Geopolymers (GPs) are a new class of inorganic polymers that have been considered as good candidate materials for many applications, including fire resistant and refractory panels, adhesives, and coatings, waste encapsulation material, etc. The aim of this study is to establish relationship between structural and mechanical properties of geopolymers with different chemical compositions. The metakaolin-based geopolymers were prepared by mechanically mixing metakaolin and alkaline silicate aqueous solutions to obtain samples with SiO2/Al2O3 molar ratio that ranges from 2.5 to 5, and Na/Al or K/Al atomic ratios equal to 1. Geopolymer samples were cured in a laboratory oven at 80°C and ambient pressure for different times in the sealed containers. Structural characterization of the samples with different chemical compositions was carried out using X-Ray Diffraction (XRD), Fourier Transform Infrared (FTIR) spectroscopy, Nuclear Magnetic-Resonance (NMR) spectroscopy and Scanning Electron Microscopy (SEM) with Energy Dispersive Spectroscopy (EDS). The mechanical characterization included Micro-indentation, Vickers indentation and fracture toughness measurement, as well as compressive testing. It was found that structure and mechanical properties of GPs depend on their chemical composition. The Na-GPs with ratio 3 have a highest compressive strength and Young‘s modulus of 39 MPa and 7.9 GPa, respectively. The results of mechanical testing are discussed in more detail in this thesis and linked to structural properties of processed geopolymers.

In this study, a simple and inexpensive membrane mechanical property measuring system was developed. By applying the force on a membrane and recording the corresponding out-of-plane displacement fields, then the Young¡¦s modules and Possion¡¦s ratio of the membrane can be obtained from those deformations through the inverse approach. Firstly, a loading frame was designed to fix the membrane and allow the membrane can be loaded and its deformations can be measured precisely. In order to measure the out-of-plane displacement fields of the loaded membrane, the digital image correlation (DIC) was used and an easier 3-D DIC measuring method was proposed in this study. The proposed 3-D DIC measuring method was verified by using a loaded cantilever beam with ESPI. The error was within in 10%. In this study, the smallest in-plane displacement that can be measured by proposed method is 2 £gm and the smallest out-of-plane displacement that that can be measured is 6£gm. In this study, in order to determine the mechanical properties of the membrane, digital image correlation, finite element method (FEM) and optimization method were combined with the measured out-of-plane displacement fields, then the Young¡¦s modules and Possion¡¦s ratio of the membrane were determined through the inverse approach. The FEM simulations were performed by using ANSYS. Several optimization theorems were adopted and their corresponding merits on this study were compared The obtained Young's modulus was compared with the results obtain from the nano-indentor and the error was within in 3% ~ 12%. Keyword: digital image correlation, membrane, Young¡¦s modules, Possion¡¦s ratio, finite element method, optimization method.

Carbon nanotubes (CNTs) have extraordinary electrical and mechanical properties, and many potential applications have been proposed, ranging from nanoscale devices to reinforcement of macroscopic structures. However, due to their small sizes, characterization of their mechanical properties and deformation behaviours are major challenges. Theoretical modelling of deformation behaviours has shown that multi-walled carbon nanotubes (MWCNTs) can develop ripples in the walls on the contracted side when bent above a critical curvature. The rippling is reversible and accompanied by a reduction in the bending stiffness of the tubes. This behaviour will have implications for future nanoelectromechanical systems (NEMS). Although rippling has been thoroughly modelled there has been a lack of experimental data thus far. In this study, force measurements have been performed on individual MWCNTs and vertically aligned carbon nanofibers (VACNFs). This was accomplished by using a custom-made atomic force microscope (AFM) inside a scanning electron microscope (SEM). The measurements were done by bending free-standing MWCNTs/VACNFs with the AFM sensor in a cantilever-to-cantilever fashion, providing force-displacement curves. From such curves and the MWCNT/VACNF dimensions, measured from SEM-images, the critical strain for the very onset of rippling and the Young’s modulus, E, could be obtained. To enable accurate estimations of the nanotube diameter, we have developed a model of the SEM-image formation, such that intrinsic diameters can be retrieved. We have found an increase in the critical strain for smaller diameter tubes, a behaviour that compares well with previous theoretical modelling. VACNFs behaved very differently, as they did not display any rippling and had low bending stiffnesses due to inter-wall shear. We believe that our findings will have implications for the design of future NEMS devices that employ MWCNTs and VACNFs. / <p>Artikel 2 Image formation mechanisms tidigare som manuskript, nu publicerad: urn:nbn:se:kau:diva-16425 (MÅ 150924)</p>

Posterior tibial tendon dysfunction (PTTD) is a common degenerative condition leading to a severe impairment of gait. There is currently no effective method to determine whether a patient with advanced PTTD would benefit from several months of bracing and physical therapy or ultimately require surgery. Tendon degeneration is closely associated with irreversible degradation of its collagen structure, leading to changes to its mechanical properties. If these properties could be monitored in vivo, it could be used to quantify the severity of tendonosis and help determine the appropriate treatment. Ultrasound elasticity imaging (UEI) is a real-time, noninvasive technique to objectively measure mechanical properties in soft tissue. It consists of acquiring a sequence of ultrasound frames and applying speckle tracking to estimate displacement and strain at each pixel. The goals of my dissertation were to 1) use acoustic simulations to investigate the performance of UEI during tendon deformation with different geometries; 2) develop and validate UEI as a potentially noninvasive technique for quantifying tendon mechanical properties in human cadaver experiments; 3) design a platform for UEI to measure mechanical properties of the PTT in vivo and determine whether there are detectable and quantifiable differences between healthy and diseased tendons. First, ultrasound simulations of tendon deformation were performed using an acoustic modeling program. The effects of different tendon geometries (cylinder and curved cylinder) on the performance of UEI were investigated. Modeling results indicated that UEI accurately estimated the strain in the cylinder geometry, but underestimated in the curved cylinder. The simulation also predicted that the out-of-the-plane motion of the PTT would cause a non-uniform strain pattern within incompressible homogeneous isotropic material. However, to average within a small region of interest determined by principal component analysis (PCA) would improve the estimation. Next, UEI was performed on five human cadaver feet mounted in a materials testing system (MTS) while the PTT was attached to a force actuator. A portable ultrasound scanner collected 2D data during loading cycles. Young's modulus was calculated from the strain, loading force and cross sectional area of the PTT. Average Young's modulus for the five tendons was (0.45±0.16GPa) using UEI. This was consistent with simultaneous measurements made by the MTS across the whole tendon (0.52±0.18GPa). We also calculated the scaling factor (0.12±0.01) between the load on the PTT and the inversion force at the forefoot, a measurable quantity in vivo. This study suggests that UEI could be a reliable in vivo technique for estimating the mechanical properties of the human PTT. Finally, we built a custom ankle inversion platform for in vivo imaging of human subjects (eight healthy volunteers and nine advanced PTTD patients). We found non-linear elastic properties of the PTTD, which could be quantified by the slope between the elastic modulus (E) and the inversion force (F). This slope (ΔE/ΔF), or Non-linear Elasticity Parameter (NEP), was significantly different for the two groups: 0.16±0.20 MPa/N for healthy tendons and 0.45±0.43 MPa/N for PTTD tendons. A receiver operating characteristic (ROC) curve revealed an area under the curve (AUC) of 0.83±0.07, which indicated that the classifier system is valid. In summary, the acoustic modeling, cadaveric studies, and in vivo experiments together demonstrated that UEI accurately quantifies tendon mechanical properties. As a valuable clinical tool, UEI also has the potential to help guide treatment decisions for advanced PTTD and other tendinopathies.

This research work presents the first comprehensive study on nanocrystalline materials produced in bulk quantities using a novel continuous electrodeposition process. A series of nanocrystalline Ni and Ni-Fe alloy continuous foils were produced and an intensive investigation into their structure and various properties was carried out. High-resolution transmission electron microscopy (HR-TEM) revealed the presence of local strain at high and low angle, and twin boundaries. The cause for these local strains was explained based on the interpretation of non-equilibrium grain boundary structures that result when conditions of compatibility are not satisfied. HR-TEM also revealed the presence of twin faults of the growth type, or &ldquo;growth faults&rdquo;, which increased in density with the addition of Fe. This observation was found to be consistent with a corresponding increase in the growth fault probabilities determined quantitatively using X-ray diffraction (XRD) pattern analysis. Hardness and Young&rsquo;s modulus were measured by nanoindentation. Hardness followed the regular Hall-Petch behaviour down to a grain size of 20 nm after which an inverse trend was observed. Young&rsquo;s modulus was slightly reduced at grain sizes less than 20 nm and found to be affected by texture. Microstrain based on XRD line broadening was measured for these materials and found to increase primarily with a decrease in grain size or an increase in intercrystal defect density (i.e., grain boundaries and triple junctions). This microstrain is associated with the local strains observed at grain boundaries in the HR-TEM image analysis. A contribution to microstrain from the presence of growth faults in the nanocrystalline Ni-Fe alloys was also noted. The macrostresses for these materials were determined from strain measurements using a two-dimensional XRD technique. At grain sizes less than 20 nm, there was a sharp increase in compressive macrostresses which was also owed to the corresponding increase in intercrystal defects or interfaces in the solid.

This research work presents the first comprehensive study on nanocrystalline materials produced in bulk quantities using a novel continuous electrodeposition process. A series of nanocrystalline Ni and Ni-Fe alloy continuous foils were produced and an intensive investigation into their structure and various properties was carried out. High-resolution transmission electron microscopy (HR-TEM) revealed the presence of local strain at high and low angle, and twin boundaries. The cause for these local strains was explained based on the interpretation of non-equilibrium grain boundary structures that result when conditions of compatibility are not satisfied. HR-TEM also revealed the presence of twin faults of the growth type, or &ldquo;growth faults&rdquo;, which increased in density with the addition of Fe. This observation was found to be consistent with a corresponding increase in the growth fault probabilities determined quantitatively using X-ray diffraction (XRD) pattern analysis. Hardness and Young&rsquo;s modulus were measured by nanoindentation. Hardness followed the regular Hall-Petch behaviour down to a grain size of 20 nm after which an inverse trend was observed. Young&rsquo;s modulus was slightly reduced at grain sizes less than 20 nm and found to be affected by texture. Microstrain based on XRD line broadening was measured for these materials and found to increase primarily with a decrease in grain size or an increase in intercrystal defect density (i.e., grain boundaries and triple junctions). This microstrain is associated with the local strains observed at grain boundaries in the HR-TEM image analysis. A contribution to microstrain from the presence of growth faults in the nanocrystalline Ni-Fe alloys was also noted. The macrostresses for these materials were determined from strain measurements using a two-dimensional XRD technique. At grain sizes less than 20 nm, there was a sharp increase in compressive macrostresses which was also owed to the corresponding increase in intercrystal defects or interfaces in the solid.

Estimating the in situ mechanical properties of sediments containing gas hydrates from seismic or log data is essential for evaluating the risks posed by mechanical failure during drilling, completions, and producing operations. In this paper, a method is presented for constructing correlations between the mechanical properties of gas hydrate bearing sediments and geophysical data. A theory based on micromechanics models was used to guide the selection of parameters that govern the physical behavior of sediments. A set of nondimensionalized relations between elastoplastic properties and those that could be inferred from log or seismic data was derived. Using these relations, a correlation for the Young’s modulus was constructed for sands with methane and THF hydrate using data from a wide variety of sources. It was observed that the correlation did not fit data obtained from samples with high THF hydrate saturations, due possibly to the existence of cohesive mechanisms that operate in such regimes.

Geopolymerization has been considered as a new technology to replace the ordinary Portland cement in construction industry. It provides an option to manage the industry waste and byproducts like fly ash, mine tailings. At the same time, the CO₂ emissions can be reduced about 80% compared to that of ordinary Portland cement. The present research includes three main parts. First part is applying mine tailings as construction materials using geopolymerization method. The study is focused on efficiently activating mine tailings, reducing alkali consumption, decreasing curing time and improving compressive strength. We investigate the activation temperature effects, the impacts of additives and effects of forming pressures. The results show that a 40 MPa unconfined compressive strength (UCS) can be achieved with the geopolymerization samples after mine tailings are activated by sodium hydroxide at 170°C for 1 hour with the addition of calcium hydroxide and alkali dissolved aluminium oxide, further compressed with a 10 MPa forming pressure and finally cured at 90°C for 3 days. To elucidate the mechanism for the contribution of additives to geopolymerization, microscopic and spectroscopic techniques including scanning electron microscopy/ energy-dispersive X-ray spectroscopy (SEM/EDX), X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy are used to investigate the micro/nanostructure and the elemental and phase composition of geopolymerization specimens. The stress-strain behavior was also characterized. The results shows that the mechanical behavior is similar with that of concrete and the dynamic modulus is 22 GPa, which is comparable with that of concrete. The Young's modulus of geopolymer product was also calculated and the value is in the range of 2.9 to 9.3 GPa. The findings of the present work provide a novel method for the geopolymerization of mine tailings as construction materials. Second section is applying fly ash as a high strength water-resistant construction material. Through the present investigation, a procedure has been studied. The experiment results indicate that the concentration of NaOH, water content, and curing condition can significantly affect the mechanical property of geopolymer matrix. At the same time, the chemical composition, especially the Si/Al ratio and calcium content, is also an important factor during geopolymerization. XRD results show that the amorphous feature can be observed for both high and low calcium fly ash. It is the key of the success of geopolymerizaton due to its high reactivity. XRD, FTIR and SEM tests were performed to study how experiment conditions and the properties of fly ash affect geopolymerization. The obtained compressive strength of the geopolymerization product can reach above 100 MPa. The stress-strain behavior was also characterized. The results shows that the dynamic modulus is 36.5 GPa. The product obtained from the present work shows very high water resistance without losing any compressive strength even after a one month soaking time. Third part is applying the mixture of class C fly ash and mine tailings as construction materials. Through the present investigation, a protocol has been set up. The experiment results of the present work also help set up the working conditions such as activation temperature and time, the concentration of NaOH, the addition of Ca(OH)₂, forming pressure, mine tailing to class C fly ash weight ratio, curing temperature and curing time. To elucidate the mechanism for the contribution of additives to geopolymerization, microscopic and spectroscopic techniques such as SEM/EDX, X-ray diffraction and FTIR spectroscopy were used to investigate the micro/nanostructure and the elemental and phase composition of geopolymerization composite. The obtained compressive strength of the geopolymerization product can reach above 60 MPa. The stress-strain behavior of the geopolymer matrix of the mixture of mine tailing and fly ash were also characterized and the results show that the mechanical behavior is similar to that of concrete with a 24 GPa dynamic modulus. The Young's modulus of geopolymer product was also calculated and the value is in the range of 4.0 to 13.5 GPa. The findings of the present work provide a novel method for the geopolymerization of the mixture of mine tailings and class C fly ash as construction materials, such as bricks for construction and road pavement.

Graphite is used within a reactor as a moderator and a reflector material. During fast neutron irradiation, the physical properties and dimensions of nuclear graphite are changed significantly. Graphite shrinkage could lead to disengagement of individual component and loss of core geometry; differential shrinkage in the graphite component could lead to the generation of internal stresses and component failure by cracking. The latter behaviour is complicated by the irradiation induced changes in Young's modulus and strength. These dimensional and modulus change have been associated with the irradiation-induced closure of many thousands of micro-cracks associated with the graphite crystallites due to crystal dimensional change. Closure of microcracks in nuclear graphite was simulated by external pressure (hydrostatic loading, deviatory stress and dynamic loading) and not by irradiation, whilst Young's modulus was measured to check if there was any correlation between the two mechanisms. A study of the deformation behaviour of polycrystalline graphite hydrostatically loaded up to 200MPa are reported. Gilsocarbon specimens (isotropic) and Pile Grade A (PGA) specimens are (anisotropic in nature) were investigated. Strain measurements were made in the axial and circumferential directions of cylindrical samples by using strain gauges. Dynamic Young's modulus was also investigated from the propagation velocity of an ultrasonic wave. Porosity measurements are made to determine the change in the porosity before and after deformation and also their contribution towards the compression and dilatation of graphite under pressure. Graphite crystal orientation during loading was also investigated by using XRD (X-ray diffraction) pole figures. Effective medium models were also investigated to describe the effect of porosity on graphite elastic modulus. All the graphite specimens investigated exhibited non-linear pressure- volumetric strain behaviour in both direction (axial and circumferencial). In most of the experiments, the deformation was closing porosity despite new porosity being generated. Under hydrostatic loading, PGA graphite initially stiff then it became less stiff after a few percent of volume strain and then after about ~20% volumetric strain they stiffen up again, whist Gilsocarbon showed similar behaviour at lower volumetric strain (~10-13%). Gilsocarbon was stiff than PGA; this behaviour is due to the fact that Gilsocarbon has higher density and lower porosity than PGA. During unloading, a large hysteresis was formed. The stressed grains are relieved; the initial closed pores began to reopen. It is suggested that during this stage, the volume of pore re-opening superseded the volume of pores closing, the graphite sample volume almost fully recovered. In the axial compression test, PGA perpendicular to the extrusion direction (PGA-AG) was less stiff than PGA parallel to the extrusion direction (PGA-WG); in the hydrostatic compaction test, the PGA-WG sample deformed more because it had to undergo a less complicated shape change. This is because the symmetry of their anisotropy is parallel to the symmetry of the sample. The Pole figures showed an evidence of slight crystal reorientation after hydrostatic loaded up to 200MPa. The effective medium model revealed the importance of porosity interaction in graphite during loading.

In the TRISO (tristructural isotropic) coated fuel particle used in the High Temperature Reactor, the most important layer is a silicon carbide layer which acts as a pressure vessel. In this study, we have focused our study on the investigation of the Young’s modulus, hardness, residual stress, and fracture toughness of the SiC layer. Moreover, microstructures and impurities in silicon carbide were characterised and then related to both Young’s modulus and hardness of the SiC layer. Both nanoindentation and micro-indentation were used to determine Young’s modulus and hardness of the SiC. Raman spectroscopy, X-ray diffraction, and scanning electron microscopy techniques were used to examine impurities, phases and microstructure of silicon carbide layers, respectively. Young’s modulus was measured at different positions of a polished surface of the SiC with different CVD growth and crystal orientations. With help from the finite element modelling, it has been found that Young’s modulus of the SiC is dependent on the grain orientation of the SiC. Mechanical properties of silicon carbide are affected by the presence of excess silicon, excess carbon, stacking faults, texture, grain size, property of grain boundary. The effect of these factors on Young’s modulus and hardness, are investigated with the orthogonal analysis. The analysis concludes that the most important factor on Young’s modulus is texture while the most significant factor on hardness is grain boundary. Grain size is secondarily important factor to affect hardness. Stacking faults and impurities almost have no influence on Young’s modulus and hardness. The residual stress in the silicon carbide layer was measured based on the peak shift in Raman spectra of the SiC and is in a range of 150-300 MPa. Fracture resistance in the radial direction of the SiC layer is larger than those in the circumferential direction. The difference is controlled by the layer-like structure of the SiC coating.