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Additive manufacturing has become a very popular and well mentioned technique in recent years. The technique, where 3 dimensional (3D) printing is included, creates opportunities to develop new designs and processing systems. As a research institute within the forest based processes and products, Innventia AB has an idea of combining 3D printing with cellulose. The addition of cellulose will increase the proportion of renewable raw material contributing to more sustainable products. However, when cellulose is added the composition of the filaments changes. The main aim for the project is to devise methodologies to improve properties of composite filaments used for 3D printing. Filament in 3D printing refers to a thread-like object made of different materials, such as PLA and ABS, that is used for printing processes. A literature study was combined with an extensive experimental study including extrusion, 3D printing and a new technique that was tested including 3D scanning for comparing the printed models with each other. The extruding material consisted of polypropylene and cellulose at different ratios, and filaments were produced for 3D printing. The important parameters for extruding the material in question was recorded. Because the commingled material (PPC) was in limited amount, UPM Formi granulates, consisting of the same substances, was used first in both the extrusion and printing process. Pure polypropylene filaments were also created in order to strengthen the fact that polypropylene is dimensional unstable and by the addition of cellulose, the dimensional instability will decrease. After producing filaments, simple 3D models were designed and printed using a 3D printing machine from Ultimaker. Before starting to print, the 3D model needed to be translated into layer-by-layer data with a software named Cura. Many parameters were vital during printing with pure polypropylene, UPM and PPC. These parameters were varied during the attempts and marked down for later studies. With the new technique, in which 3D scanning was included, the 3D printed models were compared with the original model in Cura in order to overlook the deformation and shape difference. The 3D scanner used was from Matter and Form. Photographs of the printed models, results from the 3D scanner, and screenshots on the model in Cura were meshed together, in different angles, using a free application named PicsArt. The result and conclusion obtained from all three parts of the experimental study was that polypropylene’s dimensional stability was improved after the addition of cellulose, and the 3D printed models’ deformation greatly decreased. However, the brittleness increased with the increased ratio of cellulose in the filaments and 3D models. / Additiv tillverkning har på den senare tiden blivit en mycket populär och omtalad teknik. Tekniken, där tredimensionell (3D) utskrivning ingår, ger möjligheter att skapa ny design och framställningstekniker. Som ett forskningsinstitut inom massa- och pappersindustrin har Innventia AB en ny idé om att kombinera 3D-utskrivning med cellulosa. Detta för att höja andelen förnybar råvara som leder till mer hållbara produkter. Dock kommer filamentens sammansättning vid tillsättning av cellulosa att ändras. Det främsta syftet med detta projekt är att hitta metoder för att förbättra egenskaperna hos de kompositfilament som används för 3D-utskrifter. Filament inom 3D-utskrivning är det trådlika objektet gjort av olika material, såsom PLA och ABS, som används vid utskrivningsprocessen. En enkel litteraturstudie kombinerades med en experimentell studie. Det experimentella arbetet var i fokus i detta projekt som omfattade extrudering, 3D-utskrivning samt en ny teknik som prövades, där 3D-scanning ingick, för att jämföra de utskrivna modellerna med varandra. Extruderingsmaterialet bestod av polypropen och cellulosa av olika halter, och av detta material tillverkades filament för 3D-utskrivning. De viktiga parametrarna för extrudering med det önskade materialet antecknades. Eftersom mängden cominglat material (PPC) var begränsat, användes först UPM Formi granuler, som består av samma substanser som i PPC, i både extruderingen och utskrivningen. Filament av ren polypropen tillverkades också för att stärka det faktum att polypropen är dimensionellt instabil. Genom att tillsätta cellulosa minskades dimensionsinstabiliteten. Efter att filamenten hade tillverkats, designades enkla 3D-modeller för utskrivning med en 3D-utskrivare från Ultimaker. Innan utskrivningen kunde börja behövde 3D-modellen bli översatt till lager-på-lager-data med hjälp av en programvara vid namn Cura. Många parametrar är viktiga vid utskrivning med ren polypropen, UPM samt PPC. Temperatur och hastighet varierades för de olika försöken och antecknades för senare studier.Med den nya tekniken, där 3D-scanning ingår, jämfördes de utskrivna 3D-modellerna med originalmodellen i Cura för att se över deformationen och formskillnaden. Den 3D-scanner som användes kom från Matter and Form. Fotografier på de utskrivna modellerna, resultaten från 3D-scannern och bilder på modellerna i Cura sammanfogades i olika vinklar med hjälp av ett gratisprogram som heter PicsArt. Det resultat som erhölls och den slutsats som kunde dras utifrån alla tre delarna av den experimentella studien var att polypropens dimensionsinstabilitet minskades efter tillsatsen av cellulosa, och att de 3D-utskrivna modellernas deformation minskade kraftigt. Skörheten ökade ju högre halt cellulosa som filamenten och de utskrivna modellerna innehöll.

No / Mechanochemistry provides a method to reduce or eliminate the use of solvents by carrying out reactions through the grinding of neat reagents. Until recently a significant drawback of this form of synthesis has been the limited ability to scale up. However, it has been shown that twin screw extrusion (TSE) may overcome this problem as demonstrated in the continuous synthesis of co-crystals, Metal Organic Frameworks (MOFs) and Deep Eutectic Solvents (DES), in multi kg h−1 quantities. TSE has provided a means to carry out mechanochemical synthesis in a continuous, large scale and efficient fashion, which is adaptable to a manufacturing process. Herein, we highlight the potential of this technique for organic synthesis by reporting four condensation reactions, the Knoevenagel condensation, imine formation, aldol reaction and the Michael addition, to produce analytically pure products, most of which did not require any post synthetic purification or isolation. Each reaction was carried out in the absence of solvents and the water byproduct was conveniently removed as water vapour during the extrusion process due to the elevated temperatures used. Furthermore, the Knoevenagel condensation has been studied in detail to gain insight into the mechanism by which these mechanochemical reactions proceed. The results point to effective wetting of one reactant by another as being critical for these reactions to occur under these reaction conditions. / EPSRC EP/L019655/1

An environmentally benign process, which uses supercritical carbon dioxide (sc-CO₂) as a processing aid, was developed in this work to help exfoliate and disperse nanoclay into the polymer matrices at high clay content. The process involves the use of a pressurized CO₂ chamber to assist in the exfoliation and delivery of the clay into a stream of polypropylene (PP) melt within the extruder. This CO₂ method was evaluated and compared to other conventional processing techniques. It was observed that the conventional direct-melt compounding methods, with and without the direct injection of CO₂, did not show much improvement in the mechanical properties due to their inability to adequately exfoliate the nanoparticles into the polymer matrix. The commercial RTP sample prepared using a TSE and a MA compatibilizer showed moderate improvements in the clay dispersion and properties due to high shear forces and mixing capabilities of TSE. The most improvements were seen from the technique of using the pressurized CO₂ chamber, which directly injected pre-mixed sc-CO₂ and nanoclay into the polypropylene melt during extrusion. It was observed that the mechanical properties of the PP nanocomposites prepared using the CO₂ chamber technique, especially when combined with maleic anhydride (MA) compatibilizer, outperformed those of the commercial RTP samples and those of samples prepared using conventional melt compounding techniques. WAXD and TEM data showed a good degree of exfoliation for clay concentrations as high as 6.8 wt% when the clay was expanded and mixed with CO₂. At this concentration, mechanical properties such as yield strength and modulus increased by as much as 13% and 69%, respectively, relative to the pure PP, and approximately 15% higher than those of samples prepared by direct melt compounding (without the use of CO₂). Furthermore, yield-like behavior in the viscosity and a plateau in the low-frequency behavior of storage modulus, Gâ , was also attributed to polymer-clay interaction due to strong hydrogen bonding between MA groups and the hydroxyl groups on the clay surface, not just solely to the formation of percolation network due to exfoliation between clay platelets that is commonly reported in literature for clay-filled functionalized polypropylene. / Ph. D.

Although additive manufacturing technologies are often referred to as "3D printing," the family of technologies typically deposit material on a layer-by-layer basis. For material extrusion (ME) in particular, the deposition process results in weak inter- and intra-layer bonds that reduce mechanical performance in those directions. Despite this shortcoming, ME offers the opportunity to specifically and preferentially align the reinforcement of a composite material throughout a part by customizing the toolpath. Recent developments in multi-axis deposition have demonstrated the ability to place material outside of the XY-plane, enabling depositions to align to any 3D (i.e., non-planar) vector. Although mechanical property improvements have been demonstrated, toolpath planning capabilities are limited; the geometries and load paths are restricted to surface-based structures, rather than fully 3D load paths. By specifically planning deposition paths (roads) where the composite reinforcement is aligned to the load paths within a structure, there is an opportunity for a step-change in the mechanical properties of ME parts. To achieve this goal for arbitrary geometries and load paths, the author presents a design and process planning workflow that concurrently optimizes the topology of the part and the toolpath used to fabricate it. The workflow i) identifies the optimal structure and road directions using topology optimization (TO), ii) plans roads aligned to those optimal directions, iii) orders those roads for collision-free deposition, and iv) translates that ordered set of roads to a robot-interpretable toolpath. A TO algorithm, capable of optimizing 3D material orientations, is presented and demonstrated in the context of 2D and 3D load cases. The algorithm achieved a 38% improvement in final solution compliance for a 3D Wheel problem relative to existing TO algorithms with planar orientation optimization considerations. Optimized geometries and their associated orientation fields were then propagated with the presented alignment-focused deposition path planner and conventional toolpath planners. The presented method resulted in a 97% correlation between the road directions and the orientation field, while the conventional methods only achieved 77%. A planar multi-load case was then fabricated using each of these methods and tested in both tension and bending; the presented alignment-focused method resulted in a 108.24% and 29.25% improvement in each load case, respectively. To evaluate the workflow in a multi-axis context, an inverted Wheel problem was optimized and processed by the workflow. The resulting toolpaths were then fabricated on a multi-axis deposition platform and mechanically evaluated relative to geometrically similar structures using a conventional toolpath planner. While the alignment in the multi-axis specimen was improved from the conventional method, the mechanical properties were reduced due to limitations of the multi-axis deposition platform. / Doctor of Philosophy / The material extrusion additive manufacturing process is widely used by hobbyists and industry professionals to produce demonstration parts, but the process is often overlooked for end-use, load bearing parts. This is due to the layer-by-layer fabrication method used to create the desired geometries; the bonding between layers is weaker than the direction material is deposited. If load paths acting on the printed structure travel across those layer interfaces, the part performance will decrease. Whereas gantry-based systems are forced into this layer-by-layer strategy, robotic arms allow the deposition head to rotate, which enables depositions to be placed outside of the XY-plane (i.e., the typical layer). If depositions are appropriately planned using this flexibility, the layer interfaces can be oriented away from the load paths such that all of the load acts on the (stronger) depositions. Although this benefit has been demonstrated in literature, the existing methods for planning robotic toolpaths have limits on printability; certain load paths and geometries cannot be printed due to concerns that the robotic system will collide with the part being printed. This work focuses on increasing the generality of these toolpath planning methods by enabling any geometry and set of load paths to be printed. This is achieved through three objectives: i) identify the load paths within the structure, ii) plan roads aligned to those load paths, iii) order those roads such that collisions will not occur. The author presents and evaluates a design workflow that addresses each of these three objectives by simultaneously optimizing the geometry of the part as well as the toolpath used to fabricate it. Planar and 3D load cases are optimized, processed using the presented workflow, and then fabricated on a multi-axis deposition platform. The resulting specimens are then mechanically tested and compared to specimens fabricated using conventional toolpath planning methods.

Filament-based material extrusion (MatEx) additive manufacturing has garnered huge interest in both academic and industrial communities. Moreover, there is an increasing need to expand the material catalog for MatEx to produce end use parts for a wide variety of functional applications. Current approaches towards MatEx of semicrystalline thermoplastics are in their nascent stage with fiber reinforcements being one of the most common techniques. MatEx of commodity semicrystalline thermoplastics has been investigated but most of the current methods are extremely material and machine specific. The goal of this dissertation is to enable MatEx of semicrystalline polymers with mechanical properties approaching that of injection molded parts. Tailored molecular architectures of blends that can control the crystallization kinetics from the melt state are investigated. By modifying the crystallization time window, the time during which chain diffusion can occur across the deposited layers is prolonged, which allows for a stronger bond between layers. Such differences in the crystallization process impact the z-axis adhesion and residual stress state, which directly affect mechanical properties and warpage in the printed parts. The impact of blend composition on polymer chain diffusion, crystallization profiles, and print properties resulting from the repeated non-uniform thermal history in filament based MatEx is studied. The melt flow behaviour is characterized using rheology and its effect on the interlayer adhesion of printed parts and print precision is explored. The extent of polymer chain re-entanglement post deposition on the printer bed is quantitatively determined using interrupted shear rheology protocols. Tensile bars are printed and mechanically characterized to analyze the tensile performance of the printed parts. Correlating the rheological findings with the mechanical performance of the printed parts provides valuable insights into the complex interlayer welding process during MatEx and is critical to improving existing machine designs and feedstocks in order to achieve printed parts with properties approaching their injection molded counterparts. The results will be essential in identifying optimal processing conditions to maximize material specific printed part performance as well as highlight the associated limitations to enable MatEx of next generation materials. / Doctor of Philosophy / Compared to traditional subtractive manufacturing techniques, additive manufacturing (AM) has the potential to transform modern manufacturing capabilities due to its unique advantages including design flexibility, mass customization, energy efficiency, and economic viability. The filament-based material extrusion (MatEx), also referred to as fused filament fabrication (FFF), employing thermoplastic polymers (and composites) has emerged as one of the most common AM modality for industrial adoption due to its operational simplicity. However, the widespread application of MatEx has been limited due to the lack of compatible materials, anisotropic mechanical properties, and lack of quality assurance. Most of the research on FFF has been performed on amorphous polymers with almost negligible levels of crystalline content such as polylactic acid (PLA) and acrylonitrile-butadiene-styrene (ABS). Semicrystalline polymers are an attractive choice for FFF feedstocks compared to the amorphous ones due to their improved thermal resistance, toughness, and deformability. However, processing semicrystalline polymers using FFF is challenging due to the volumetric shrinkage encountered during crystallization from the melt state. This results in the buildup of significant levels of residual stresses at temperatures lower than the crystallization temperature of the polymer resulting in warpage of the printed parts. The research presented in this dissertation aims to address the aforementioned challenges by characterizing semicrystalline polymer feedstocks under conditions representative of the multiphysics encountered during a typical FFF process. Several strategies to limit shrinkage and warpage are discussed that involve tuning the thermal profile and crystallization kinetics during printing. The former is achieved by addition of thermally conductive carbon fiber reinforcements while the latter is realized by blending amorphous resins or low crystallinity polymers to the semicrystalline polymer matrix. The fibers results in a more homogenous temperature distribution during printing while the incorporation of the resins modify the rate of crystallization; both of which play a pivotal role in reducing the residual stress build-up and hence minimizing the warpage during printing. The printability of the materials is investigated based on the shear- and temperature dependent viscous response of the polymers. The printed parts with fiber reinforcements exhibit high levels of mechanical anisotropy compared to the blends with the resins, likely due to differences in polymer chain mobility at the interface. The tensile properties of the printed polymer blends are slightly inferior to those obtained using traditional manufacturing techniques; however, properties close to 90-95% of injection molded properties are recovered through a simple post-processing thermal annealing step. The obtained results will assist in optimizing the processing parameters and feedstock formulation in order to consistently produce printed parts with minimal defects and tailored mechanical properties for functional applications.

Cooking extrusion is becoming an essential processing step in a number of food processes. Modeling of extruder performance is the first step towards the ultimate goal of prediction of product properties and quality based on governing extruder characteristics and operation. The purpose of this study was to develop a numerical model of the cooking extrusion process. This involved. many facets of investigation. A 50% added moisture soy flour dough was selected as the material of study. The material properties for this 50% added moisture dough were then determined. The viscosity of this material was found to be both shear and temperature dependent in addition to exhibiting a yield stress. Both thermal conductivity and heat capacity were determined to be constant over the temperature range of investigation. Finally, although it was discovered that a reaction associated with cooking was present in the system, it was determined that it did not occur under the extrusion processes tested which were to be modelled and hence would not have to be accounted for in the model. These material properties were then incorporated in the three-dimensional finite element program, FIDAP, to model the flow of the l 50% added moisture soy flour dough through an extruder and die assembly. These numerical simulations yielded limited results. Only one case out of the multiple conditions which were attempted converged to a viable solution. As more success was found with a two-dimensional model, it is suggested that the problems of convergence could be due to mesh size and discretization of the three dimensional model as well as the difficult power law index of the material. Suggestions as to methods to overcome these problems are included. / Ph. D.

Tesis por compendio / [ES] «Aplicación de nuevas tecnologías a la alcalinización de cacao» es una tesis doctoral centrada, por un lado, en el estudio de los cambios fisicoquímicos y funcionales causados por dos técnicas de alcalinización alternativas a la convencional y, por otro, en la comparación de dichas propiedades con las de muestras comerciales. En el capítulo I, se describe un sistema de alcalinización basado en extrusión. Esta tecnología se ha aplicado a la alcalinización de cacao dada su capacidad de tratar la materia prima de forma rápida y continúa, y su bajo consumo energético. En primer lugar, se estudiaron los efectos de diversas variables de proceso sobre las propiedades fisicoquímicas y funcionales de cacaos en polvo. En general, de todas las variables, el tipo y la concentración de álcali fueron las principales responsables del incremento de pH, del oscurecimiento de las muestras y de la reducción en el contenido de compuestos funcionales. En cuanto a la humedad, fueron la temperatura y el contenido en agua las que mostraron causar los mayores efectos, llegando a producir reducciones de casi un 50%. Además de evaluarse el efecto de las diferentes variables, en este capítulo también se compararon los cacaos producidos mediante extrusión con los alcalinizados por el método convencional. Los resultados mostraron que la extrusión, en menos de cinco minutos, fue capaz de oscurecer y de producir cacaos en polvo con un perfil sensorial, una capacidad antioxidante y un contenido en polifenoles totales relativamente similar al de los productos comerciales. En cuanto al capítulo II, en este se ha estudiado la técnica de calentamiento por microondas como una alternativa al tratamiento de alcalinización tradicional. La tecnología microondas ha demostrado ser rápida, versátil y capaz de preservar las características funcionales y sensoriales, lo que ha hecho interesante su aplicación a la alcalinización de cacao. En los trabajos que forman este segundo capítulo, se estudiaron los efectos de diversas variables de proceso sobre el producto. En general, el tipo y la concentración de álcali fueron las variables principalmente responsables del oscurecimiento del cacao, del incremento del pH y de la reducción de las concentraciones de catequina y epicatequina. Sin embargo, el álcali empleado no redujo la actividad antioxidante ni al contenido en fenoles totales, propiedades que se vieron incrementadas por la presión, la potencia y la duración del tratamiento. Estos incrementos se relacionaron con la capacidad de estas variables para liberar a los polifenoles no extractables y para promover determinadas reacciones químicas. Además, también se estudió el efecto de las diferentes variables sobre la humedad. La potencia y la duración del tratamiento fueron las que se mostraron esenciales para lograr el secado del producto, llegando a producir reducciones de hasta el 70%. Por otro lado, además de estudiarse el impacto de las diferentes variables, también se compararon cacaos producidos por microondas con muestras producidas por el método convencional para evaluar su similitud con los cacaos comerciales. Los resultados mostraron que el microondas, en solo cuatro minutos, fue capaz de oscurecer el cacao y de mantener un perfil sensorial similar al producido por el método tradicional, a la par que conducía a una mejora en sus propiedades funcionales. En resumen, los métodos para la alcalinización de cacao desarrollados en el marco de la presente tesis doctoral han demostrado ser unas alternativas muy prometedoras a la tecnología convencional. Ambas técnicas no solo han sido capaces de oscurecer el cacao tanto como el método comercial en un tiempo mucho menor, sino que también han conseguido el secado parcial de la muestra y unas características sensoriales y funcionales comparables o incluso mejores que las del método convencional. / [CA] «Aplicació de noves tecnologies a l'alcalinització de cacau» és una tesi doctoral centrada, d'una banda, en l'estudi dels canvis fisicoquímics i funcionals causats per dos tècniques d'alcalinització alternatives a la convencional i, d'altra banda, en la comparació d'aquestes propietats amb les de mostres comercials. En el capítol I, es descriu un sistema d'alcalinització similar al convencional però basat en extrusió. Aquesta tecnologia s'ha aplicat a l'alcalinització de cacau per la seua capacitat de tractar la matèria primera de forma ràpida i continua, i pel seu baix consum energètic. En primer lloc, es van estudiar els efectes de diverses variables de procés sobre les propietats fisicoquímiques i funcionals de cacaus en pols. En general, de totes les variables, el tipus i la concentració d'àlcali van ser les principals responsables de l'increment de pH, de l'enfosquiment de les mostres i de la reducció en el contingut de compostos funcionals. Pel que fa a la humitat, van ser la temperatura i el contingut en aigua les que van causar els majors efectes, arribant a produir reduccions d'un 50%. A més d'avaluar l'efecte de les diferents variables, en aquest capítol també es van comparar els cacaus produïts mitjançant extrusió amb els alcalinizats pel mètode convencional. Els resultats van mostrar que l'extrusió, en menys de cinc minuts, va a ser capaç d'enfosquir i de produir cacaus en pols amb un perfil sensorial, una capacitat antioxidant i un contingut en polifenols totals relativament similar al dels productes comercials. Pel que fa al capítol II, en aquest s'ha estudiat la tècnica de calfament per microones com una alternativa a l'alcalinització tradicional. La tecnologia microones ha demostrat ser ràpida, versàtil i capaç de preservar les característiques funcionals i sensorials, el que ha fet interessant la seua aplicació a l'alcalinització de cacau. En els treballs que formen aquest segon capítol, es van estudiar els efectes de diverses variables de procés sobre el producte. En general, el tipus i la concentració d'àlcali van ser les variables principalment responsables de l'enfosquiment del cacau, de l'increment del pH i de la reducció de les concentracions de catequina i epicatequina. No obstant això, l'àlcali empleat no va reduir l'activitat antioxidant ni al contingut en fenols totals, propietats que es van incrementar per la pressió, la potència i la duració del tractament. Aquests increments es van relacionar amb la capacitat d'aquestes variables per alliberar els polifenols no extractables i per promoure determinades reaccions químiques. A més, també es va estudiar l'efecte de les diferents variables sobre la humitat. La potència i la duració del tractament van ser les que es van mostrar essencials per aconseguir la deshidratació del producte, arribant a produir reduccions de fins al 70%. D'altra banda, a més d'estudiar-se l'impacte de les diferents variables, també es van comparar els cacaus produïts per microones amb mostres produïdes pel mètode convencional per tal d'avaluar la seua similitud amb els cacaus comercials. Els resultats van mostrar que el microones, en només quatre minuts, va ser capaç d'enfosquir el cacau i de mantenir un perfil sensorial similar al produït pel mètode tradicional, al mateix temps que conduïa a una millora en les seues propietats funcionals. En resum, els mètodes per a l'alcalinització de cacau desenvolupats en el marc de la present tesi doctoral han demostrat ser unes alternatives molt prometedores per a substituir la tecnologia convencional. Les dos tècniques no només han estat capaces d'enfosquir el cacau tant com el mètode comercial en un temps molt menor, sinó que també han aconseguit la deshidratació parcial de la mostra i unes característiques sensorials i funcionals comparables a les del mètode convencional. / [EN] "Application of new technologies to cocoa alkalization" is a PhD thesis that aims to study the effects of two alternative techniques on the physicochemical and functional features of alkalized cocoa, and to evaluate their suitability to replace the traditional treatment. In chapter I, the conventional system for alkalization in closed and pressurized vessels has been replaced by extrusion. This technique has been proved to be a fast, continuous and less energy-consuming method, characteristics that the traditional system lacks and that have promoted its application to cocoa alkalization. On the one hand, the effects produced by temperature, water content and alkali type and concentration were evaluated on the physicochemical and functional features of cocoa. In general, alkali type and concentration were the main variables increasing the pH, darkening the sample, but also reducing the functional content, while water content and temperature exerted minor effects. On the other hand, the temperature and the water content were the variables exhibiting the greatest effect on the moisture content, leading to reductions of almost 50%. Moreover, the extrusion alkalization products were compared to traditionally produced cocoa powders based on physicochemical, functional and sensory criteria. The results revealed that extrusion was faster and able to dark cocoa in a greater extent than the conventional treatment and to produce sensory acceptable powders. These results confirm that extrusion is a feasible and promising alternative method able to alkalize cocoa in a fast, continuous and less energy-consuming manner. In chapter II, microwave heating has been studied as a substitute of the traditional alkalization treatment. This heating method has proven to be fast, versatile and able to preserve functional and sensory features of the treated products, which has made interesting its application to cocoa alkalization. The effects of the microwave heating technique on water content, power, duration, pressure application and alkali type and concentration were analyzed. In general, alkali type and concentration were the main variables inducing the darkening of cocoa, increasing its pH and reducing the concentrations of catechin and epicatechin. However, these variables did not affect the antioxidant activity and the total phenol content of the treated cocoas in comparison to the untreated one. Treatment pressure, power and duration exerted positive effects on the antioxidant activity, the total phenol content or both. These changes were related to the capacity of these variables, in combination with the alkali agent, to release non-extractable polyphenols from the matrix and to the induction of different chemical reactions. Additionally, the effects of the different variables were studied on the moisture content. Power and duration of the microwave heating treatment were decisive in the reduction of the water content, which was significantly reduced up to 70%. In terms of the evaluation of the suitability of the developed microwave heating alkalization method, the produced cocoas were compared to the traditionally alkalized ones in their physicochemical, functional and sensory characteristics. The developed fast microwave heating treatment showed to be able to dark cocoa as much as the traditional method, to produce sensory equivalent powders and to lead to the obtaining of cocoas with higher antioxidant activity and phenol content. In conclusion, this PhD thesis has applied extrusion and microwave heating as promising alternatives to cocoa alkalization. These technologies have demonstrated to dark cocoa in a significantly faster fashion than the traditional alkalization treatment, while keeping similar sensory profile and functional features, and substantially drying the product. / The authors would like to acknowledge the financial support of the Spanish Government and European Regional Development Fund (Project RTC-2016-5241- 2) / Valverde García, D. (2020). Application of new technologies to cocoa alkalization [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/140311 / Compendio