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Metal fatigue is a recurring problem for metallurgists and materials engineers, especially in structural applications. It has been responsible for many disastrous accidents and tragedies in history. Understanding the micro-mechanisms during cyclic deformation and combating fatigue failure has remained a grand challenge. Environmental effects, like temperature or a corrosive medium, further worsen and complicate the problem. Ultimate design against fatigue must come from a materials perspective with a fundamental understanding of the interaction of microstructural features with dislocations, under the influence of stress, temperature, and other factors. This research endeavors to contribute to the current understanding of the fatigue failure mechanisms. Cast aluminum alloys are susceptible to fatigue failure due to the presence of defects in the microstructure like casting porosities, non-metallic inclusions, non-uniform distribution of secondary phases, etc. Friction stir processing (FSP), an emerging solid state processing technique, is an effective tool to refine and homogenize the cast microstructure of an alloy. In this work, the effect of FSP on the microstructure of an A356 cast aluminum alloy, and the resulting effect on its tensile and fatigue behavior have been studied. The main focus is on crack initiation and propagation mechanisms, and how stage I and stage II cracks interact with the different microstructural features. Three unique microstructural conditions have been tested for fatigue performance at room temperature, 150 °C and 200 °C. Detailed fractography has been performed using optical microscopy, scanning electron microscopy (SEM) and electron back scattered diffraction (EBSD). These tools have also been utilized to characterize microstructural aspects like grain size, eutectic silicon particle size and distribution. Cyclic deformation at low temperatures is very sensitive to the microstructural distribution in this alloy. The findings from the room temperature fatigue tests highlight the important role played by persistent slip bands (PSBs) in fatigue crack initiation. At room temperature, cracks initiate along PSBs in the absence of other defects/stress risers, and grow transgranularly. Their propagation is retarded when they encounter grain boundaries. Another major finding is the complete transition of the mode of fatigue cracking from transgranular to intergranular, at 200 °C. This occurs when PSBs form in adjacent grains and impinge on grain boundaries, raising the stress concentration at these locations. This initiates cracks along the grain boundaries. At these temperatures, cyclic deformation is no longer microstructure- dependent. Grain boundaries don’t impede the progress of cracks, instead aid in their propagation. This work has extended the current understanding of fatigue cracking mechanisms in A356 Al alloys to elevated temperatures.

Pt-aluminide (PtAl) coatings form an integral part of thermal barrier coating (TBC) systems that are applied on Ni-based superalloy components operating in the hot sections of gas turbine engines. These coatings serve as a bond coat between the superalloy substrate and the ceramic yttrium stabilized zirconia (YSZ) coating in the TBC system and provide oxidation resistance to the superalloy component during service at high temperatures. The PtAl coatings are formed by the diffusion aluminizing process and form an integral part of the superalloy substrate. The microstructure of the PtAl coatings is heavily graded in composition as well as phase constitution. The matrix phase of the coating is constituted of the B2-NiAl phase. Pt, in the coating, is present as a separate PtAl2 phase as well as in solid solution in B2-NiAl. The oxidation resistance of the PtAl bond coat is derived from the B2-NiAl phase. At high temperatures, Al from the B2-NiAl phase forms a regenerative layer of alumina on the coating surface which, thereby, lowers the overall oxidation rate of the superalloy substrate. The presence of Pt is beneficial in improving the adherence of the alumina scale to the surface and thereby enhancing the oxidation resistance of the coating. However, despite its excellent oxidation resistance, the B2-NiAl being an intermetallic phase, renders the PtAl coating brittle and imparts it with a high brittle-to-ductile-transition-temperature (BDTT). The PtAl coating, therefore, remains prone to cracking during service. The penetration of these cracks into the substrate is known to degrade the strain tolerance of the components. Evaluation of the mechanical behavior of these coatings, therefore, becomes important from the point of views of scientific understanding as well as application of these coatings in gas turbine engine components. Studies on the mechanical behavior of coatings have been mostly carried on coated bulk superalloy specimens. However, since the coating is brittle and the superalloy substrate more ductile when compared to the coating, the results obtained from these studies may not be representative of the coating. Therefore, it is imperative that the mechanical behavior of the coating in stand-alone condition, i.e. the free-standing coating specimen without any substrate attached to it, be evaluated for ascertaining the true mechanical response of the coating. Study of stand-alone bond coats involves complex specimen preparation techniques and challenging testing procedures. Therefore, reports on the evaluation of mechanical properties of stand-alone coatings are limited in open literature. Further, no systematic effort has so far been made to examine important aspects such as the effect of temperature and strain rate on the tensile behavior of these coatings. The deformation mechanisms associated with these bond coats have also not been reported in the literature. In light of the above, the present research study aims at evaluating the tensile behavior of free-standing PtAl coatings by the micro-tensile testing technique. The micro-tensile testing method was chosen for property evaluation because of its inherent ability to generate uniform strain in the specimen while testing, which makes the results easy to interpret. Further, since the technique offers the feasibility to test the entire graded PtAl coating in-situ, the results remain representative of the coating. Using the above testing technique, the tensile behavior of the PtAl coating has been evaluated at various temperatures and strain rates. The effect of strain rate on the BDTT of the coating has been ascertained. Further, the effect of Pt content on the tensile behavior of these coatings has also been evaluated. Attempts have been made to identify the mechanisms associated with tensile deformation and fracture in these coatings. The thesis is divided into nine chapters. Chapter 1 presents a brief introduction on the operating environment in gas turbine engines and the materials that are used in the hot sections of gas turbine engines. The degradation mechanisms taking place in the superalloy in gas turbine environments and the need for application of coatings has also been highlighted. The basic architecture of a typical thermal barrier coating (TBC) system applied on gas turbine engine components has been presented. The constituents of the TBC system, i.e. the ceramic YSZ coating, MCrAlY overlay as well as diffusion aluminide bond coats and, the various techniques adopted for the deposition of these coatings have been described in brief. Chapter 2 presents an overview of the literature relevant to this study. This chapter is divided into four sub-chapters. The formation of diffusion aluminide coatings on Ni-based superalloys has been described in the first sub-chapter. Emphasis has been laid on pack cementation process for the formation of the coatings. The fundamentals of pack aluminizing process, including the thermodynamic and kinetic aspects, have been mentioned in brief. The microstructural aspects of high activity and low activity plain aluminide and Pt-aluminide coatings have also been illustrated. The techniques applied for the mechanical testing of bond coats have been discussed in the second sub-chapter. The macro-scale testing techniques have been mentioned in brief. The small scale testing methods such as indentation, bend tests and micro-tensile testing have also been discussed in the context of evaluation of mechanical properties of bond coats. Since the matrix in the aluminide bond coats is constituted of the B2-NiAl phase, a description of the crystal structure and deformation characteristics of this phase including the flow behavior, ductility and fracture behavior has been mentioned in the third sub-chapter. In the fourth sub-chapter, reported literature on the tensile behavior and brittle-to-ductile-transition-temperature (BDTT) of diffusion aluminide bond coats has been discussed. In Chapter 3, details on experiments carried out for the formation of various coatings used in the present study and, their microstructural characterization, are provided. The method for extraction of stand-alone coating specimens and their testing is discussed. The microstructure and composition of the various coatings used in the present study are discussed in detail in Chapter 4. Unlike in case of bulk tensile testing, for which standards on the design of specimens exist, there are no standards available for the design of micro-tensile specimens. Therefore, as part of the present research work, a finite element method (FEM)-based study was carried out for ascertaining the dimensions of the specimens. The simulation studies predicted that failure of the specimens within the gage length can be ensured only when certain correlations between the dimensional parameters are satisfied. Further, the predictions from the simulation study were validated experimentally by carrying out actual testing of specimens of various dimensions. Details on the above mentioned aspects of specimen design are provided in Chapter 5. The PtAl coatings undergo brittle fracture at lower temperatures while ductile fracture occurs at higher temperatures. Further, the coatings exhibit a scatter in the yielding behavior at temperatures in the vicinity of BDTT. Therefore, the BDTT, determined as the temperature at which yielding is first observed in the stress-strain curves, may not be representative of the PtAl coatings. In Chapter 6, a method for the precise determination of BDTT of aluminide bond coats, based on the variation in the plastic strain to fracture with temperature, has been demonstrated. The BDTT determined by the above method correlated well with the variation in fracture surface features of the coating and was found representative of these coatings. In Chapter 7, the effect of temperature and strain rate on the tensile properties of a PtAl bond coat has been evaluated. The temperature and strain rate was varied between room temperature (RT)-1100°C and 10-5 s-1-10-1 s-1, respectively. The effect of strain rate on the BDTT of the PtAl bond coat has been examined. Further, the variation in fracture surface features and mechanism of fracture with temperature and strain rate are illustrated. The micro-mechanisms of deformation and fracture in the coating at different temperature regimes have also been discussed. The coating exhibited brittle-to-ductile transition with increase in temperature at all strain rates. The BDTT was strain rate sensitive and increased significantly at higher strain rates. Above BDTT, YS and UTS of the coating decreased and its ductility increased with increase in the test temperature at all strain rates. Brittle behavior occurring in the coating at temperatures below the BDTT has been attributed to the lack of operative slip systems in the B2-NiAl phase of the coating. The onset of ductility in the coating in the vicinity of BDTT has been ascribed to generation of additional slip systems caused by climb of dislocations onto high index planes. The coating exhibited two distinct mechanisms for plastic deformation as the temperature was increased from BDTT to 1100°C. For temperatures in the range BDTT to about 100°C above it, deformation was controlled by dislocations overcoming the Peierls-Nabarro barrier. Above this temperature range, non-conservative motion of jogs by jog dragging mechanism controlled the deformation. The transition temperature for change of deformation mechanism also increased with increase in strain rate. For all strain rates, fracture in the coating at test temperatures below the BDTT, occurred by initiation of cracks in the intermediate single phase B2-NiAl layer of the coating and subsequent inside-out propagation of the cracks across the coating thickness. Ductile fracture in the coating above the BDTT was associated with micro-void formation throughout the coating. The effect of Pt content on the tensile behavior of PtAl coating, evaluated at various temperatures ranging from room temperature (RT) to 1100°C and at a nominal strain rate of 10-3 s-1, is presented in Chapter 8. Irrespective of Pt content in the coating, the variation in tensile behavior of the coating with temperature remained similar. At temperatures below BDTT, the coatings exhibited linear stress-strain response (brittle behavior) while yielding (ductile behavior) was observed at temperatures above BDTT. At any given temperature, the elastic modulus decreased while the strength increased with increase in Pt content in the coating. On the other hand, the ductility of the coating remained unaffected with Pt content. The BDTT of the coating also increased with increase in Pt content in the coating. Addition of Pt did not affect the fracture mechanism in the coating. Fracture at temperatures below BDTT was caused by nucleation of cracks at the intermediate layer and their subsequent inside-out propagation. At high temperatures, fracture occurred in a ductile manner comprising void formation, void linkage and subsequent joining with cracks. The deformation sub-structure of the coating did not get affected with Pt incorporation. Short straight dislocations were observed at temperatures below BDTT, while, curved dislocations marked by jog formation were observed at temperatures above BDTT. The factors controlling fracture stress and strength in the PtAl coatings at various temperatures have also been assessed. The overall summary of the present research study and recommendations for future studies are presented in the last chapter, i.e. Chapter 9.

Die 3D-Drucktechnologie bietet eine Möglichkeit zur digitalen Funktionalisierung textiler Substrate. Jedoch hemmen fehlende Grundlagen, die geringe Materialpalette für textile Anwendungen, hohe Investitionskosten und lange Druckzeiten den Einsatz in der Textilindustrie. Die Arbeit befasst sich mit verschiedenen Einflüssen auf die Haftfestigkeit von 3D-Druck-Textil-Verbunden. Zudem werden die Effekte der 3D-Druckschichten auf die Eigenschaften der Textilien ermittelt. Dafür werden vier Gewebe und zwei Gestricke durch drei Druckmodule mit drei thermoplastischen Filamenten, einem thermoplastischen Granulat sowie einem Silikonkautschuk bedruckt. Die Einflüsse der Faktoren Textilart, Faserstoff, Textilausrichtung, Textildicke und -oberfläche sowie die Druckmodule mit den verarbeitbaren Druckmaterialien werden experimentell untersucht. Die größten signifikanten Effekte auf die Haftfestigkeit hat die Materialwahl, wobei der Effekt des Druckmaterials größer ist als der Einfluss des Textils. Die Druckschichten beeinflussen die textilen Eigenschaften unterschiedlich stark. Die thermoplastischen Materialien erhöhen die breitenbezogene Biegesteifigkeit der Textilien je nach Druckmaterial und Schichtdicke. Das Zugverhalten der Substrate wird durch die Druckschichten bis auf einzelne Ausnahmen kaum beeinflusst. Die Abriebbeständigkeit der Textilien kann durch 3D-gedruckte Strukturen soweit erhöht werden, dass sie Scheuerversuchen mit erhöhten Anforderungen gegenüber Sandpapier standhalten. Insgesamt ergänzt die Arbeit den Forschungsstand um Erkenntnisse zum 3D-Druck auf Textilien mithilfe unterschiedlicher Druckmodule. Zur verwendbaren Materialpalette gehören auch in anderen Veredlungsprozessen verwendete Materialien. Beispiele und Druckmuster veranschaulichen Anwendungspotenziale in den Bereichen der Sport-, Arbeits- und technischen Textilien.:Abkürzungen und Symbole Abbildungsverzeichnis Tabellenverzeichnis 1 Einleitung 2 Theoretische Grundlagen 2.1 Begriffe und Verfahren in der additiven Fertigung 2.1.1 Polymerisation/Stereolithographie 2.1.2 Sintern und Schmelzen 2.1.3 Extrusionsverfahren/Schmelzschichtung 2.2 Forschungsstand der additiven Fertigungsverfahren in der Textilindustrie 2.2.1 Textil- bzw. Bekleidungsherstellung 2.2.2 Textilmodifikation 2.2.3 Zusammenfassung zum Forschungsstand 2.3 Überblick zur Haftfestigkeit 2.4 Zielstellung 3 Maschinentechnik, Materialien und Methoden 3.1 Versuchsanlage am STFI 3.1.1 Filamentextruder 3.1.2 Nadelventil 3.1.3 Dispensersystem 3.2 Materialien 3.2.1 Textile Substrate 3.2.2 Druckmaterialien 3.3 Versuchsplanung und -durchführung 3.3.1 Datenvorbereitung und Druckparameter 3.3.2 Versuchsplanung 3.3.3 Prüfverfahren 3.4 Methoden der statistischen Auswertung 4 Untersuchung zur Haftfestigkeit 4.1 Einzeleffekte des Drucksubstrats 4.2 Einzeleffekte des Druckmaterials 4.3 Zusammenfassung der Erkenntnisse zu den Einzeleffekten auf die Haftfestigkeit 4.4 Interaktion der Parameter unterschieden nach Wahl des Textils 4.5 Interaktion der Parameter unterschieden nach verwendetem Druckmodul 4.6 Zusammenfassung der Erkenntnisse zur Haftfestigkeit 5 Charakterisierung der hergestellten Verbunde 5.1 Qualitative Beurteilung der Grenzflächen durch mikroskopische Aufnahmen 5.2 Dickenabweichung von der Sollschichtdicke 5.2.1 Abweichung von der Solldicke der reinen Druckschichten 5.2.2 Abweichung von der Sollschichtdicke der bedruckten Textilien 5.2.3 Zusammenfassung der Erkenntnisse zur Dickenabweichung von der Sollschichtdicke 6 Einfluss der applizierten 3D-Druckschichten auf die textilen Eigenschaften 6.1 Einfluss auf die Biegesteifigkeit 6.1.1 Biegesteifigkeiten der Ausgangsmaterialien 6.1.2 Biegesteifigkeiten der bedruckten Textilien 6.1.3 Einfluss der Biegerichtung auf die Biegesteifigkeiten 6.1.4 Zusammenfassung der Erkenntnisse zur Biegesteifigkeit 6.2 Einfluss auf das Zugverhalten 6.2.1 Zugverhalten der Ausgangsmaterialien 6.2.2 Zugverhalten der bedruckten Textilien 6.2.3 Zusammenfassung der Erkenntnisse zum Zugverhalten 6.3 Einfluss auf das Abriebverhalten 6.3.1 Abriebverhalten der Ausgangsmaterialien 6.3.2 Abriebverhalten der bedruckten Textilien 6.3.3 Einfluss der verwendeten Druckgeometrie auf das Abriebverhalten 6.3.4 Zusammenfassung der Erkenntnisse zum Abriebverhalten 6.4 Waschbeständigkeit der bedruckten Textilien 7 Bewertung der erzielten Ergebnisse 7.1 Bewertung und Vergleich der Ergebnisse mit dem Forschungsstand 7.2 Anwendungsmöglichkeiten des 3D-Drucks auf textilen Substraten 8 Zusammenfassung und Ausblick 9 Literaturverzeichnis 10 Anhang 10.1 Anhang zum Kapitel Methoden der statistischen Auswertung 10.2 Anhang zum Kapitel Haftfestigkeit 10.3 Anhang zum Kapitel Mikroskopie 10.4 Anhang zum Kapitel Dickenabweichung 10.5 Anhang zum Kapitel Biegesteifigkeit 10.6 Anhang zum Kapitel Zugverhalten 10.7 Anhang zum Kapitel Abriebverhalten / 3D printing technology offers an opportunity for digital functionalization of textile substrates. But lack of fundamentals, the small range of materials for textile applications, high investment costs and long printing times inhibit its use in the textile industry. This thesis addresses various influences on the adhesion strength of 3D printed textile composites. In addition, the effects of the 3D printed layers on the properties of the textiles are determined. For this purpose, four woven and two knitted fabrics are printed by three printing modules with three thermoplastic filaments, one thermoplastic granulate and one silicone rubber. The influences of the factors textile type, fiber material, textile orientation, textile thickness and surface as well as the printing modules with the processable printing materials are investigated experimentally. The greatest significant effects on adhesion are due to the choice of material, with the effect of the printing material being greater than the influence of the textile. The printing layers affect the textile properties to different degrees. The thermoplastic materials increase the width-related bending stiffness of the textiles depending on the printing material and layer thickness. With a few exceptions, the tensile behavior of the substrates is hardly affected by the printing layers. The abrasion resistance of the textiles can be increased by 3D-printed structures to such an extent that they can withstand abrasion tests with increased requirements compared to sandpaper. All in all, the work adds to the state of research knowledge on 3D printing on textiles using different printing modules. The range of materials that can be printed also includes materials used in other finishing processes. Examples and printed samples illustrate potential applications in the fields of sports, work and technical textiles.:Abkürzungen und Symbole Abbildungsverzeichnis Tabellenverzeichnis 1 Einleitung 2 Theoretische Grundlagen 2.1 Begriffe und Verfahren in der additiven Fertigung 2.1.1 Polymerisation/Stereolithographie 2.1.2 Sintern und Schmelzen 2.1.3 Extrusionsverfahren/Schmelzschichtung 2.2 Forschungsstand der additiven Fertigungsverfahren in der Textilindustrie 2.2.1 Textil- bzw. Bekleidungsherstellung 2.2.2 Textilmodifikation 2.2.3 Zusammenfassung zum Forschungsstand 2.3 Überblick zur Haftfestigkeit 2.4 Zielstellung 3 Maschinentechnik, Materialien und Methoden 3.1 Versuchsanlage am STFI 3.1.1 Filamentextruder 3.1.2 Nadelventil 3.1.3 Dispensersystem 3.2 Materialien 3.2.1 Textile Substrate 3.2.2 Druckmaterialien 3.3 Versuchsplanung und -durchführung 3.3.1 Datenvorbereitung und Druckparameter 3.3.2 Versuchsplanung 3.3.3 Prüfverfahren 3.4 Methoden der statistischen Auswertung 4 Untersuchung zur Haftfestigkeit 4.1 Einzeleffekte des Drucksubstrats 4.2 Einzeleffekte des Druckmaterials 4.3 Zusammenfassung der Erkenntnisse zu den Einzeleffekten auf die Haftfestigkeit 4.4 Interaktion der Parameter unterschieden nach Wahl des Textils 4.5 Interaktion der Parameter unterschieden nach verwendetem Druckmodul 4.6 Zusammenfassung der Erkenntnisse zur Haftfestigkeit 5 Charakterisierung der hergestellten Verbunde 5.1 Qualitative Beurteilung der Grenzflächen durch mikroskopische Aufnahmen 5.2 Dickenabweichung von der Sollschichtdicke 5.2.1 Abweichung von der Solldicke der reinen Druckschichten 5.2.2 Abweichung von der Sollschichtdicke der bedruckten Textilien 5.2.3 Zusammenfassung der Erkenntnisse zur Dickenabweichung von der Sollschichtdicke 6 Einfluss der applizierten 3D-Druckschichten auf die textilen Eigenschaften 6.1 Einfluss auf die Biegesteifigkeit 6.1.1 Biegesteifigkeiten der Ausgangsmaterialien 6.1.2 Biegesteifigkeiten der bedruckten Textilien 6.1.3 Einfluss der Biegerichtung auf die Biegesteifigkeiten 6.1.4 Zusammenfassung der Erkenntnisse zur Biegesteifigkeit 6.2 Einfluss auf das Zugverhalten 6.2.1 Zugverhalten der Ausgangsmaterialien 6.2.2 Zugverhalten der bedruckten Textilien 6.2.3 Zusammenfassung der Erkenntnisse zum Zugverhalten 6.3 Einfluss auf das Abriebverhalten 6.3.1 Abriebverhalten der Ausgangsmaterialien 6.3.2 Abriebverhalten der bedruckten Textilien 6.3.3 Einfluss der verwendeten Druckgeometrie auf das Abriebverhalten 6.3.4 Zusammenfassung der Erkenntnisse zum Abriebverhalten 6.4 Waschbeständigkeit der bedruckten Textilien 7 Bewertung der erzielten Ergebnisse 7.1 Bewertung und Vergleich der Ergebnisse mit dem Forschungsstand 7.2 Anwendungsmöglichkeiten des 3D-Drucks auf textilen Substraten 8 Zusammenfassung und Ausblick 9 Literaturverzeichnis 10 Anhang 10.1 Anhang zum Kapitel Methoden der statistischen Auswertung 10.2 Anhang zum Kapitel Haftfestigkeit 10.3 Anhang zum Kapitel Mikroskopie 10.4 Anhang zum Kapitel Dickenabweichung 10.5 Anhang zum Kapitel Biegesteifigkeit 10.6 Anhang zum Kapitel Zugverhalten 10.7 Anhang zum Kapitel Abriebverhalten