Silicon nitride thin films are of interest in the biomedical engineering field due to their biocompatibility and favorable tribological properties. Evaluation and understanding of the properties of these films under diverse loading and failure conditions is a necessary prerequisite to their use in biomedical devices. Three wafers of silicon nitride-coated silicon were obtained from Lawrence Livermore National Laboratory and used to create 96 samples. Samples were subjected to nanoindentation testing to evaluate the mechanical properties of the film. Samples were subjected to nanoimpact testing to compare the damage resistance of the film to separate nanoimpact types. Samples were subjected to nanoscratch testing to evaluate the consistency of the critical load of the film. Results showed that there were no significant differences in the mechanical properties of the film across the tested groups. There was a significant difference observed in the rate of damage to the film between pendulum oscillation nanoimpact testing and sample oscillation nanoimpact testing, with the former causing more damage with all experiment variables controlled for. Results showed that the critical load measure for the film was significantly different between different nanoscratch test parameters. The conclusions from this study will support future work for in vitro and in vivo testing of ceramic thin films for biomedical applications.

The doctoral thesis deals with the study of morphology and mechanical properties of thin plasma polymer films based on tetravinylsilane monomer and its mixtures with oxygen and argon. Thin films were prepared by plasma-enhanced chemical vapour deposition on silicon and glass substrates. Atomic force microscopy was used for characterization of thin film surface and for depiction of composite interphase with functional interlayer. Mechanical properties of thin films, namely Young’s modulus and hardness, were studied by cyclic nanoindentation technique. Nanoindentation device was also used to carry out scratch test, which was helpful to describe adhesion of films to substrate. In this thesis the influence of deposition conditions on surface and mechanical properties of thin films prepared in continual and pulse wave on planar substrates is discussed. Also, the suitability of few atomic force microscopy techniques for depiction of composite interphase was reviewed.

Kenaf fiber is increasingly getting the attention of the industries due to its excellent mechanical properties, feasibility, growth rate, and ease of cultivation. On the other hand, cellulose nanofibril is one of the important building blocks of all the bast fibers which significantly contributes to their mechanical properties. However, most of the studies in the literature have estimated the value of axial elastic modulus for fiber-bundles which has some unavoidable issues resulting in incorrect modulus. Moreover, the transverse elastic modulus is another important parameter that also needs to be studied. Hence, to compensate for the gap in the literature, a single unit of both kenaf microfiber and cellulose nanofibril have been subjected to nanomechanical characterization to analyze their surface morphology and determine their elastic modulus in the axial and transverse direction. The experiments also pave to a protocol to characterize micro and nanofibrils nanomechanically and determine their elastic moduli.

京都大学 / 0048 / 新制・課程博士 / 博士(エネルギー科学) / 甲第20484号 / エネ博第353号 / 新制||エネ||70(附属図書館) / 京都大学大学院エネルギー科学研究科エネルギー変換科学専攻 / (主査)教授 木村 晃彦, 教授 星出 敏彦, 教授 今谷 勝次 / 学位規則第4条第1項該当 / Doctor of Energy Science / Kyoto University / DFAM

Near equi-atomic nickel titanium (NiTi) shape memory alloys (SMAs) are a class of materials characterized by their unique deformation behavior. In these alloys, deformation mechanisms such as mechanical twinning and stress induced phase transformation between a high symmetry phase (austenite) and a low symmetry phase (martensite) additionally occur and influence mechanical behavior and thus their functionality. Consequently, applications of SMAs usually call for precise phase transformation temperatures, which depend on the thermomechanical history and the composition of the alloy. Instrumented indentation, inherently a mechanical characterization technique for small sampling volumes, offers a cost effective means of empirically testing SMAs in the form of centimeter scaled buttons prior to large-scale production. Additionally, it is an effective probe for intricate SMA geometries (e.g., in medical stents, valves etc.), not immediately amenable to conventional mechanical testing. The objective of this work was to study the deformation behavior of NiTi SMAs using instrumented indentation. This involved devising compliance calibration techniques to account for instrument deformation and designing spherical diamond indenters. Substantial quantitative information related to the deformation behavior of the shape memory and superelastic NiTi was obtained for the first time, as opposed to existing qualitative indentation studies. For the case of shape memory NiTi, the elastic modulus of the B19' martensite prior to twinning was determined using spherical indentation to be about 101 GPa, which was comparable to the value from neutron diffraction and was substantially higher than typical values reported from extensometry (68 GPa in this case). Twinning at low stresses was observed from neutron diffraction measurements and was attributed to reducing the elastic modulus estimated by extensometry. The onset of predominantly elastic deformation of the twinned martensite was identified from the nanoindentation response and the elastic modulus of the twinned martensite was estimated to be about 17 GPa. Finite element modeling was used to validate the measurements. For the case of the superelastic NiTi, the elastic modulus of the parent austenite was estimated to be about 62 GPa. The onset of large-scale stress induced martensite transformation and its subsequent elastic deformation were identified from the nanoindentation response. The effect of cycling on the mechanical behavior of the NiTi specimen was studied by repeatedly indenting at the same location. An increase in the elastic modulus value for the austenite and a decrease in the associated hysteresis and residual depth after the initial few cycles followed by stabilization were observed. As for the case of shape memory NiTi, finite element modeling was used to validate the measurements. This work has initiated a methodology for the quantitative evaluation of shape memory and superelastic NiTi alloys with instrumented spherical indentation. The aforementioned results have immediate implications for optimizing thermomechanical processing parameters in prototype button melts and for the mechanical characterization of intricate SMA geometries (e.g., in medical stents, valves etc.) This work was made possible by grants from NASA (NAG3-2751) and NSF (CAREER DMR-0239512) to UCF.

No description available.

<p>Silicon-based dielectric thin films including amorphous hydrogenated aluminium-doped silicon oxides (<em>a-</em>SiAl_xO_y:H), amorphous hydrogenated silicon nitrides (<em>a-</em>SiN_x:H), and amorphous hydrogenated silicon carbides (<em>a-</em>SiC_x:H) were deposited by remote plasma chemical vapour deposition (RPECVD) techniques including electron cyclotron resonance plasma enhanced chemical vapour deposition (ECR-PECVD) and inductively-coupled-plasma chemical vapour deposition (ICP-CVD) on silicon (Si) wafers, soda-lime glass microscope slides, and glassy carbon (C) plates. Aluminium (Al) in the SiAlO films was incorporated by way of a metalorganic Al(TMHD)₃ precursor.</p> <p>Thickness, refractive index, and growth rate of the films were measured using variable angle spectroscopic ellipsometry (VASE). Film composition was measured using energy dispersive X-ray spectroscopy (EDX) for the SiAlO films and Rutherford backscattering spectrometry (RBS) for the SiC_x films. Elastic modulus and hardness of the SiAlO and SiC_x films were measured using nanoindentation and their adhesion was characterized via progressive load scratch testing.</p> <p>All films were observed to be optically transparent at near-IR and red wavelengths with many SiN_x and SiC_x films exhibiting significant optical absorption above 2.25eV. Modification of a previously developed deposition recipe produced doubled growth rates in SiN_x and SiC_xfilms. SiAlO films were produced with up to 1.6±0.1at% aluninium (Al) incorporation, while SiC_x films with composition ranging from SiC_0.25:H to SiC₂:H could be produced depending on the growth gas flow ratios. SiAlO films exhibited hardness and reduced modulus (<em>H</em> and <em>E</em>) up to 8.2±0.4 and 75±2GPa, respectively; <em>H </em>and <em>E</em> for the SiC_xfilmsreached 11.9±0.2 and 87±3 GPa. Initially, adhesion to Si wafers was extremely poor with films delaminating at loads of 1.5±0.3N when scratched with a 3/16” alumina (Al₂O₃) sphere; implementation of a rigorous pre-deposition surface cleaning procedure produced films showing only cracking and no delamination up to 30N loads vs. a 200μm radius Rockwell C diamond stylus.</p> / Master of Applied Science (MASc)

Arterial mechanical properties have received increasing attention in the past few decades due to their vast effect on predicting cardiovascular diseases and injuries. The heterogeneity of thoracic aortic tissue was characterized in terms of viscoelastic material properties and correlations were obtained between these properties and tissue morphology. Additionally, the effect of material preservation on the material properties was determined. Changes in the mechanical properties of porcine thoracic aorta wall in the radial direction were characterized using a quasi-linear viscoelastic modeling of nanoindentaiton tests. Two layers of equal thickness were mechanically distinguishable in descending aorta based on the radial variations in the instantaneous Young's modulus E and reduced relaxation function G(t). Overall, comparison of E and Ginf of the outer half (70.27±2.47 kPa and 0.35±0.01) versus the inner half (60.32±1.65 kPa and 0.33±0.01) revealed that the outer half was stiffer and showed less relaxation. The results were used to explain local mechanisms of deformation, force transmission, tear propagation and failure in arteries. A multimodal and multidisciplinary approach was adopted to characterize the transmural morphological properties of aorta. The utilized methods included histology and multi-photon microscopy for describing the wall micro-architecture in the circumferential-radial plane, and Fourier-Transform infrared imaging spectroscopy for determining structural protein, and total protein content. The distributions of these quantified properties across the wall thickness of the porcine descending thoracic aorta were characterized and their relationship with the mechanical properties was determined. It was revealed that there is an increasing trend in mechanical stiffness, Elastic lamella Density (ELD), Structural Protein (SPR), Total Protein (TPR), and Elastin and Collagen Circumferential Percentage (ECP and CCP) from inner layers toward the outer ones. Finally two larger regions with equal thickness (inner and outer halves) were determined based on cluster analysis results of ELD which were in agreement with the cluster analysis of instantaneous Young's modulus. Changes to the local viscoelastic properties of fresh porcine thoracic aorta wall due to three common storage temperatures (+4 oC, -20 oC and -80 oC) within 24 hours, 48 hours, 1 week and 3 weeks were characterized. The changes to both elastic and relaxation behaviors were investigated considering the multilayer, heterogeneous nature of the aortic wall. For +4 oC storage samples, the average instantaneous Young's modulus (E) decreased while their permanent average relaxation amplitude (Ginf) increased and after 48 hours these changes became significant (10%, 13% for E, Ginf respectively). Generally, in freezer storage, E increased and Ginf showed no significant change. In prolonged preservation (> 1 week), the results of +20 oC storage showed significant increase in E (20% after 3 weeks) while this increase for -80 oC was not significant, making it a better choice for tissue cold storage applications. Results from this dissertation present a substantial step toward the anatomical characterization of the aortic wall building blocks and establishing a foundation for understanding the role of microstructural components on the functionality of blood vessels. A better understanding of these relationships would provide novel therapeutic targets and strategies for the prevention of human vascular disease. / Mechanical Engineering

Nanoindentation is an increasingly used tool to investigate the mechanical properties of very small volumes of material. Gold single crystals were chosen as a model system for surface modification studies, because of the electrochemical advantages and the simple structure of the material. Experiments on these samples displayed a spectrum of residual deformation, with measured hardness values on the same surface differing by over a factor of two. The yield point also exhibited considerable variation, but the depth of penetration was independent of this elastic–plastic transition. The onset of plastic deformation in these tests is observed at stress levels on the order of the theoretical yield strength. There are a limited number of defects in a single crystal specimen of gold, especially on the length scale required to influence nearly every indentation experiment. A test matrix was designed to change the concentrations of possible defects in a sample (dislocations, vacancies, and structural features), by altering some of the surface preparation parameters. The results of these experiments were extremely consistent. Observed trends within the matrix, combined with the observations of reduced hardness and earlier plasticity when compared to the preliminary testing, indicate a decline in the structural continuity of the sample. This is surprising considering the extensive material removal and thermal history of some of these surfaces. There is no indication of a cause for the dramatic inconsistencies in mechanical properties observed in preliminary testing, but a consistent surface enables the study of intentional modifications. Changes in contact area that were undetectable in preliminary results now demonstrate predictable shifts in hardness values. The deposition of a single monolayer of gold oxide raised the average load at yield by a factor of three and increased the hardness by over 26%. Attributing this change to the oxide is corroborated by the reduction of hardness when the oxide is stripped. Similar behavior is observed when a lead monolayer is deposited and tested ex-situ. It is surprising that layers <0.5 nm in thickness would have such a dramatic influence on indentation tests at least 35 nm deep. This indicates that no surface layer can be ignored at this scale. These experiments demonstrate that there is still much to be learned about nanoscale deformation mechanisms. / Ph. D.

Yes / Liquid crystal is a new emerging biomaterial. The physical property of liquid crystal plays a role in supporting the adhesion of cells. Nano and microball indentation techniques were applied to determine the elastic modulus or viscoelasticity of the cholesteryl ester liquid crystals in the culture media. Nano-indentation results (108 ± 19.78 kPa, N = 20) agreed well with the microball indentation (110 ± 19.95 kPa, N = 60) for the liquid crystal samples incubated for 24 hours at 37o C, respectively. However, nanoindentation could not measure the modulus of the liquid crystal (LC) incubated more than 24 hours. This is due to the decreased viscosity of the liquid crystal after immersion in the cell culture media for more than 24 hours. Alternatively, microball indentation was used and the elastic modulus of the LC immersed for 48 hours was found to decrease to 55 ± 9.99 kPa (N = 60). The microball indentation indicated that the LC did not creep after 40 seconds of indentation. However, the elastic modulus of the LC was no longer measurable after 72 hours of incubation due to the lost of elasticity. Microball indentation seemed to be a reliable technique in determining the elastic moduli of the cholesteryl ester liquid crystals. / Science Fund Vot. No. S024 or Project No. 02- 01-13-SF0104 and FRGS Vot. No. 1482 awarded by Malaysia Ministry of Education