Ingeniería y Ciencia de los Materiales
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Item Investigation of the rheological behavior of polyborosiloxane with magnetically responsive particles(Pontificia Universidad Católica del Perú, 2024-02-26) Vilca Bendezu, Miguel Alberto; Grieseler, RolfDurch die Entwicklung der Soft-Robotik wird der Einsatz neuer oder neuartiger Materialien forciert, die den notwendigen Anforderungen und Ansprüchen in diesem Bereich gerecht werden. In diesem Zusammenhang kommt den sogenannten Smart Materials besondere Bedeutung zu. Diese Werkstoffe haben die einzigartige Fähigkeit, ihre Eigenschaften unter dem Einfluss physikalischer Größen zu verändern, z.B. in Abhängigkeit von der Temperatur, äußeren Magnetfeldern und elektrischen Feldern. Ein solches Smart Material, das in der Vergangenheit nur als Spielzeug verwendet wurde, ist Polyborosiloxane, welches umgangssprachlich auch als "Silly Putty" bekannt ist. Dieses besitzt aufgrund seiner nicht-newtonschen Eigenschaften vielfältige Anwendungsgebiete. Um das Verhalten von Polyborosiloxane durch ein äußeres Magnetfeld beeinflussen zu können, wurden in der vorliegenden Arbeit Verbundwerkstoffe mit einer Matrix aus Polyborosiloxane sowie Partikeln aus Carbonyleisenpulver synthetisiert und untersucht. Die genannten Komponenten wurden nach der Synthese des Polyborosiloxanes aus Polydimethylsiloxane und Borsäure von Hand gemischt, wobei der Massenanteil der dem Polymer zugesetzten Partikel von 20% bis 80% in Schritten von 20% variiert wurde. Zunächst wurden eine Reihe rheologischer Untersuchungen durchgeführt, um die entstandenen Proben hinsichtlich ihres Speicher- und Verlustmoduls zu charakterisieren und zu vergleichen. Um das Fließverhalten des Materials im Schwerefeld der Erde durch ein Magnetfeld zu beeinflussen, wurde eine Helmholtz-Spule genutzt, die sich durch ein konstantes und homogenes Magnetfeld in der Mitte der Spulen auszeichnet. Die aus den Experimenten gewonnenen Ergebnisse zeigen die Fähigkeit des Materials, eine gewünschte Form unter Einwirkung eines Magnetfelds länger beizubehalten.Item Investigation of the rheological behavior of polyborosiloxane(Pontificia Universidad Católica del Perú, 2024-02-26) Ramirez Mestanza, Dante Aaron; Grieseler, RolfPolyborosiloxano, una silicona derivada de la modificación del polidimetilsiloxano con grupos B(OH)x en sus cadenas poliméricas, exhibe propiedades únicas, como su comportamiento reológico y capacidad de autorregeneración. Estas características se explican a través de su estructura química: ante deformaciones lentas, los enlaces se rompen y regeneran secuencialmente, permitiendo el movimiento de las cadenas. No obstante, al superar un límite, estos enlaces actúan como puntos de reticulación, aumentando la rigidez del material. Aunque se ha investigado la relación entre la estructura química y las propiedades, la influencia de los métodos de síntesis y diversos estímulos aún no se ha explorado completamente. En esta investigación, se fabricaron muestras de polyborosiloxano utilizando polidimetilsiloxanos con diferentes viscosidades. Estas muestras se clasifican en tres categorías: la primera consiste en polyborosiloxanos puros, la segunda en muestras obtenidas mezclando dos precursores de viscosidades diferentes en proporciones en peso (20/80, 40/60, 60/40 y 80/20 %), y la tercera en mezclas de los polyborosiloxanos puros siguiendo las mismas proporciones que la segunda categoría. Se realizaron pruebas de barrido de amplitud y frecuencia para evaluar las propiedades reológicas de las muestras. Además, se emplearon diversas técnicas para caracterizar la estructura química y morfología, con el fin de identificar los diferentes enlaces químicos y residuos de ácido bórico no reaccionado. Con el propósito de analizar el impacto de las vibraciones, se realizó una prueba de cambio de forma a diversas frecuencias para determinar las tasas de deformación de las muestras de polyborosiloxano puro. El análisis químico y morfológico de las muestras confirma la existencia de enlaces Si-O-B en la estructura, validando la correcta síntesis del polyborosiloxano. Además, se identificaron residuos de ácido bórico no reaccionado en todas las muestras sometidas a ensayo. En relación con la caracterización reológica, se constató que las muestras pertenecientes a la segunda categoría exhibieron una distribución más homogénea en la influencia de uno de los polyborosiloxanos en sus propiedades en comparación con las de la tercera categoría. Además, en estas últimas, la adición de polyborosiloxano de menor viscosidad afectó el comportamiento reológico para valores superiores al 40%. Los gráficos de cambio de forma evidencian el impacto de los estímulos mecánicos en la capacidad de retención de forma del polyborosiloxano. En el caso de la muestra de menor viscosidad, se registraron las mayores y menores deformaciones a 0 Hz y 1 Hz, respectivamente; en contraste, para la otra muestra, dichas frecuencias fueron de 5 Hz y 1 Hz.Item Synthesis and characterization of nanostructured ternary MAX-phase thin films prepared by magnetron sputtering as precursors for twodimensional MXenes(Pontificia Universidad Católica del Perú, 2023-03-07) Miranda Marti, Marta; Grieseler, RolfMAX phase thin films can be fabricated through firstly depositing a precursor thin film consisting of the initial elements M, A, and X close to the MAX phase stoichiometry employing physical vapor deposition techniques with a subsequent thermal annealing process. This work presents different deposition configurations (multilayer and co-sputtering) for the fabrication of the Ti2AlC and Ti3AlC2 MAX phase thin films by magnetron sputtering from three elemental targets (Ti, Al, and C). It was found that the depositions followed mainly amorphous thus the MAX phase was not able to form. By implementing the deposition parameters such as temperature and substrate voltage, the deposition morphology could be tailored to crystalline and MAX phases could be created. Moreover, Ti2AlC and Ti3AlC2 nanostructured MAX phase thin films were fabricated by magnetron sputtering with three elemental targets (Ti, Al, and C) at oblique angle, resulting in a columnar thin film, and the properties of the thin film were described as a function of the column tilt angle. Lastly, the MAX phases at normal configuration and at oblique angle configuration were wet etched and the properties of the resulting MXene thin films were analyzed. It was demonstrated that only the surface of the sample was attacked by the etching solution. Thus, only the surface of the MAX phase was transformed into MXene. This hypothesis was verified by multiple characterizations such as e.g., X-Ray Diffraction and Raman spectroscopy to understand the possible morphology and chemical transformation and its influence on the etched thin film properties. The aim of this work is to unravel the connection between the morphology of the MAX phase thin films and the properties of the resulting MXenes. By understanding this relationship, it would be possible to tailor their features for specific applications.Item Durability of porous glasses(Pontificia Universidad Católica del Perú, 2022-01-10) Rodríguez Valdivieso, Christian Raúl; Grieseler, RolfThe investigations of this work are dedicated to the production of highly alkali resistant porous glasses, evaluating the effect of adding ZrO2 to the sodium borosilicate Vycortype glass. The additions were made with the purpose of improving the ability of the silica porous structure to withstand alkaline solutions. Base glasses (BG) with 0 mol% ZrO2 (Zr0), 3 mol% ZrO2 (Zr3) and 6 mol% ZrO2 (Zr6) were produced by the conventional melting and quenching method. The vitreous structure of the BG was confirmed by XRD. Further characterization tests such as density, ATR and DSC were performed as well. To induce spinodal phase separation and create a two-phase matrix (an insoluble silica rich phase and a soluble sodium-borate phase), BG were heat treated at different temperatures from 560 °C to 700 °C for 12 hours. Scanning electron microscopy (SEM) confirmed the expected interconnected sponge-like morphology. Pore sizes were calculated according to the DIN EN ISO 13383 norm. There is a well-defined tendency of pore size growth with increasing heat treatment temperature and time for 0 mol% ZrO2 and 3 mol% ZrO2 glasses. SEM images also show a decrease in pore size when ZrO2 is added to the glass. The 6 mol% ZrO2 glass did not show spinodal phase separation. Based on the pore size results, a heat treatment temperature of 680 °C was chosen for the following tests. To obtain a porous sample, the soluble sodium-borate phase needs to be leached with HCl solution. For this, leaching temperature and the HCl solution were varied, as well as the subsequent drying process.The best leaching results were obtained with a solution of 1 M HCl + 70 % Ethanol (ratio 9:1) at room temperature for two days and 2 M HCl + 70 % Ethanol (ratio 9:1) at 70 °C for seven days, for Zr0 and Zr3, respectively. To study the durability of porous glasses, alkali resistance tests against 0.1 M NaOH were carried out. It was shown that the alkali stability of Zr0 glass is very low (mass loss of about 20 % in 22 hours). However, when 3 mol% ZrO2 is added to the glass the weight loss percentage is reduced significantly (mass loss of about 4 % in 22 hours). It was found that the presence of zirconia in the silica rich porous structure improves the stability against alkali dramatically. A big problem is the leaching of the phase separated glasses, which very often resulted in breaking of the samples.Item Efficiency of cleaning solutions to remove difficult contamination on weathered float glass exposed in an urban environment(Pontificia Universidad Católica del Perú, 2021-12-03) Mendoza Carranza, Elena Kristel; Grieseler, RolfThis study investigates the removal of different contaminants on soda-lime float glass weathered artificially and naturally. Organic, inorganic non-metallic, metallic, and saline contaminants were selected to evaluate the degradation of float glass in contact with them. Bird droppings, cement dust, aluminum particles, and sodium chloride were deposited on the glass surface. The four contaminants altered the glass surface to varying degrees. Glass samples were weathered in a climate chamber for one and seven days. Another set of glass samples was exposed outdoors in Ilmenau, Germany, for 50 days (20 days unsheltered and 30 days sheltered). Before and after the weathering, the glass samples were cleaned with three cleaning agents (DI water, citric acid, and a commercial glass cleaner). The chosen cleaning solutions provided different cleaning results for the glass surfaces. Depending on weathering exposure (artificial or natural), contaminants seem to affect glass surfaces differently. During outdoor weathering, deposits adhere differently to the glass surface treated with different cleaning solutions. In addition, the effectiveness of a commercial protective agent is compared with the chosen cleaning agents. Optical microscopy was used to localize weathering products and evaluate glass surface degradation. Energy-dispersive X-ray spectroscopy (EDX) and Auger electron spectroscopy (AES) were used to identify chemically the unremoved weathering products. Surface analysis indicated the presence of chlorides and carbonates on the weathering products and more considerable delamination effects on glass naturally exposed under shelter conditions. It has been evaluated that the cleaning agents have influenced the removal of contaminants and the glass durability differently.Item Synthesis of Hydroxyapatite thin films on PMMA Printed Substrates(Pontificia Universidad Católica del Perú, 2018-01-19) Sauñi Camposano, Yesenia Haydee; Rädlein, Edda; Grieseler, RolfEach year millions of people suffer from bone defects resulting from trauma, tumors or bone-related injuries. Therefore there is a need to continuously develop new materials or improve the properties of the materials currently used, for bone replacement or implant applications. Polymethyl methacrylate (PMMA) has proven to be a promising alternative as a material for implants; however, there are still some limitations inherent to this material, particularly related to its surface properties. This thesis work is focused on the fabrication of hydroxyapatite (HAp) thin films on the surface of 3D printed PMMA substrates. 3D printing, particularly the Fused Deposition Modeling (FDM) technique was used to fabricate PMMA substrates with different surface porosity levels. FDM technique exhibits the potential for fabricating customized freeform structures for several applications including craniofacial reconstruction. HAp thin films were deposited by Radio Frequency Magnetron Sputtering (RFMS) and Ion Beam Sputtering (IBS) techniques, with a commercial target and an “in house” sintered target, respectively. A structural, chemical, mechanical, and morphological characterization was conducted in the generated surfaces by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and hardness and roughness measurements. The results of the XRD analysis revealed an amorphous structure for the films produced by both RFMS and IBS techniques on the PMMA substrates. The micrographs obtained by SEM showed a columnar morphology and a low density for the films produced by RFMS; the same technique revealed a structure of ridges of standing platelets with curved contours for the IBS deposited films. The amorphous structure and the morphology of the films, as well as the hardness and roughness can be propitious to improve surface properties and promote the osseointegration capabilities of PMMA. This work contributes to the basis for the development of a PMMA implant manufacturing process using 3D printing and HAp film deposition techniques, with improved osseointegration properties.Item Preparation and characterization of sputtered hydroxyapatite thin films(Pontificia Universidad Católica del Perú, 2018-01-19) Ugarte Díaz, Jorge Alfonso; Grieseler, Rolf; Schaaf, Peter; Rumiche Zapata, Francisco AurelioIn this work, hydroxyapatite (HAp) thin films were fabricated using two different sputtering techniques: Radio frequency magnetron sputtering and ion beam sputtering. In the first case, the films were grown on Ti-6Al-4V substrates using a high-purity commercial HAp target, obtaining a thickness ~200 nm. For the second method, the film were grown on pure titanium substrates using a self-produced HAp target. This target was fabricated with powders (Ca/P = 1.628, sintered and crushed). Here, the thickness of the fabricated film was ~300 nm. The sintering tests for the target fabrication were carried out using two different heating regimens at a maximum temperature of 1200 °C (holding time of 2h and 4h) using various additives. As additives, water (H2O), polyvinyl alcohol (PVA) and polyethylene glycol (PEG) were used to improve the mechanical strength of the green discs. The as-deposited films were amorphous in both cases. Therefore, the films were annealed to increase the crystallinity. Annealing was performed in air for 2h at temperatures: 400, 600 and 800 °C for RF-magnetron sputter samples; 600 and 800 °C for ion beam sputter samples. The result of the films shows in both cases that the crystallinity of HAp was improved only for the annealed samples fabricated with ion beam sputtering at 800 °C. In both cases energy dispersive X-ray spectroscopy measurements show a decrease in Ca/P ratio with increasing the temperature. Hardness results revealed an increase in this with the increase in temperature possibly due to the formation of titanium oxide. The roughness for the fabricated films with the RFmagnetron sputtering increases till an annealing temperature of 600 °C and then decreases till 800 °C, while the roughness for the fabricated films with ion beam sputtering is higher in the as-deposited samples and then this is reduced by increasing the annealing temperature.Item Characterization of carbon based nanostructures for the detection of tuberculosis(Pontificia Universidad Católica del Perú, 2017-11-29) Muñante Palacin, Paulo Edgardo; Grieseler, RolfTuberculosis is a leading killing disease worldwide with more than 9 million people a ected per year. Current diagnostic methods exhibit several disadvantages; one of the most promising alternatives to overcome this is the development of nanostructured diagnostic systems which are able to detect molecules associated with certain diseases. Graphene since its discovery has been the focus for the development of these sensing elements due to its excellent electronic properties. In this work, a graphene-based eld e ect transistor (FET) has been developed for tuberculosis DNA detection, in order to set the basis for a diagnostic method that overcomes current limitations. The sensing elements composed of graphene monolayers were manufactured in the stages of annealing of the substrate, addition of the linker and functionalization with the addition of a probe DNA for tuberculosis detection. Additionally, two conditions for the sensing element were generated; one with the addition of a complementary DNA sequence (\DNA Target") and the other with a mismatched DNA sequence (\Non-complementary DNA"). The graphene and the transistor, in each stage of the manufacturing process, were structural, chemical and morphologically characterized by Raman Spectroscopy, Energy Dispersive X-ray Spectroscopy (EDS), Optical Microscopy, Laser Scanning Microscopy (LSM), Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM). The results indicated an appropriate functionalization of the graphene surface with the linker, the immobilization of the probe tuberculosis DNA and the hybridization with the corresponding \DNA Target", demonstrated by observation of di erent homogeneous morphologies and an appropriate increase in the roughness in each stage of the manufacturing process. Also by the presence of characteristic peaks of nitrogenous bases and in the variation of graphene bands in the Raman spectrum. On the contrary, the sensor element with the \Non-complementary" showed an agglomeration of the molecules and segregation of salts on a heterogeneous surface. The results of the characterization are consistent with the electronic characteristics previously determined. This investigation contributes to a basis for the development of a tuberculosis detection system based on nanotechnology for clinical application.Item Anisotropy and humidity effect on tensile properties and electrical volume resistivity of fused deposition modeled acrylonitrile butadiene styrene composites(Pontificia Universidad Católica del Perú, 2017-09-06) Almenara Cueto, Carlos Ignacio; Grieseler, Rolf; Kups, ThomasEn la presente tesis, se estudió la influencia de la anisotropía y la humedad en las propiedades mecánicas a la tracción y la resistividad volumétrica de los compuestos de Acrilonitrilo Butadieno Estireno reforzado con Nano Tubos de Carbono y Acrilonitrilo Butadieno Estireno reforzado con Micro Fibras de Carbono impresos en 3D de por Deposición de Material Fundido. Para estudiar la influencia de la anisotropía, tres diferentes orientaciones de impresión de capa fueron comparadas (0°, 45° and 45°/-45°) esto para una altura de capa de 0.2 mm. Se concluyó que la influencia de la anisotropía es importante para el comportamiento mecánico de el Acrilonitrilo Butadieno Estireno con Micro Fibras de Carbono esto debido a la relación que existe entre la resistencia que realiza el refuerzo y el alineamiento que presentan las fibras respecto a la dirección de tracción. Por otro lado, no se encontraron mayor influencia de la anisotropía en las propiedades mecánicas del Acrilonitrilo Butadieno Estireno con Nano Tubos de Carbono. En la resistividad volumétrica para el Acrilonitrilo Butadieno Estireno con Nano Tubos de Carbono no se encontró mayor variación en los resultados debido a la anisotropía de las capas. El Acrilonitrilo Butadieno Estireno con Micro Fibras de Carbono no pudo ser ensayado debido a la alta resistividad que el material presentó. Para estudiar la influencia de la humedad, dos condiciones del filamento se compararon: seco y expuesto a la humedad. Se concluyó que la influencia de la humedad en el filamento es también importante en el comportamiento mecánico a la tracción del Acrilonitrilo Butadieno Estireno con Micro Fibras de Carbono esto debido a que la humedad absorbida por el filamento se elimina a través de burbujas de vapor que explosionan durante la impresión 3D empobreciendo así la adherencia entre la fibra y la matriz polimérica. Por otro lado, no se encontró tampoco mayor influencia en el comportamiento mecánico a la tracción del Acrilonitrilo Butadieno Estireno reforzado con Nano Tubos de Carbono debido a la humedad. En la resistividad volumétrica, se encontró que la humedad influye más en los resultados que la anisotropía, pero no llega a ser una influencia considerable. Esta influencia se debe principalmente a estructura menos uniforme que presenta el sólido impreso debido a las alteraciones producto de las explosiones de burbujas de vapor para eliminar la humedad absorbida como se mencionó anteriormente.