fully III disentangle after 105 seconds as predicted by the Maxwell model. Finally, in situ aqueous-based coating experiments proved that mixtures of triethyl acetyl citrate and acetylated monoglyceride (TEAC/AMG), even without cooling of the suspension, do not cause blocking of the spray nozzle whereas triethyl citrate (TEC) based formulae did. TEAC (alone or in a combination with AMG) exhibits superior wettability to HPMCAS than TEC/AMG formulations and can be used to enhance the efficiency and film quality of the dry coating process.

La biomasse lignocellulosique comprend les sous-produits agricoles et industriels pouvant être utilisés comme matière première dans des bioprocédés variés destinés à produire des molécules d'intérêt énergétique ou chimique. Ces ressources lignocellulosiques, peuvent notamment être fournies par l'industrie papetière qui est particulièrement adaptée pour les bio-raffineries modernes car elle est en capacité de produire en grande quantité un substrat ayant une faible teneur en lignine et sans composés inhibiteurs. La bagasse de canne à sucre est également un substrat prometteur par sa composition chimique simple et son abondance dans les pays tropicaux. Lors de l'utilisation de ces substrats, l'hydrolyse enzymatique constitue une étape cruciale permettant la transformation des fibres de cellulose en une source de carbone fermentescible. Si les aspects biochimiques de cette étape d'hydrolyse font l'objet de nombreuses recherches et de développements, les réactions sous haute teneur en matière sèche font apparaître des limitations physiques qui sont beaucoup moins étudiées et analysées mais constituent des verrous scientifiques et technologiques qui freinent actuellement l'utilisation de cette ressource abondante et durable. Ce travail s'inscrit dans ce contexte et propose l'étude de cette étape d'hydrolyse enzymatique de la lignocellulose en s'intéressant conjointement aux aspects biochimiques et physiques de façon à aller vers une compréhension et une maîtrise des transferts (de masse, de chaleur) dans les réactions à forte concentration en substrat. La stratégie adoptée a consisté à réaliser et analyser des réactions d'hydrolyse sous différentes conditions opératoires en travaillant dans un premier temps sur des concentrations intermédiaires (suspension semi-diluée), c'est-à-dire en introduisant, mais de façon limitée, les complexités dues aux interactions entre particules/fibres de lignocellulose. Les résultats obtenus sont ensuite utilisés pour élaborer une stratégie adaptée aux fortes concentrations. Les aspects physiques analysés sont essentiellement le comportement rhéologique du milieu réactionnel ainsi que la morpho-granulométrie des objets en suspension. Différentes métrologies, tant in-situ que ex-situ, ont été mises en œuvre et apportent des résultats complémentaires. Les études ont été menées sur un substrat de référence, le papier Whatman, et deux substrats à vocation industrielle: la pâte à papier et la bagasse de canne à sucre. La stratégie d'étude porte sur les aspects suivants: (i) le suivi de l'évolution des comportements rhéologiques et des propriétés morphologiques des suspensions au cours de l'hydrolyse, (ii) l'étude des mécanismes d'hydrolyse lors de la dégradation des substrats, (iii) l'étude de l'impact de la composition et de la structure des substrats sur les cinétiques de solubilisation et d'hydrolyse, (iv) la quantification de la contribution des différentes activités enzymatiques, seules ou en mélange par une approche physique multi-échelle et (v) le contrôle et l'optimisation des conditions d'alimentation dans un procédé discontinu alimenté (fed-batch) afin d'atteindre des conditions de milieu concentré. Les chapitres 1 et 2 de ce document sont consacrés à une étude bibliographique du sujet et à la présentation des matériels et méthodes mis en œuvre. Le troisième chapitre présente les résultats obtenus et leur analyse. Il est constitué de trois sections: tout d'abord une étude des propriétés des différents enzymes ou cocktail d'enzymes utilisés, des substrats retenus et des suspensions avec, notamment, la détermination des régimes semi-dilués et concentrés. Ensuite sont présentées et analysées les hydrolyses effectuées en milieu semi-dilué. Les mécanismes d'hydrolyse (fragmentation, solubilisation, hydratation et séparation des agglomérats) sont étudiés pour diverses concentrations et divers enzymes/cocktails. Enfin les résultats en milieu concentré sont présentés dans une dernière section
Lignocellulosic biomass consists of several agriculture and industrial by-products that can be used as raw material for several bioprocesses to obtain range of products. Among lignocellulosic sources, the pulp & paper industry is appropriated for modern bio-refining thank to pulp with low lignin content and free of inhibitory compounds. Besides, sugarcane bagasse is a very promising feedstock because of its simple chemical composition and its abundancy especially in tropical countries. In the bioconversion of lignocellulose, enzymatic hydrolysis is a crucial step that allows the transformation of cellulosic and hemicellulosic fibers into fermentable carbon sources. The lack of knowledge about physical limitations and hydrolysis mechanisms, especially at high dry matter content, stands as the main barrier which forbids the scale-up of bio-refinery processes. Thus, the efficient and sustainable use of lignocellulosic resources is currently a major challenge and need to be investigated. In this context, this PhD focused on the enzymatic hydrolysis of lignocellulose by both physical and biochemical approaches. The strategy consisted in carrying out and in analyzing the hydrolysis reactions under different operating conditions with semi-dilute suspensions. Then, obtained results were used to develop a hydrolysis strategy for concentrated suspensions. Different methodologies, in- and ex-situ analyses, were implemented and provided complementary results. From physical approach, analyses consisted in rheological behavior of suspensions as well as the morpho-granulometry of particles. The study was carried out on a reference substrate, Whatman paper, and on two industrial substrates, paper pulp and sugarcane bagasse. The strategy aimed to investigate different stakes: (i) evolution of rheological behaviors and the morphological properties of suspensions, (ii) hydrolysis mechanisms during the degradation of substrates, (iii) impact of substrate composition and structure on solubilization and hydrolysis kinetics, (iv) quantification of the contribution of single enzyme and enzyme mixture activities by multi-scale physical approaches and (v) control and optimization of feeding parameters for fed-batch process in order to access to concentrated suspension. Chapters 1 and 2 of this document are devoted to a research bibliographic and presentation of materials and methods. The third chapter presents obtained results and discussion in three sections. The first one is a study of the properties of different enzymes and substrates, in particular, the determination of semi-dilute and concentrated regime. Subsequently the enzymatic hydrolysis at semi-dilute regime is presented to highlight the hydrolysis mechanisms (fragmentation, solubilization, solvation and agglomerate separation) in relationship with enzyme mixtures and dosages. Finally, results in concentrated regime are discussed in the final section

This project considers the co-rotating twin screw extrusion of a confectionery paste comprising powdered proteins, sugars, water and fats. As is the case with many food industry products, this process has been developed experimentally with little quantitative understanding of how variations in processing conditions influence the formation of the extrudate. A variety of techniques have therefore been developed to characterise and quantify the dispersive mixing, distributive mixing and rheological flow properties of this complex, multiphase, viscoelastic, unstable material. These techniques have then been utilised in a pilot plant extruder study of the mechanics of mixing and paste formation during extrusion, considering the influence of both processing conditions and screw profile. The internal evolution of paste microstructure has been successfully tracked along the length of screw profile using dead-stop extractions of the screws. A rigorous off-line assessment of shear yield strength behaviour using cone penetrometry has shown the use of conventional off-line rheometers to be unviable due to rapid post extrusion hardening. This highlighted the need for an in-line rheological measurement technique for continuous extrusion analysis where the extruded material is severely time dependent and not extractable. In pursuit of this, a novel arrangement of bender elements is proposed and trialled, to rapidly characterise material parameters of viscoelastic pastes. A second technique looking to extend the application of shear wave interface reflection to multiphase pastes is also trialled. A novel analysis of thermogravimetric data (TGA) has generated a viable index of distributive mixing, suitable for use on complex multi-component materials where thermal decomposition temperatures of the components are not well defined. Quantitative image analysis of pastes using scanning electron microscopy (SEM), optical microscopy protein staining and a novel application of multiphoton microscopy (MPM) have been used to visualise paste microstructure and quantify dispersive mixing. From the pilot plant extruder study, the application of these techniques was successful in mapping the evolution of paste mixing and the resulting microstructure, as well as identifying key differences between pastes mixed by twin screw extrusion and batch mixing.

Im Rahmen der vorliegenden Arbeit wurden verschiedene duroplastische Formmassen laboranalytisch hinsichtlich der rheologischen und thermischen Eigenschaften untersucht. Es wurde u.a. gezielt die absolute Materialfeuchte gesteigert, um den Einfluss dieser auf das Fließ­ Härtungsverhalten zu charakterisieren. Anschließend wurden die Materialien auf einer hochinstrumentierten Spritzgussmaschine mit einem Fließspiralenwerkzeug untersucht. Dabei konnte ein direkter Zusammenhang zwischen dem Rückfluss und dem Plastifizierdrehmoment in Abhängigkeit der Materialfeuchte und der Prozessparameter detektiert werden . Des Weiteren wurden über die Differenzdruckmessung im Fließspiralenwerkzeug die scheinbaren Viskositäten über den Fließweg ermittelt. Hierbei konnten unterschiedliche Aufschmelzeffekte über die Fließweglänge in Abhängigke it der duroplastischen Formmasse, der absoluten Materialfeuchte und der Prozessparameter detektiert werden . Durch Schererwärmung konnte die Formmassentemperatur teilweise die Werkzeugtemperatur übersteigen. Hinsichtlich der mechanischen Eigenschaften (Schlagzähigkeit, Biegefestigkeit) konnten keine signifikanten Einflussgrößen detektiert werden. Hinsichtlich des Tg konnten systematischen Unterschiede detektiert und begründet werden. Die beste Möglichkeit zur Ermittlung des Tg lieferte die TMA. Die thermischen Glasübergänge korrelieren mit den in der DSC ermittelten Aushärtegraden , wobei mit steigender Materialfeuchte ein geringer Aushärtegrad detektiert wird.
Within this paper, the rheologieal and thermie eharaeteristies of different thermosetting molding eompounds were investigated using lab analysis methods. Among others, the absolute moisture eontent was inereased purposefully to investigate its influenee on the flow-euring behavior. Subsequently, the materials were analyzed using a highly instrumented injeetion-molding maehine and a flow spiral tool. A direet link between the baekflow and the plastifieation torque dependent on the moisture eontent and proeess parameters was deteeted . Furthermore, a measurement of the differential pressure was eondueted within the flow spiral to deteet the apparent viseosity over the flow path. Within this proeess, different melting effeets over the flow eurve length depending on the molding eompound, the absolute moisture eontent and proeess parameters were deteeted. The shear heating lead to a material temperature inerease of the molding eompound, whieh was partly higher than the tool temperature . Coneerning the meehanieal eharaeteristies (impaet strength, flexural strength), no signifieant influeneing faetors eould be deteeted. In eontrast, systematie differenees of the glass transition temperature were deteeted and their eause eould be explained. The best way to determine the glass transition is the TMA. The glass transition temperatures eorrelate with the degree of eure determined with the DSC, whereas an inereasing moisture eontent is assoeiated with a lower degree of eure.

Yes
Real time measurement of melt rheology has been investigated as a Process Analytical Technology (PAT) to monitor hot melt extrusion of an Active Pharmaceutical Ingredient (API) in a polymer matrix. A developmental API was melt mixed with a commercial copolymer using a heated twin screw extruder at different API loadings and set temperatures. The extruder was equipped with an instrumented rheological slit die which incorporated three pressure transducers flush mounted to the die surface. Pressure drop measurements within the die at a range of extrusion throughputs were used to calculate rheological parameters such as shear viscosity and exit pressure, related to shear and elastic melt flow properties respectively. Results showed that the melt exhibited shear thinning behavior whereby viscosity decreased with increasing flow rate. Increase in drug loading and set extrusion temperature resulted in a reduction in melt viscosity. Shear viscosity and exit pressure measurements were found to be sensitive to API loading. These findings suggest that this technique could be used as a simple tool to measure material attributes in-line, to build better overall process understanding for hot melt extrusion.