Continuous wet granulation using a twin-screw extruder has attracted considerable attentions in pharmaceutical industry as it ensures consistent tablet quality at a high production rate. However, challenge still exists in controlling desired granule properties especially when different sized twin-screw granulators are used. This study therefore explored the potential of scalability of two sized twin-screw extruders and the how raw materials affect granules properties in two twin-screw extruders. The first study focuses on aspects of scaling using two twin-screw extruders, 18mm and 27mm. Dimensionless groups including Fr Number, Powder Feed Number and Degree of Fill (<30%) were studied to observe their influences on granule attributes. It was found that these dimensionless groups demonstrated inconsistent effects on granule properties and the effect of Powder Feed Number was highly dependent on Degree of Fill. Different extruder still exerts significant impact on granule properties. A scaling rule was established for median granule size (d50) only, but only moderate degree of fit was found. Although a considerable number of studies have been published on controlled-release and extended-release excipients, little attentions have been given to the influence of microcrystalline cellulose (MCC) grades in twin-screw wet granulation. The second study therefore investigated the processability of five grades MCC from the Avicel® PH family using two twin-screw extruders again, 18mm and 27mm. Granule attributes including particle size, density, moisture, and strength were tested and it was found that MCC inherent density has the most significant impact on granule properties while particle size of MCC has minor positive effect on granule size. This study also concluded that better granule flowability and uniformity can be achieved by using low moisture, larger particle size and high density MCC as excipients. / Thesis / Master of Applied Science (MASc)

Modern manufacturing needs to optimize the entire product lifecycle to satisfy the customer needs. The advancement of sensing technologies has brought a data rich environment for manufacturing and provide a great opportunity for real-time, proactive quality assurance. However, due to the lack of methods for analyzing heterogeneous types of data, the transformation of data to information and knowledge for effective decision making in manufacturing is still a challenging problem. In particular, functional variables can represent the in situ process conditions and rich product performance information, and are widely encountered in various manufacturing processes. In this dissertation, I will focus on modeling of manufacturing processes with in situ process (functional) variables, and integrating these functional variables and other measured variables for the manufacturing modeling. The modeling is explored by extracting informative features through the integration of multiple functional variables, functional variables and offline setting variables, and quantitative and qualitative quality variables. After an introduction in Chapter 1, three research tasks are investigated. First, a functional variable selection problem is studied in Chapter 2 to identify the significant functional variables as well as their features in a logistic regression model. A hierarchical non-negative garrote constrained estimation method is proposed. Second, the quality-process relationships for scalar offline setting variables, functional in situ process variables, and manufacturing quality responses are studied in Chapter 3. A functional graphical model that can integrate functional variables in a graphical model is proposed and investigated. Third, the quantitative and qualitative quality responses are jointly modeled with scalar offline setting variables and functional in situ process variables in Chapter 4. A functional quantitative and qualitative model is proposed and investigated. Finally, I summarize the research contribution and discuss future research directions in Chapter 5. The proposed methodologies have broad applications in manufacturing processes with functional variables, and are demonstrated in a crystal growth process with multiple functional variables (Chapter 2), a plasma spray process with multiple scalar and functional variables (Chapter 3), and an additive manufacturing process called fused deposition modeling with quantitative and qualitative quality responses (Chapter 4). / Ph. D.

O processo de estampagem é influenciado por diferentes variáveis, tais como, propriedades mecânicas e rugosidade da chapa, lubrificação do blank, coeficiente de atrito entre o blank e a ferramenta, parâmetros da prensa (força relativamente constante e velocidade), bem como variações nas ferramentas de conformação (deformação elástica). Este trabalho se dedica a investigação da influência do atrito entre a ferramenta e o blank. Em particular, será investigado o desenvolvimento de padrões artificiais de rugosidade de chapas metálicas (textura de superfície). O foco do presente trabalho é o estudo, em condições industriais, da inter-relação entre topografia superficial caracterizada pelos parâmetros de rugosidade 2D e 3D e estampabilidade de chapas de aço para painéis automotivos. Diferentes texturas superficiais de chapas de aço foram analisadas em termos de estampabilidade (medido pelo deslocamento do blank durante a estampagem) e tentativamente relacionadas com os parâmetros de rugosidades (2D e 3D) obtidos na chapa antes de estampar. Algumas tendências relevantes foram estabelecidas entre estes parâmetros. Os resultados aqui apresentados estão em concordância com publicações recentes mostrando uma clara relação entre estes parâmetros e que trabalhos futuros são necessários. / The stamping process is influenced by several variables such as sheet mechanical properties and roughness, blank lubrication, friction coefficient, press parameters (press force and speed), as well as variations in the forming tools (elastic strain). This work is dedicated to study the influence of friction between the tool and the blank. In this sense, it is necessary to study the development of artificial roughness patterns of sheet metals (surface textures). The aim of this research work is to study the inter-relationship, using the surface topography characterized by 2D and 3D roughness parameters and the formability of steel sheets for automotive panels. Different surface textures of sheet metal have been evaluated in terms of formability (measured by material flow during the process stamping) and tentatively related to roughness parameters (2D and 3D) obtained in the sheet metal prior to stamping. Some relevant tendencies have been established amongst these parameters. The results presented here are in accordance with other recently published research work showing that there is a clear relationship between these parameters, and that further detailed studies are needed.

O processo de estampagem é influenciado por diferentes variáveis, tais como, propriedades mecânicas e rugosidade da chapa, lubrificação do blank, coeficiente de atrito entre o blank e a ferramenta, parâmetros da prensa (força relativamente constante e velocidade), bem como variações nas ferramentas de conformação (deformação elástica). Este trabalho se dedica a investigação da influência do atrito entre a ferramenta e o blank. Em particular, será investigado o desenvolvimento de padrões artificiais de rugosidade de chapas metálicas (textura de superfície). O foco do presente trabalho é o estudo, em condições industriais, da inter-relação entre topografia superficial caracterizada pelos parâmetros de rugosidade 2D e 3D e estampabilidade de chapas de aço para painéis automotivos. Diferentes texturas superficiais de chapas de aço foram analisadas em termos de estampabilidade (medido pelo deslocamento do blank durante a estampagem) e tentativamente relacionadas com os parâmetros de rugosidades (2D e 3D) obtidos na chapa antes de estampar. Algumas tendências relevantes foram estabelecidas entre estes parâmetros. Os resultados aqui apresentados estão em concordância com publicações recentes mostrando uma clara relação entre estes parâmetros e que trabalhos futuros são necessários. / The stamping process is influenced by several variables such as sheet mechanical properties and roughness, blank lubrication, friction coefficient, press parameters (press force and speed), as well as variations in the forming tools (elastic strain). This work is dedicated to study the influence of friction between the tool and the blank. In this sense, it is necessary to study the development of artificial roughness patterns of sheet metals (surface textures). The aim of this research work is to study the inter-relationship, using the surface topography characterized by 2D and 3D roughness parameters and the formability of steel sheets for automotive panels. Different surface textures of sheet metal have been evaluated in terms of formability (measured by material flow during the process stamping) and tentatively related to roughness parameters (2D and 3D) obtained in the sheet metal prior to stamping. Some relevant tendencies have been established amongst these parameters. The results presented here are in accordance with other recently published research work showing that there is a clear relationship between these parameters, and that further detailed studies are needed.

[EN] Dehydration is one of the most commonly used operations in the food industry, and although its aim is to extend the shelf life of foods by reducing their water activity, it could also involve quality degradation. Vacuum freeze-drying may be considered one of the best drying methods for the purposes of preserving the organoleptic and nutritional properties of the fresh product, but its high processing cost limits its use to high value-added products. Convective drying at low temperatures could be considered an alternative means of obtaining high quality products at lower cost. However, the low drying rates at low temperatures (T<20ºC) and atmospheric pressure makes its industrial application difficult. In this sense, high intensity ultrasound (US) has been used to intensify mass transfer phenomena in food processing. It could be of great interest to apply US in low temperature drying because the ultrasonic effects are mainly mechanical (non-thermal). In this context, the main aim of this thesis was to determine the feasibility of US application in low temperature drying, addressing the effect on both the drying kinetics and the quality of the obtained products. For this purpose, apple, eggplant and cod samples were dried at different temperatures (-10, -5, 0, 5 and 10ºC), air velocities (1, 2, 4 and 6 m/s) and applying different ultrasonic powers (0, 25, 50 and 75 W). Diffusion models were used to describe the drying kinetics and to quantify the influence of the process variables. Moreover, different quality parameters (rehydration capacity, texture, antioxidant capacity...) of the dried products were determined. The application of US significantly (p<0.05) shortened the drying time under every drying condition and with each product tested, reducing the drying time by up to 80, 87 and 60% in apple, eggplant and cod samples, respectively. Thus, the greater the ultrasonic power applied, the shorter the drying time. The drying temperature and air velocity influenced the US efficiency and the best performance was achieved at the lowest drying temperatures and air velocities. In general terms, the diffusion model adequately fitted the drying kinetics of the three products tested. Although, in the case of US assisted drying, a better fit of the experimental data was obtained when the external resistance to water transfer was considered. The URIF (Uniformly Retreating Ice Front) model successfully fitted the atmospheric freeze drying kinetics. This model was validated under different experimental conditions. As regards the effect of the process variables on the quality parameters, in overall terms, it was observed that neither the US application nor the air velocity greatly influenced the quality of the obtained products. However, the temperature affected some quality parameters, such as rehydration capacity and color, especially at temperatures below the samples' freezing point. Finally, as a technology employed for the purposes of obtaining porous food matrices to be used further in the development of functional foods, US-assisted low temperature drying could be considered of great potential. Thus, from dried apple samples impregnated with olive leaf extract, it was observed that US application during drying did not significantly (p<0.05) influence the infusion capacity but did increase the antioxidant capacity of the final product. Therefore, high intensity ultrasound could be considered an interesting technology with which to speed-up the low temperature drying processes without greatly affecting the quality of the dried product. / [ES] La deshidratación, una de las operaciones más utilizadas en la industria agroalimentaria, mejora la estabilidad de los alimentos al reducir su actividad de agua, aunque puede afectar a su calidad. Entre las diferentes técnicas de secado existentes, destaca la liofilización a vacío por ser una de las que mejor conservan las propiedades organolépticas y nutricionales de los productos. Sin embargo, esta operación resulta muy cara y sólo se utiliza en productos de alto valor añadido. El secado convectivo a baja temperatura (T<20ºC) representa una alternativa para obtener productos de alta calidad a menor coste aunque su baja velocidad de proceso dificulta su implementación a nivel industrial. En este sentido, los ultrasonidos de alta intensidad (US) se han aplicado para intensificar operaciones de transferencia de materia en diferentes procesos agroalimentarios. Sus efectos son principalmente mecánicos (no térmicos), por lo que su uso en el secado a baja temperatura resulta altamente interesante. En este contexto, el objetivo general de la presente tesis doctoral fue determinar la viabilidad de la aplicación de US en procesos de secado a baja temperatura, abordando tanto su efecto en la cinética como en la calidad de los productos obtenidos. Para ello, se deshidrataron muestras de manzana, berenjena y bacalao a diferentes temperaturas (-10, -5, 0, 5 y 10ºC) y velocidades de aire (1, 2, 4 y 6 m/s) y aplicando diferentes niveles de potencia acústica (0, 25, 50 y 75 W). Se utilizaron modelos difusivos para describir las cinéticas de secado y cuantificar la influencia de las variables de proceso. Además, se determinaron diferentes parámetros de calidad (capacidad de rehidratación, textura, capacidad antioxidante,¿) de los productos deshidratados. La aplicación de US permitió reducir significativamente (p<0.05) el tiempo de secado en todas las condiciones experimentales y productos analizados, obteniendo reducciones de tiempo de secado de hasta el 80, 87 y 60% en manzana, berenjena y bacalao, respectivamente. La reducción del tiempo de secado fue mayor cuanto mayor fue la potencia acústica aplicada. La temperatura y la velocidad del aire de secado influyeron en la efectividad de la aplicación de US, siendo mayor el efecto de los US a las temperaturas y velocidades más bajas. En general, la teoría difusional describió adecuadamente la cinética de secado de los tres productos estudiados. En las experiencias con aplicación de US se obtuvo un mejor ajuste a los datos experimentales cuando se consideró la resistencia externa en el modelo. Asimismo, en condiciones de liofilización a presión atmosférica, el modelo URIF (Uniformly Retreating Ice Front) se ajustó adecuadamente a los datos experimentales. Además, este modelo se validó en diferentes condiciones experimentales. Respecto al efecto de las variables de proceso en los parámetros de calidad, en general, se observó que ni la aplicación de US ni la velocidad de aire influyeron de manera importante en la calidad de los productos obtenidos. En cambio, la temperatura afectó de manera relevante a parámetros como la capacidad de rehidratación y el color, especialmente a temperaturas por debajo del punto de congelación de las muestras. Por otro lado, el secado a baja temperatura asistido con US tiene un alto potencial para la obtención de matrices porosas alimentarias para su posterior utilización en el desarrollo de alimentos funcionales. Así, en muestras de manzana deshidratada e impregnada con extracto de hoja de olivo, se observó que la aplicación de US durante el secado no afectó significativamente (p<0.05) a la capacidad de impregnación, pero sí incrementó la capacidad antioxidante del producto obtenido. Por lo tanto, los ultrasonidos de alta intensidad se pueden considerar como una tecnología interesante para acelerar los procesos de secado a baja temperatura sin afectar en gran medida a la calidad del producto obtenido. / [CAT] La deshidratació, una de les operacions més utilitzades en la indústria agroalimentària, millora l'estabilitat dels aliments en reduir la seua activitat d'aigua, encara que pot afectar-ne la qualitat. Entre les diferents tècniques d'assecatge que hi ha, destaca la liofilització al buit per ser una de les que millor conserven les propietats organolèptiques i nutricionals dels productes, però resulta molt cara i només s'utilitza en productes d'alt valor afegit. L'assecatge convectiu a baixa temperatura (T<20ºC) representa una alternativa per a obtenir productes d'alta qualitat a menor cost. No obstant això, la baixa velocitat d'assecatge dificulta la seua implementació a nivell industrial. En aquest sentit, els ultrasons d'alta intensitat (US) s'han aplicat per a intensificar operacions de transferència de matèria en diferents processos agroalimentaris. El seu ús en l'assecatge a baixa temperatura resulta altament interessant pel fet que els seus efectes són principalment mecànics (no tèrmics). En aquest context, l'objectiu general de la present tesi doctoral va ser determinar la viabilitat de l'aplicació d'US en processos d'assecatge a baixa temperatura, abordant tant l'efecte en la cinètica del procés com en la qualitat dels productes obtinguts. Amb aquesta finalitat, es van deshidratar mostres de poma, albergínia i bacallà a diferents temperatures (-10, -5, 0, 5 i 10ºC) i velocitats d'aire (1, 2, 4 i 6 m/s) i aplicant diferents nivells de potència acústica (0, 25, 50 i 75 W). Es van utilitzar models difusius per a descriure les cinètiques de l'assecatge i quantificar la influència de les variables del procés. A més, es van determinar diferents paràmetres de qualitat (capacitat de rehidratació, textura, capacitat antioxidant...) dels productes deshidratats. L'aplicació d'US va permetre reduir significativament (p<0.05) el temps d'assecatge en totes les condicions experimentals i tots els productes analitzats; es van obtenir reduccions de temps de fins al 80%, 87% i 60% en pomes, albergínies i bacallà, respectivament. La reducció del temps d'assecatge va ser més alta com més alta va ser la potència acústica aplicada. La temperatura i la velocitat de l'aire de l'assecatge van influir en l'efectivitat de l'aplicació d'US, sent major l'efecte dels US a les temperatures i velocitats més baixes. En general, la teoria difusional va descriure adequadament la cinètica de l'assecatge dels tres productes estudiats. En les experiències amb aplicació d'US es va obtenir un millor ajust a les dades experimentals quan es va considerar la resistència externa en el model. Així mateix, en condicions de liofilització a pressió atmosfèrica, el model URIF (Uniformly Retreating Ice Front) es va ajustar correctament a les dades experimentals. A més, aquest model es va validar en diferents condicions experimentals. Respecte a l'efecte de les variables del procés en els paràmetres de qualitat, en general, es va observar que ni l'aplicació d'US ni la velocitat de l'aire van influir de manera important en la qualitat dels productes obtinguts. En canvi, la temperatura va afectar de manera rellevant a paràmetres com la capacitat de rehidratació i el color, especialment a temperatures per davall del punt de congelació de les mostres. D'altra banda, l'assecatge a baixa temperatura assistit amb US presenta un alt potencial per a obtenir matrius poroses alimentàries per a la posterior utilització en el desenvolupament d'aliments funcionals. Així, en mostres de poma deshidratada i impregnada amb extracte de fulles d'olivera, es va observar que l'aplicació d'US durant l'assecatge no va afectar significativament (p<0.05) la capacitat d'impregnació, però sí que va incrementar la capacitat antioxidant del producte obtingut. Per tant, els ultrasons d'alta intensitat es poden considerar com una tecnologia interessant per a accelerar els processos d'assecatge a baixa temperatura sense afectar de manera re / Santacatalina Bonet, JV. (2016). Contribución al estudio de la aplicación de ultrasonidos de alta intensidad en procesos de secado a baja temperatura [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/61484 / TESIS

Tungsten carbide (WC) based metallic matrix coatings sprayed using high velocity air fuel (HVAF) technique have attracted increasing attention as they show excellent tribological performance in various wear conditions. In the HVAF method, particles’ in-flight temperature and velocity can be influenced by the process variables including nozzle configuration as well as feedstock particle size range. On the other hand, the chemistry of metallic binder can also play a key role in determining both properties and performance of these coatings. In this thesis, characteristics and tribological behaviour of HVAF-sprayed WC-based coatings were investigated employing four different nozzle configurations (4L2, 4L4, 5L2and 5L4), and three different feedstock particle sizes of WC-CoCr feedstock powder (5/20, 5/30 and 15/45 μm). Also, characteristics and performance of coatings processed with four different WC-based feedstocks comprising alternative binders to traditionally used CoCr (namely CoCr, NiMoCrFeCo,FeNiCrMoCu and FeCrAl) were investigated. Characteristics of the coatings were explored by conducting scanning electron microscopy observations, microindentation testing and X-ray diffraction analysis. Performance of the coatings was evaluated by conducting sliding wear, dry jet erosion wear and sand rubber wheel abrasion wear testing. Moreover, material removal mechanisms in the coatings subjected to the above tests were investigated through post wear analysis. X-ray diffraction analysis showed that no considerable phase change compared to the starting feedstock was observed in any of the coatings sprayed by HVAF technique. It was revealed that decrease in powder particle size range can result in an improvement in microstructural characteristics, such as homogeneity and density, as well as hardness of the coatings. Besides, it can lead to a substantial improvement in wear performance of the coatings. It was shown that using various nozzle configurations does not result in any considerable change in characteristics or performance of the HVAF-sprayed WC-CoCr coatings. It was further shown that, by decreasing particle sizes from coarse to medium or fine, a significant difference can be observed. While wear mechanisms for medium and fine feedstock coatings were dominated by ploughing and fracture of individual carbide grains, for the coarse feedstock coatings ploughing and grooving along with the local removal of coating material were observed. Hardness values for all the four coatings with different binder chemistries were in a narrow range of 1100 – 1300 HV0.3. WC-NiMoCrFeCo and WC-FeNiCrMoCu coatings showed better or comparable sliding wear performance compared to WC-CoCr coating (as reference). WC-FeNiCrMoCu and WC-FeCrAl coatings showed comparable performance under erosion conditions while all the three binder alternatives yielded slightly inferior coating performance under abrasion wear, compared to the reference coating. While ploughing was the common wear mechanism in all the four coatings, pitting was noted in coatings with CoCr and FeNiCrMoCu binders in case of sliding wear. / Populärvetenskaplig Sammanfattning Cermet-beläggningar består av WC-partiklar inbäddade i ett metallbindemedel,sprutat med High Velocity Air Fuel (HVAF) uppvisar utmärkt tribologiskprestanda under olika slitage förhållanden. Med HVAF-tekniken kan partiklarnasflygtemperatur och hastighet påverkas av konfigurationen av den utrustning somanvänds såväl som partikelstorleksintervallet för råmaterialet. Därtill kan kemin hos det metalliska bindemedlet spela en nyckelroll för beläggningarnas egenskaper och prestanda. I denna avhandling undersöktes egenskaper och tribologiskt beteende hos HVAF-besprutade WC-baserade beläggningar. Undersökningen gjordes genom att använda fyra olika uppsättningar av ändra sprutparametrar förHVAF-processen där fyra olika munstyckskonfigurationer (4L2, 4L4, 5L2 och5L4) och tre olika partikelstorleksintervaller av WC-CoCr råvarupulver (5/20,5/30 och 15/45 μm). Studieegenskaper och prestanda för alla deponerade beläggningar, påverkan av processvariabler (olika munstyckskonfigurationer och olika partikelstorlekar) undersöktes. Dessutom undersöktes egenskaper och prestanda för tre olika WC-baserade råvaror med alternativa bindemedel till CoCr (NiMoCrFeCo, FeNiCrMoCu och FeCrAl) och jämfördes med WC-CoCrbeläggningsom referens. Beläggningens egenskaper undersöktes genom att genomföra SEM-analys, mikroindragningstest och röntgenanalys. Beläggningens prestanda utvärderades genom att utföra glidförslitning, erosionsslitage under torra förhållanden och test med torr sand/gummihjulanordning. Vidare undersöktes mekanismer för materialavlägsning i beläggningarna med ovanstående tester genom analys efter slitage. Ingen avsevärd fasförändring observerades för alla beläggningar som besprutades med HVAF-teknik. Det avslöjades att minskning av pulvrets genomsnittliga partikelstorlek resulterade i en förbättring av mikrostrukturella egenskaper, såsom homogenitet och densitet, samt beläggningarnas hårdhetsvärde. Dessutom leder det till en avsevärd förbättring av beläggningens slitageförmåga. Det visades att användning av olika munstycken till HVAF-processen inte resulterar i en avsevärd förändring i egenskaper eller prestanda hos WC-CoCr-beläggningarna. När det gäller förslitningsmekanismer visades det att genom att minska partikelstorleken från grov till medium eller fin sågs en avsevärd skillnad. För beläggningar besprutade med fina och medelstora partiklar dominerades förslitningsmekanismer av plöjningsslitage och sprickor av enskilda hårdmetallkorn. För grova beläggningar observerades plöjningsslitage och spårning tillsammans med avlägsnande av material. Ingen signifikant skillnad i mikrostruktur eller fasförändring observerades i alla beläggningar med alternativa bindemedel såväl som WC-CoCr som referensbeläggning. Hårdhetsvärdet för alla de fyra beläggningarna låg inom x intervallet 1100 - 1300 HV0.3. NiMoCrFeCo och FeNiCrMoCu visade bättre eller jämförbar glidförmåga med referensbeläggningen. FeNiCrMoCu och FeCrAl visade jämförbara prestanda under erosionsförhållanden och alla de tre undersökta beläggningsmaterialen visade något sämre prestanda under nötningsslitage jämfört med referensbeläggningen. Medan plöjningsslitage var den vanliga förslitningsmekanismen i alla de fyra beläggningarna noterades gropning i beläggningarna CoCr och FeNiCrMoCu vid glidförslitning.

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