abstract: Materials have been the backbone of every major invention in the history of mankind, e.g. satellites and space shuttles would not exist without advancement in materials development. Integral to this, is the development of nanocrystalline (NC) materials that promise multitude of properties for advanced applications. However, they do not tend to preserve structural integrity under intense cyclic loading or long-term temperature exposures. Therefore, it is imperative to understand factors that alter the sub-features controlling both structural and functional properties under extreme conditions, particularly fatigue and creep. Thus, this dissertation systematically studies the tensile creep and fatigue behaviour of a chemically optimized and microstructurally stable bulk NC copper (Cu)-3at.% tantalum (Ta) alloy. Strategic engineering of nanometer sized clusters of Ta into the alloy’s microstructure were found to suppress the microstructure instability and render remarkable improvement in the high temperature tensile creep resistance up to 0.64 times the melting temperature of Cu. Primary creep in this alloy was found to be governed by the relaxation of the microstructure under the applied stress. Further, during the secondary creep, short circuit diffusion of grain boundary atoms resulted in the negligible steady-state creep rate in the alloy. Under fatigue loading, the alloy showed higher resistance for crack nucleation owing to the inherent microstructural stability, and the interaction of the dislocations with the Ta nanoclusters. The underlying mechanism was found to be related to the diffused damage accumulation, i.e., during cyclic loading many grains participate in the plasticity process (nucleation of discrete grain boundary dislocations) resulting in homogenous accumulation rather than localized one as typically observed in coarse-grained materials. Overall, the engineered Ta nanoclusters were responsible for governing the underlying anomalous high temperature creep and fatigue deformation mechanisms in the alloy. Finally, this study presents a design approach that involves alloying of pure metals in order to impart stability in NC materials and significantly enhance their structural properties, especially those at higher temperatures. Moreover, this design approach can be easily translated to other multicomponent systems for developing advanced high-performance structural materials. / Dissertation/Thesis / Doctoral Dissertation Materials Science and Engineering 2019

The objective of the research presented in this thesis was to develop a concrete bridge deck topping mixture that resists the effects of differential shrinkage by decreasing shrinkage and increasing creep. . In addition, the amount of tensile creep that concrete experiences under long-term tensile stresses were quantified and compared to compressive creep values in order to gain a better understanding of how concrete behaves under tension. Test results show that the amount of tensile creep exceeded compressive creep by a factor of 2-5. Various shrinkage and creep models were compared against test data in order to quantify results and determine the best model to use for the mixes examined during this research project. Data analysis revealed that the AASHTO time dependent effects (shrinkage and creep) models outperformed the other models used in this research project. Other material property data including compressive strength, splitting tensile strength, Young's modulus of elasticity, and unrestrained shrinkage was also collected to compare against a common bridge deck topping mix to ensure that the mixes used in this research project are suitable for use in the field. A parametric study utilizing the Age Adjusted Effective Modulus (AAEM) method was performed which showed that the most important factor in reducing tensile stresses was to decrease the amount of shrinkage experienced by the concrete bridge deck topping mixture. Three concrete mixtures, one included saturated lightweight aggregates (SLWA), one including ground granulated blast furnace slag (GGBFS), and one incorporating both were tested. Preliminary results show that the inclusions of SLWA into a concrete mixture reduced shrinkage by 25% and overall tensile stress by 38%. / Master of Science

Thesis (MScEng)--Stellenbosch University, 2012. / ENGLISH ABSTRACT: Research in concrete has advanced to such an extent that it is now possible to add steel fibres to concrete in order to improve its durability and ductility. This led to a research group in Europe, FIB, who has provided guidelines to designing Steel Fibre Reinforced Concrete (SFRC) structures. They have found that it is possible for SFRC beams in flexure to be in static equilibrium. However, the time-dependent behaviour of SFRC has not been researched fully and it requires further investigation. When looking at a concrete beam in flexure there are two main stress zones, the compression zone and the tension zone, of which the tensile zone will be of great interest. This study will report on the investigation of the tensile time-dependent behaviour of SFRC in order to determine how it differs from conventional concrete. The concrete has been designed specifically to exhibit strain-softening behaviour so that the material properties of SFRC could be investigated fully. Factors such as shrinkage and tensile creep of SFRC were of the greatest importance and an experimental test setup was designed in order to test the tensile creep of concrete in a simple and effective manner. Comparisons were be made between the tensile creep behaviour of conventional concrete and SFRC where emphasis was placed on the difference between SFRC specimens before and after cracking occurred in order to determine the influence of steel fibre pull-out. The addition of steel fibres significantly reduced the shrinkage and tensile creep of concrete when un-cracked. It was however found that the displacement of fibre pull-out completely overshadowed the tensile creep displacements of SFRC. It was necessary to investigate what effect this would have on the deflection of SFRC beams in flexure once cracked. Viscoelastic behaviour using Maxwell chains were used to model the behaviour of the tensile creep as found during the tests and the parameters of these models were used for further analyses. Finite Element Analyses were done on SFRC beams in flexure in order simulate creep behaviour of up to 30 years in order to determine the difference in deflections at mid-span between un-cracked and pre-cracked beams. The analyses done showed that the deflections of the pre-cracked SFRC beams surpassed the requirements of the Serviceability Limit States, which should be taken into account when designing SFRC beams. / AFRIKAANSE OPSOMMING: Die navorsing in beton het gevorder tot so ‘n mate dat dit nou al moontlik is om staal vesels by die beton te voeg sodat dit beton se duursaamheid en duktiliteit te verbeter. Dit het gelei tot ‘n groep in Europa, FIB, wat dit moontlik gemaak het om Staal Vesel Beton (SVB) strukture te ontwerp. Hulle het gevind dat dit moontlik is vir SVB balke om in statiese ewewig te wees tydens buiging. Die tyd afhanklike gedrag van SVB is egter nog nie deeglik ondersoek nie en benodig dus verdure ondersoek. Wanneer ‘n balk in buiging aanskou word kan twee hoof spanningzones identifiseer word, ‘n druk zone en ‘n trek zone, waarvan die trek zone van die grootste belang is. Hierdie studie gaan verslag lewer oor die ondersoek van tyd-afhanklike trekgedrag van SVB om te bepaal hoe dit verskil van konvensionele beton. Die beton was spesifiek ontwerp om vervormingsversagtende gedrag te wat maak dat die materiaal eienskappe van SVB ten volle ondersoek kan word. Faktore soos krimp en die trekkruip van SVB was van die grootste belang en ‘n eksperimentele toets opstelling was ontwerp om die trekkruip van beton op ‘n eenvoudige en effektiewe manier te toets. Daar was vergelykings getref tussen die trekkruip gedrag van konvensionele beton en SVP en groot klem was geplaas op die verskil tussen SVB monsters voor en na die monsters gekraak het om te bepaal wat die invloed was van staalvesels wat uittrek. Die byvoeging van staalvesels het beduidend die kruip en trekkruip van beton verminder. Daar was alhoewel gevind dat die verplasing van die uittrek van staalvesels heeltemal die trekkruip verplasings van SVB oorskadu het. Dit was nodig om te sien watse effek dit op die verplasing van SVB balke in buiging sal hê. Viskoelastiese gedrag deur Maxwell kettings was gebruik om die gedrag van trekkruip, soos gevind deur die toetse, te modelleer en die parameters van hierdie modelle was verder gebruik vir analises. Eindige Element Analises was gedoen op SVB balke in buiging om die trekkruip gedrag tot op 30 jaar te simuleer op die verskil tussen die defleksies by midspan tussen ongekraakte en vooraf gekraakte balke te vind. Die analises het gewys dat die defleksies van die vooraf gekraakte balke nie voldoen het aan die vereistes van die Diensbaarheid limiete nie, wat in ag geneem moet word wanneer SVB balke ontwerp word.

Cementitious materials with strain-hardening property and high tensile ductility are promising materials on account of their mechanical and durability performances. These materials require special ingredients which make it costly to be used in conventional constructions. Hence, potential applications of Engineered Cementitious Composites (ECC) generally focus on layered systems or repairs which require the use of ECC together with another material. For it to be used especially as a repair material, it should have sufficient dimensional compatibility for preventing restrained shrinkage cracking. In this thesis, a strain-hardening fiberreinforced cementitious composite, named Engineered Cementitious Composites, was produced with local ingredients and their mechanical performance, dimensional stability properties were investigated. For investigating the effect of materials and mix proportions on mechanical properties, compressive strength, flexural strength with mid-span beam deflections and matrix fracture toughness tests were conducted. For determining the dimensional compatibility properties, autogenous, drying and restrained shrinkage tests were conducted along with tensile creep tests. As a result it was shown that, mechanical and dimensional stability properties are affected by the ingredients and mix proportions. It was shown that especially autogenous shrinkage of mixtures was relatively high which can cause early age cracking. In order to mitigate the adverse effect of autogenous shrinkage, the effect of pre-soaked expanded perlite aggregate replacement on mechanical, shrinkage and dimensional compatibility properties was investigated. As a result it was found out that autogenous shrinkage can be mitigated by the use of pre-soaked expanded perlite aggregate replacement.

L'allègement des structures est devenu un enjeu majeur pour les industries du transport. Afin de répondre à cette demande, une stratégie de recherche d'élaboration de nouveaux matériaux, présentant des propriétés spécifiques égalant a minima les propriétés des matériaux en service, a été mise en place. C'est dans ce contexte général que s'inscrivent ces travaux sur la phase MAX Ti3AlC2. La tenue à l'oxydation et les propriétés en traction et en fluage traction à haute température (800-1000°C) ont été évaluées pour des échantillons élaborés au cours de cette étude par métallurgie des poudres (frittage naturel + frittage flash). Les différents essais menés en oxydation ont montré l'existence de deux comportements (oxydation passivante ou catastrophique suivant la nature des oxydes formés) majoritairement contrôlés par les caractéristiques microstructurales des échantillons (taille de grains, nature des éléments en site A, rugosité et porosité). Les premiers essais de fluage traction réalisés sur la phase MAX Ti3AlC2 ont souligné la bonne ductilité de ces matériaux. De plus, les propriétés spécifiques sont comparables, voire dépassent, celles de superalliages polycristallins et d'aluminures de titane. Une étude multi-échelle a mis en évidence une déformation se produisant par glissement aux joints de grains à 900 et 1000°C et par mouvement de dislocations à 800°C. Un endommagement de type cavitation accompagné par des phénomènes d'oxydation de fissures en surface des fûts a été mis en lumière. / The lightening of structures has become a major challenge for transport industries. New materials with, at least, equivalent specific properties to currently used materials have been designed in order to cope with this challenge. In this regard, Ti3AlC2 MAX phase has been studied. The high temperature (800-1000°C) oxidation resistance and tension and tensile creep properties were assessed for Ti3AlC2 samples elaborated using a powder metallurgy process (pressureless sintering + spark plasma sintering). The various oxidation tests pointed out two different behaviors (protective oxidation or catastrophic one depending on the grown oxides nature) mainly controlled by samples microstructural features (grains size, elements on A site, roughness and porosity). The first tensile creep tests ever performed on Ti3AlC2 MAX phase indicates the high ductility of these materials whose specific properties reach or surpass those of polycrystalline superalloys and titanium aluminides. A multi-scale study highlights deformation mechanisms occurring through intergranular sliding at 900 and 1000°C and through dislocations glide at 800°C. Damage mechanisms occurring through cavitation supported by crack oxidation phenomena on gauge length surface were also underlined.

In this experimental investigation, the tensile creep behavior of commercial-purity molybdenum sheet at temperatures between 1300°C and 1700°C is critically evaluated, based upon experimental creep testing and microstructural characterizations. The high-temperature properties of molybdenum are of interest because there are many applications in which molybdenum and molybdenum alloys are used at elevated temperatures. Understanding of the creep mechanisms and the constitutive relations between stress and strain at elevated temperatures is needed in order to determine if molybdenum is an appropriate choice for a given high-temperature design application and to accurately predict its creep life. The creep behavior of two commercially-available grades of molybdenum was determined using short-term creep tests (1/2 to 14 hours) at slow to moderate true-strain rates of 10⁻⁶ to 10⁻⁴ s⁻¹ and temperatures between 1300°C and 1700°C. High-temperature, uniaxial tensile testing was used to produce data defining the relationship between tensile creep strain-rate and steady-state flow stress at four temperatures: 1340°C, 1440°C, 1540°C, 1640°C. Microstructural changes that occurred during creep testing were evaluated and compared to changes resulting from elevated temperature exposure alone. Mechanisms for dynamic abnormal grain growth that occurred during creep testing and the causes of the microstructural changes that occurred as a function of temperature are discussed. / text