This work is focused on the design, fabrication and characterization of high performance MEMS-based micro gas chromatography columns having wide range of applications in the pharmaceutical industry, environmental monitoring, petroleum distillation, clinical chemistry, and food processing. The first part of this work describes different approaches to achieve high-performance microfabricated silicon-glass separation columns for micro gas chromatographic (µgC) systems. The capillary width effect on the separation performance has been studied by characterization of 250 µm-, 125 µm-, 50 µm-, and 25 µm-wide single-capillary columns (SCCs) fabricated on a 10à 8 mm2 die. The plate number of 12500/m has been achieved by 25 µm-wide columns coated by a thin layer of polydimethylsiloxane stationary phase using static coating technique. To address the low sample capacity of these narrow columns, this work presents the first generation of MEMS-based "multicapillary" columns (MCCs) consisting of a bundle of narrow-width rectangular capillaries working in parallel. The second contribution of this work is the first MEMS-based stationary phase coating technique called monolayer protected gold (MPG) for ultra-narrow single capillary (SCC) and multicapillary (MCC) microfabricated gas chromatography (μGC) columns yielding the highest separation performance reported to date. This new μGC stationary phase has been achieved by electrodepositing a uniform functionalized gold layer with an adjustable thickness (250nm-2µm) in 25μm-wide single columns as well as in four-capillary MCCs. The separation performance, stability, reproducibility and bleeding of the stationary phase have been evaluated over time by separating n-alkanes as non-polar and alcohols as polar gas mixtures. / Master of Science

Yes / The fluidized bed coating system is a conventional process of particles coating in various industries. In this work, an experimental investigation was conducted using Response Surface Methodology (RSM) to optimize the coating mass of particles in a top-spray fluidized bed coating. The design of experiments (DOEs) is a useful tool for controlling and optimization of products in industry. Thus, DOE was conducted using MINITAB software, version 16. This process used a sodium silicate solution for coating the sodium percarbonate particles. The effect of the fluidization air flow rate, atomization air flow rate and liquid flow rate on the coating mass in the top-spray fluidized bed coating was investigated. The experimental results indicated that the coating mass of particles is directly proportional to the liquid flow rate of the coating solution and inversely proportional to the air flow rate. It was demonstrated that the flow rate of the coating solution had the greatest influence on the coating efficiency. / Metallic Material Processing Research Group, ACECR, Branch of Tehran University, Tehran, Iran.

Yes / The deactivation of the oxidative desulfurization (ODS) catalysts is a challenge and is a major concern in industrial catalytic processes. In this work, an activated carbon (AC) was prepared from agricultural waste and modified to withstand the ODS activity loss over time. The AC was impregnated with manganese and coated with aluminum oxide to prolong the activity lifetime. The catalysts were characterized by nitrogen adsorption-desorption, scanning electron microscope, energy dispersive X-ray, X-ray diffraction (XRD), thermogravimetric analysis (TGA), and transition electron microscope (TEM). The BET surface areas of the examined AC materials were 814.48 m2/g, 784.76 m2/g, and 755.03 m2/g for the AC, Mn/AC, and coated Mn/AC catalysts, respectively with a dominance of microporous pore size. The TGA showed that the coating layer retards the degradation of the active metal and suppresses phase transitions. XRD showed no change in the structure of the catalyst with a coating layer, and from the TEM analysis, the coating layer thickness was 3.6 nm. The kinetics of the ODS catalysts were investigated. It was shown that the ODS reaction follows the first-order kinetics and is not influenced by the coating layer. The activity decay was also investigated. It is found that the activation energy of the deactivation reaction over the coated catalyst was higher than the uncoated catalyst.

As a type of steel with notable resistance to thermal fatigue, cracking, and abrasion, AISI H13, is known for its machining ease, high hardness, and consistent heat treatment response. These qualities make AISI H13 a preferred choice for fabricating dies, moulds, and tools exposed to high temperatures, rendering it popular in metalworking. Enhanced cooling technology in die and casting moulds necessitates intricate geometries achievable through additive manufacturing (AM). To further advance part complexity and surface finish in inaccessible regions, the industry is increasingly adopting additive-subtractive hybrid manufacturing (ASHM), showing promising growth. There are, however, some concerns associated with this process, especially with the subtraction part, which is done through machining. These include the low machinability of the workpiece due to the higher hardness of additively manufactured parts compared to conventional methods. These issues are more pronounced in ASHM processes because liquid coolants or lubricants cannot be easily used, nor can the parts be heat-treated before machining. As a first step in this study, we performed a comprehensive literature review on solid lubricants used in machining so far. Their effectiveness, mechanisms, challenges, and recent developments were discussed in detail. The main purpose of this study was to introduce and investigate the effectiveness of our novel metallic solid lubricant coating for machining of AISI H13 additive manufactured parts in ASHM processes. Since the goal of this study was to mimic the ASHM process, the lubricant coating was used in dry machining, without the application of any liquid lubricant or coolant. Moreover, the workpiece was not heat treated and the tests were performed on an as-built additively manufactured AISI H13 part. A detailed study was performed to assess the impact of these lubricant coatings on AISI H13 surface integrity. The findings showed that the soft metallic lubricant coating considerably reduced the machining force and improved the surface roughness subsurface properties of the part. This method proved to be an effective solution for avoiding lubricants in ASHM processes, while significantly improving the machinability of AISI H13 parts in ASHM processes. / Thesis / Master of Applied Science (MASc) / AISI H13 tool steel is extensively utilized in tooling applications due to its exceptional wear resistance, toughness, and capability to maintain hardness at high temperatures, making it an asset for industrial uses, particularly in die and tooling manufacturing. One significant application is in the fabrication of conformal cooling channels, where additive manufacturing (AM) is the preferred method for creating intricate geometries. With the introduction of additive subtractive hybrid manufacturing (ASHM), there's an opportunity to enhance both the surface finish and the complexity of designs. However, ASHM introduces specific challenges, notably in machining. This study aims to tackle these challenges by focusing on a dry machining process for AISI H13, omitting the use of coolant and investigating the impact on surface integrity. By integrating a novel class of solid lubricant coating, the research seeks to bypass traditional methods, aiming for an improvement in machining outcomes. The results indicate that this new class of lubricant coating could significantly enhance the machining process, providing an exceptional alternative to conventional approaches and contributing to the advancement of manufacturing technologies.

No description available.

Yes / With the technological advances in the field of building materials, there has been an increasing focus on the research of lightweight concrete made with coated aggregates for improving the durability of concrete. In this study, pumice aggregates were coated with cast-based polyester to obtain polymer-coated pumice aggregates (PCPA). Lightweight concretes were produced with different cement dosages (200, 250 and 300) and PCPAs at different ratios (0%, 50% and 100%). Physical properties, mechanical strength, thermal properties and internal structure analysis (SEM-EDS) of the produced concrete samples were performed. According to the RILEM functional classification of lightweight concrete, the test results showed that REF D300 and REF D250 dosage series are in the semi-load-bearing lightweight concrete class, and the other all series are in the insulation concrete class, and the produced concretes can be classified as lightweight insulation materials. It can also be used in non-load-bearing walls or as an alternative lightweight insulation material. / The first author wish to thank the support of Scientific and Technical Research Council (TUBITAK) BIDEB-2219 Postdoctoral Research (Project Number: 1059B192100644) and the second author also thank to the Düzce University.

Tesis por compendio / [ES] En esta Tesis, se han analizado diferentes estrategias para adaptar las formulaciones de almidón con el fin de obtener recubrimientos útiles en la conservación poscosecha de frutas. El almidón se sustituyó parcialmente por gomas de origen microbiano (xantano, gelano y pululano) para mejorar las propiedades funcionales de las películas. La adición de gelano a la matriz de almidón, redujo su capacidad de adsorción de agua y la permeabilidad al vapor de agua y oxígeno. Tuvo un efecto positivo en las propiedades mecánicas, mejorando su resistencia a la rotura y previniendo la retrogradación. La goma xantana aumentó la resistencia a la rotura de las películas de almidón, pero no redujo su capacidad de adsorción de agua y la permeabilidad al vapor de agua. La sustitución del almidón por un 10 o 20% de gelano, podría ser una buena estrategia para obtener películas con propiedades más adecuadas con fines de envasado/recubrimiento de alimentos. Se analizaron películas mezcla de almidón-gelano con aceite esencial de tomillo (EO), con el objetivo de proporcionar actividad antifúngica a las formulaciones. El aceite se incorporó mediante emulsificación directa o encapsulado en liposomas de lecitina. Las películas mostraron un efecto antifúngico en las pruebas in vitro contra A. alternata y B. cinerea. La encapsulación del EO promovió una mayor retención del aceite, mejorando su actividad antifúngica, siendo éstas más efectivas contra B. cinerea que contra A. alternata. Una mayor proporción de almidón en el film dio lugar a mayor crecimiento fúngico a baja concentración del compuesto activo. Todas las películas exhibieron alta capacidad de barrera al oxígeno. La lecitina mejoró la capacidad de barrera al vapor de agua y redujo la rigidez, la resistencia a la rotura y la extensibilidad. Las películas con EO encapsulado, con una proporción de almidón-gelano de 8:2, fueron las más efectivas para controlar el crecimiento fúngico. Para aplicar las formulaciones de almidón-gelano como recubrimientos, se analizaron las propiedades superficiales de distintas frutas (manzana, tomate y caqui), y el coeficiente extensibilidad de las formulaciones sobre la superficie de la frutas, en función de la concentración de Tween 85. Las pieles de las frutas evaluadas se comportaron como superficies de baja energía. La adición de Tween 85 a las muestras sin EO, tuvo un efecto positivo en el ángulo de contacto y la tensión superficial. Sin embargo, cuando contenían EO, emulsionado o encapsulado en lecitina, el surfactante ejerció un efecto negativo en estas propiedades, dependiendo de su concentración. Las formulaciones con EO, emulsionado o encapsulado, no requirieron surfactante para mejorar su extensibilidad, mientras que la adición de Tween 85 a una concentración de 5x104 mg/L, mejoró notablemente esta propiedad en formulaciones S:G sin EO. Recubrimientos a base de almidón-gelano, con o sin EO emulsionado o encapsulado en liposomas de lecitina, fueron aplicados en manzanas y caquis. Los recubrimientos no redujeron la pérdida de peso en las manzanas, pero evitaron la pérdida de agua en los caquis. No se observó un efecto significativo de los recubrimientos en las tasas de respiración y el cociente de respiración de los caquis, mientras que estos parámetros aumentaron en manzanas. En los ensayos in vivo, los recubrimientos sin lecitina redujeron la incidencia y severidad de la mancha negra por A. alternata en caquis, y la severidad del moho gris por B. cinerea en manzanas. A pesar de su acción antifúngica in vitro, el EO no ejerció un efecto antifúngico adicional en la fruta. Esto podría explicarse por las interacciones particulares entre los componentes del recubrimiento, la superficie de la fruta y el patógeno. Los recubrimientos a base de almidón-gelano sin lecitina ni EO podrían aplicarse en caquis para controlar la pérdida de peso y reducir la incidencia de A. alternata. / [CA] En esta Tesi, s'han analitzat diferents estratègies per a adaptar les formulacions de midó a fi d'obtenir recobriments útils per a la conservació postcollita de fruites. El midó es va substituir parcialment per gomes d'origen microbià (xantano, gelano i pululano) per a millorar les propietats funcionals de les pel¿lícules. L'addició de gelano a les pel¿lícules de midó, va reduir la seua capacitat d'adsorció d'aigua. També va tindre un efecte positiu en les propietats mecàniques, i va millorar la seua resistència a la ruptura i va prevenir els fenòmens de retrogradació. La goma de xantano també va augmentar la resistència a la ruptura de les pel¿lícules de midó, però no va reduir la seua capacitat d'adsorció d'aigua i la permeabilitat al vapor d'aigua. La substitució del midó per un 10 o 20% de gelano, podria ser una bona estratègia per a obtenir pel¿lícules amb propietats més adequades per al envasat/recobriment d'aliments. S'analitzaren les pel¿lícules mescla de midó-gelano amb oli essencial de timó (EO), amb l'objectiu de proporcionar activitat antifúngica a les formulacions. L'oli es va incorporar mitjançant emulsificació directa o encapsulat en liposomes de lecitina. Estes pel¿lícules van mostrar un efecte antifúngic en les proves in vitro contra A. alternata i B. cinerea. L'encapsulació de l'EO en els liposomes de lecitina va promoure una major retenció de l'oli i va millorar la seua activitat antifúngica, sent estes més efectives contra B. cinerea que contra A. alternata. En les formulacions amb una major proporció de midó amb baix contingut en compost actiu va haver un major creixement fúngic. Totes les pel¿lícules van exhibir alta capacitat de barrera a l'oxigen. La presència de lecitina va millorar la capacitat de barrera al vapor d'aigua i va reduir la rigidesa, la resistència a la ruptura i l'extensibilitat. Les pel¿lícules amb EO encapsulat, amb una proporció de midó-gelano 8: 2, van ser les més efectives per a controlar el creixement fúngic. Amb l'objectiu d'aplicar les formulacions de midó-gelano com a recobriments, es van analitzar les propietats superficials de distintes fruites (poma, tomaca i caqui), i el coeficient d'extensibilitat d'estes formulacions sobre la superfície de la fruita, en funció de la concentració de Tween 85. Les pells de les fruites avaluades es van comportar com a superfícies de baixa energia. L'addició de Tween 85 a les formulacions sense EO, va tenir un efecte positiu en els angles de contacte i la tensió superficial. En presència de l'EO, emulsionat o encapsulat en liposomes de lecitina, el tensioactiu va exercir un efecte negatiu en estos valors, depenent de la seua concentració. Els recobriments amb EO, emulsionat o encapsulat, no van requerir tensioactiu per a millorar la seua extensibilitat, mentre que l'addició de Tween 85 a una concentració de 5x104 mg/L, va millorar notablement esta propietat en les formulacions sense EO. Recobriments a base de midó-gelano, amb o sense l'agregat d'EO emulsionat o encapsulat en liposomes, van ser aplicats en pomes i caquis.. Els recobriments no van reduir la pèrdua de pes en les pomes, però van evitar la pèrdua d'aigua en els caquis. No es va observar un efecte significatiu dels recobriments en les taxes de respiració i el quocient de respiració dels caquis, mentre que les taxes i el quocient de respiració van augmentar en les pomes. En els assajos in vivo, els recobriments sense lecitina van reduir la incidència i severitat de la taca negra per A. alternata en els caquis, i la severitat de la floridura grisa per B. cinerea en les pomes. No obstant això, la incorporació de l'EO no va exercir un efecte antifúngic addicional en la fruita. Açò podria explicar-se per les interaccions particulars entre els components del recobriment, la superfície de la fruita i el patogen. Els recobriments a base de midó-gelano sense lecitina o EO de timó podrien aplicar-se en caqui / [EN] In this Thesis, different strategies have been analysed to tailor starch formulations for the purposes of obtaining useful coatings in postharvest fruit preservation. Starch was partially substituted by microbial gums (xanthan, gellan, and pullulan) in order to improve film functional properties. Moisture sorption capacity and water vapour and oxygen permeability were reduced by the presence of gellan gum in the starch films. It also had a positive effect on the tensile properties, enhancing the films' strength and resistance to break and preventing retrogradation phenomena. Xanthan gum increased the tensile strength of the starch films, but did not reduce their water sorption capacity and water vapour permeability. Functional properties were not notably improved by the addition of pullulan. Then, 10 and 20 % starch could be substituted by gellan gum to obtain films with more adequate properties for food packaging/coating purposes. Starch-gellan blend films containing thyme essential oil (EO) were also studied in order to provide antifungal activity to the formulations. This was incorporated either by direct emulsification or encapsulated in lecithin liposomes. These films exhibited antifungal effect in in vitro tests against A. alternata and B. cinerea. The encapsulation of the EO in lecithin liposomes allowed for greater EO retention in the films, enhancing their antifungal activity, which were more effective against B. cinerea than against A. alternata. The antifungal action was slightly affected by the polymer matrix composition. Thus, the greatest starch ratio enhanced the fungal growth when the content of the active compound was low. All the films exhibited high oxygen barrier capacity. The presence of lecithin enhanced their water vapour barrier capacity and reduced the film stiffness, resistance to break and extensibility. The films with lecithin-encapsulated EO, with a starch-gellan ratio of 8:2, were the most effective at controlling fungal growth. In order to apply these starch-gellan formulations as fruit coatings, the surface properties of apple, tomato and persimmon, and the spreadability coefficient of these liquid formulations on the fruit surface, were analysed as a function of the concentration of Tween 85, as surfactant. The fruit skins behaved as low-energy surfaces. The values of the contact angles and surface tension of EO-free formulations were positively influenced by the addition of Tween 85. However, in the presence of emulsified or lecithin-encapsulated thyme EO, the surfactant exerted a negative effect, depending on its concentration. Coating-forming systems containing emulsified or encapsulated EO did not require surfactant to improve their already good spreadability, while Tween 85 at 5x104 mg/L notably improved this property in EO-free formulations. Starch-gellan coatings, containing or not emulsified or lecithin-encapsulated EO, were applied on apples and persimmons. Coatings did not reduce the weight loss in apples, but they prevented water loss in persimmons. In contrast, no significant effect of the coatings was observed on respiration rates and respiration quotient of persimmons, whereas they increased the respiration rates and quotient in apples. Coatings did not affect the changes in fruit firmness either in apples or persimmons. In the in vivo assays, the coatings without lecithin reduced the incidence and severity of black spot caused by A. alternata in persimmons, and the severity of grey mould caused by B. cinerea in apples. The incorporation of EO did not exert an additional antifungal effect on the fruit and seemed to exert a negative effect on some other fruit quality attributes. This could be explained by the particular interactions of the coating components, fruit surface and pathogen. Starch-gellan coatings without lecithin or thyme EO could be used in persimmons to control weight loss and reduce the incidence of infections caused by A. alternata. / This work has been founded by the “Ministerio de Economía y Competitividad” of Spain, through the Project AGL2016-76699-R and the “Conselleria de Educación, Investigación, Cultura y Deporte de la Generalitat Valenciana” trough the Santiago Grisolía grant GRISOLIA/2015/001. / Sapper, MI. (2019). Starch based coatings with thyme essential oil for fruit preservation [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/124342 / Compendio

Direct measurements of surface temperatures produced during fretting contact are an unknown area in the discipline of tribology; in addition, the possible effects of such temperatures on the behavior of protective anti-fretting coatings (e.g., polymeric) have never been investigated. An oscillating contact device was designed and built to study fretting contact behavior in tribological processes. The contact geometry consisted of a stationary spherical test specimen loaded against a vibrating sapphire disk driven by an electromagnetic shaker. Surface temperatures generated by frictional heating were measured during fretting contact using an infrared microscope. A photo/video technique was developed to view the fretting contact interface during an experiment and to measure the size and distribution of real area(s) of contact. The effects of size and distribution of the areas on the experimental surface temperatures for polymer-coated steel spheres-on- sapphire were investigated. Archard's theoretical model was also modified to account for multiple contact areas, and the calculated surface temperatures were compared to the experimental results. Polymeric coatings - including polystyrene (PS), polymethylmethacrylate (PMMA), polysulfone (PSO), polyvinylchloride (PVC), and polyvinylidenechloride (PVDC) were studied at a given load (20 N), frequency (150 Hz), amplitude (100 JLm), and film thickness (55 p.m). The surface temperatures generated were generally low and below the glass transition temperatures of the rigid polymers studied. The magnitude of the surface temperatures was found to be particularly dependent on the size and distribution of real area(s) of contact. The most extensive studies were performed using polystyrene coatings. Effects of load, frequency, amplitude, and film thickness on surface temperature rise and the size and distributions of real area of contact were examined. In addition, uncoated steel specimens were studied under various loads and fretting amplitudes. The observed formation of iron oxide at low surface temperature (60°C) tribologica1 experiments was explained in terms of exoelectron emission. There were considerable differences observed in the behavior of polymeric coatings under various fretting conditions. The fretting behavior of the coatings was explained in terms of mechanical and thermo-elastic effects. Thermo-elastic predictions of size distributions of real contact areas (patches) showed good agreement with the observed photo/video studies. A mechanism was proposed for tribological behavior and fretting protection of polystyrene coatings. / Ph. D.

A superhydrophobic coating can be produced using a hydrophobic material textured with surface roughness on the micro-/nano-scale. Such a coating on the outside of a submersible body may result in reduced skin-friction drag due to a trapped layer of air in the coating. However, this layer may become unstable when subjected to elevated hydrostatic pressures, and a coating’s performance is compromised beyond a certain threshold (critical pressure). This thesis presents a numerical model for predicting the pressure tolerances of superhydrophobic coatings comprised of randomly deposited hydrophobic particles or fibers. We have also derived a set of force-balance-based analytical equations for predicting critical pressure in surfaces with ordered roughness, and compared our numerical model against it, observing reasonable agreement. The numerical model was then applied in a large parameter study, predicting critical pressure for coatings with a given set of microstructure properties.

"Catalytic growth of Carbon Nanotubes (CNT) provides important advantages of controlling their diameters and possibly chirality. Our work involved growing CNT on model and supported catalyst by catalytic decomposition of carbon source such as benzene, methane and propylene. On supported catalyst, iron nitrate was deposited on alumina and reduced to form metallic iron clusters. These were reacted at 700 - 950 C under varying benzene concentrations. Multi Walled CNT (MWNT) grew below 800 C and Single Wall CNT (SWNT) are observed at 850 C and above as confirmed by TEM and Raman. Model catalysts were studied by producing CNT from ferrocene which acted as the carbon and catalyst source on Silica/Si (100). Large yield of MWNT was observed at 900 C. MWNT grew perpendicular to the model support as seen by SEM. In another model catalyst study, iron salt clusters were deposited on silica/Si (100) by spin coating, controlling their diameters by solution concentration and speed of spinning. Agglomeration of clusters at high temperatures produces only MWNT on silica/Si (100). Cluster agglomeration can be reduced with strong support metal interaction such as with alumina. We deposited alumina on silica/Si (100) by atomic layer deposition, with conformal coatings on surface and low relative roughness. Alumina film was stable under reaction temperatures of 900 C. Cluster deposition on alumina by spin coating was difficult because of different surface acidity compared to silica. Clusters on alumina did not agglomerate at high reaction temperatures. We report effect of parameters such as the temperature of reaction, conditions of pretreatment such as reduction and oxidation of catalyst precursor, type of precursor, type of carbon source, and type of support material on growth of CNT. The role of spin coating in controlling the diameter of salt clusters deposited is discussed. We also report deposition of alumina on top of silica/Si (100) by atomic layer deposition and the effect of deposition and calcination temperatures on the alumina film integrity."