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Fiber sizings are used to improve the performance of fiber-reinforced polymer composites made from low-cost fiber and matrix materials. Evaluation of three sizings, poly(vinylpyrrolidone) (PVP), a carboxyl modified polyhydroxyether (PHE), and a standard industrial sizing (G'), have revealed tremendous improvements in static mechanical and enviro-mechanical properties. The focus of this work is to determine if these improvements in performance can be ascertained from a micromechanical test for interfacial shear strength (IFSS) on as-processed materials. The accomplishment of this goal would create more information with fewer experiments and a need for less experimental materials. In this study, a nanoindenter uniquely outfitted with a blunt tip is effectively used to obtain microindentation results where the debond load is extracted directly from the experimental load-deflection curve. Shear lag and finite element analyses are used to evaluate the mechanics of the system, but both methods show limitations with regard to determining interfacial stresses in an experimental system. In the results obtained, the PHE and Gâ materials outperform the PVP in IFSS, but the bulk properties for PVP and PHE outperform the Gâ material, suggesting the presence of another dominant mechanism. Despite better retention of bulk properties after hygrothermal exposure, PHE experiences degradation in IFSS that PVP does not. The PHE loses 10% of its original IFSS after 576 hours of 65ºC moisture exposure, while PVP improves by 25%. The tensile strengths for PHE and PVP decrease 7% and 10% respectively at 576 hours exposure. Finite element modeling shows that matrix swelling due to moisture absorption increases interfacial shear stresses, a finding supported by a comparison of wet and dry specimens subjected to equivalent aging times. Matrix swelling is not, however, responsible for the increase in IFSS of the PVP material. The relationship between tensile strength and IFSS proves to be small as predicted by a tensile strength model, but processing defects and other failure processes that are not included in the tensile strength model appear to have strong influences over the experimental results. IFSS is important in composite materials, but in the case of the G', PHE and PVP materials, other factors dominate fiber direction tensile performance. Therefore, this one simple micromechanical test provides significant insight into the composite material behavior, but it does not provide the same magnitude of information as from bulk composite experiments. / Master of Science

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Bulk Metallic Glasses (BMGs), also known as amorphous metals, are of considerable scientific and commercial interest due to their random or chaotic structure. Given their potential use as engineering materials, there is a concomitant need to establish their mechanical properties. However, BMGs are not conveniently available in sufficient volumes (especially experimental and combinatorial compositions), making property determination via conventional tensile or compression testing problematic. Instrumented indentation is ideally suited for this purpose because the testing requires only small sampling volumes and can probe multiaxial deformation characteristics at various length scales. In this technique, conducted generally on a sub-micron regime, the depth of penetration of an indenter, usually a diamond, is measured as a function of the applied load and expressed graphically as load (P) - displacement (h) curves from which a host of mechanical properties can be extracted and studied. In this work, a methodology for using instrumented indentation at nano- and micro- scales to determine the mechanical response of BMGs was developed and implemented. The implementation primarily focused on deformation in the elastic regime but included preliminary results related to the onset of inelastic deformation. The methodology developed included calibration techniques, formulations to extract the machine compliances, verifications using standards and verification for uniqueness of instrument deformation under a spherical indenter. The methodology was different for the two platforms used based on the load-depth response characteristics of the instrument. In the case of the Micro Test platform, the load-depth response of the instrument was linear. In the case of the Nano Test platform, the instrument load-depth response followed a 3/2 power law, representative of Hertzian behavior. The load-depth response of the instrument was determined by subtracting the theoretical response from the corresponding raw load-depth response obtained by elastically indenting a standard steel specimen of known modulus. The true response of the sample was then obtained by subtracting the instrument's response from the corresponding uncorrected load-depth response (raw data). An analytical model to describe the load-train compliance was developed. The methodology was verified using quartz and tungsten standards. Indentation experiments were conducted on Zr41.25Ti13.75Cu12.5Ni10Be22.5 (Vitreloy 1), Cu60Hf25Ti15, Cu60Zr30Ti10 and Fe60Co7Zr10Mo5W2B16 bulk metallic glasses using spherical indenters with diameters 2.8 mm and 100 [micro]m. The spherical geometry results in a simpler stress distribution under the indenter (when compared to a sharp geometry) and furthermore by recourse to spherical indenters the onset of plastic deformation was delayed. In the case of the Zr-based BMG, the experiments showed that the elastic response did not depend on the diameter of the indenter used indicative of the absence of residual stresses in the sample. Large scale plastic deformation was observed when the sample was indented using a smaller diameter indenter. Log scale analysis (i.e., examining the results on a log load vs. log depth response to check for deviation from Hertzian behavior) showed a deviation from a 3/2 fit indicating a deviation from elastic behavior. The onset implied a yield strength value of ~ 4 GPa, higher than the value reported in the literature (~ 2 GPa). Hence, it is believed that the first signs of plastic deformation occurred at lower loads than the predicted loads from the log scale analysis procedure and is expected to occur as discrete bursts. Discrete plastic events or "pop-ins" were observed in the load-depth indentation responses under quasistatic loading conditions, which were believed to be associated with shear band activity. An attempt was made to formulate a mathematical model based on three yield criteria (Drucker-Prager, Mohr-Coulomb and von Mises). Based on the von Mises predictions and comparable experiments on a quartz standard, it was established that the pop-ins observed were real and not an instrument artifact. Multiple load cycles following partial unload experiments showed that the pop-ins affected the subsequent indentation response. The moduli and the yield strength values obtained for the Cu-based BMGs were comparable to the values reported in the literature. There was significant scatter in the indentation data from the Fe-based BMG. Porosity and lack of 100 % compaction were believed to be the reasons for scatter in the data. The financial support of NSF through grant DMR 0314212 is gratefully acknowledged.

In the human genome, the SOST gene codes for a protein sclerostin. Sclerostin is an osteocyte-expressed negative regulator of bone formation. When the SOST gene is not coded, bone formation is reduced in individuals during skeletal maturation. This study utilizes nanoindentation methods to test for the mechanical properties of bones that both express and do not express the SOST gene. 100 transgenic murine femurs were obtained from Lawrence Livermore Labs in the form of 6 and 8 month SOST transgenic mice, 6 and 12 month SOST knockout mice, and wild type control littermates for each of the 4 age groups. Prior to nanoindentation the bones were broken in a previous experiment under three-point bending tests. Samples were embedded in epoxy and polished to a 0.05 micron level before indentation. Results showed significant difference amongst the treatment group effects for maximum load, hardness and elastic modulus. SOST KO mice had significantly higher values for these properties in comparison to the transgenic and wild type littermates. Additionally, side by side limb differences were examined in which there was a significant difference found amongst the treatment groups. Indentations were conducted in the 4 anatomical regions of each femur in expectation of examining any differences amongst them which resulted with no significant findings amongst them. Data from this study will support research which may result in potential new gene therapies targeted for the treatment of bone diseases such as osteoporosis.

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