Effect of anisotropy on elastic moduli measured by nanoindentation in human tibial cortical bone

Many biological materials are known to be anisotropic. In particular, microstructural components of biological materials may grow in a preferred direction, giving rise to anisotropy in the microstructure. Nanoindentation has been shown to be an effective technique for determining the mechanical properties of microstructures as small as a few microns. However, the effects of anisotropy on the properties measured by nanoindentation have not been fully addressed. This study presents a method to account for the effects of anisotropy on elastic properties measured by nanoindentation. This method is used to correlate elastic properties determined from earlier nanoindentation experiments and from earlier ultrasonic velocity measurements in human tibial cortical bone. Also presented is a procedure to determine anisotropic elastic moduli from indentation measurements in multiple directions. © 2001 John Wiley & Sons, Inc. J Biomed Mater Res.

Investigation of the oxidative degradation mechanisms and melt stabilisation of a new generation metallocene polytehylene

The two main objectives of the research work conducted were firstly, to investigate the processing and rheological characteristics of a new generation metallocene catalysed linear low density polyethylene (m-LLDPE), in order to establish the thermal oxidative degradation mechanism, and secondly, to examine the role of selected commercial stabilisers on the melt stability of the polymers. The unstabilised m-LLDPE polymer was extruded (pass I) using a twin screw extruder, at different temperatures (210-285°C) and screw speeds (50-20rpm) and was subjected to multiple extrusions (passes, 2-5) carried out under the same processing conditions used in the first pass. A traditional Ziegler/Natta catalysed linear low density polyethylene (z-LLDPE) produced by the same manufacturer was also subjected to a similar processing regime in order to compare the processability and the oxidative degradation mechanism (s) of the new m-LLDPE with that of the more traditional z-LLDPE. The effect of some of the main extrusion characteristics of the polymers (m-LLDPE and z-LLDPE) on their melt rheological behaviour was investigated by examining their melt flow performance monitored at two fixed low shear rate values, and their rheological behaviour investigated over the entire shear rates experienced during extrusion using a twin-bore capillary rheometer. Capillary rheometric measurements, which determine the viscous and elastic properties of polymers, have shown that both polymers are shear thinning but the m-LLDPE has a higher viscosity than z-LLDPE and the extent of reduction in viscosity of the former when the extrusion temperature was increased from 210°C to 285°C was much higher than in the case of the z-LLDPE polymer. This was supplied by the findings that the m-LLDPE polymer required higher power consumption under all extrusion conditions examined. It was fUliher revealed that the m-LLDPE undergoes a higher extent of melt fracture, the onset of which occurs under much lower shear rates than the Ziegler-based polymer and this was attributed to its higher shear viscosity and narrower molecular weight distribution (MWD). Melt flow measurements and GPC have shown that after the first extrusion pass, the initial narrower MWD of m-LLDPE is retained (compared to z-LLDPE), but upon further multiple extrusion passes it undergoes much faster broadening of its MWD which shifts to higher Mw polymer fractions, paliicularly at the high screw speeds. The MWD of z-LLDPE polymer on the other hand shifts towards the lower Mw end. All the evidence suggest therefore the m-LLDPE undergoes predominantly cross-linking reactions under all processing conditions whereas z-LLDPE undergoes both cross-linking and chain scission reactions with the latter occurring predominantly under more severe processing conditions (higher temperatures and screw speeds, 285°CI200rpm). The stabilisation of both polymers with synergistic combinations of a hindered phenol (Irganox 1076) and a phosphite (Weston 399) at low concentrations has shown a high extent of melt stabilisation in both polymers (extrusion temperatures 210-285°C and screw speeds 50-200rpm). The best Irganox 1076/Weston 399 system was found to be at an optimum 1:4 w/w ratio, respectively and was found to be most effective in the z-LLDPE polymer. The melt stabilising effectiveness of a Vitamin E/Ultranox 626 system used at a fraction of the total concentration of Irganox 1076/Weston 399 system was found to be higher in both polymers (under all extrusion conditions). It was found that AOs which operate primarily as alkyl (Re) radical scavengers are the most effective in inhibiting the thermal oxidative degradation of m-LLDPE in the melt; this polymer was shown to degrade in the melt primarily via alky radicals resulting in crosslinking. Metallocene polymers stabilised with single antioxidants of Irganox HP 136 (a lactone) and Irganox E201 (vitamin E) produced the highest extent of melt stability and the least discolouration during processing (260°C/1 OOrpm). Furthermore, synergistic combinations of Irganox HP I 36/Ultranox 626 (XP-60) system produced very high levels of melt and colour stability (comparable to the Vitamin E based systems) in the mLLDPE polymer. The addition of Irganox 1076 to an Irganox HP 136/Ultranox 626 system was found not to result in increasing melt stability but gave rise to increasing discolouration of the m-LLDPE polymer. The blending of a hydroxylamine (lrgastab FS042) with a lactone and Vitamin E (in combination with a phosphite) did not increase melt stability but induced severe discolouration of resultant polymer samples.

The mechanical behaviour of cylindrical GRP panels

Glass reinforced plastic (GRP) is now an established material for the fabrication of sonar windows. Its good mechanical strength, light weight, resistance to corrosion and acoustic transparency, are all properties which fit it for this application. This thesis describes a study, undertaken at the Royal Naval Engineering College, Plymouth, into the mechanical behaviour of a circular cylindrical sonar panel. This particular type of panel would be used to cover a flank array sonar in a ship or submarine. The case considered is that of a panel with all of its edges mechanically clamped and subject to pressure loading on its convex surface. A comprehensive program of testing, to determine the orthotropic elastic properties of the laminated composite panel material is described, together with a series of pressure tests on 1:5 scale sonar panels. These pressure tests were carried out in a purpose designed test rig, using air pressure to provide simulated hydrostatic and hydrodynamic loading. Details of all instrumentation used in the experimental work are given in the thesis. The experimental results from the panel testing are compared with predictions of panel behaviour obtained from both the Galerkin solution of Flugge's cylindrical shell equations (orthotropic case), and finite element modelling of the panels using PAFEC. A variety of appropriate panel boundary conditions are considered in each case. A parametric study, intended to be of use as a preliminary design tool, and based on the above Galerkin solution, is also presented. This parametric study considers cases of boundary conditions, material properties, and panel geometry, outside of those investigated in the experimental work Final conclusions are drawn and recommendations made regarding possible improvements to the procedures for design, manufacture and fixing of sonar panels in the Royal Navy.

Examining crystallographic orientation dependence of hardness of silica stishovite

We conducted nanoindentation to explore the hardness and elastic properties of silica stishovite, synthesized at high pressure and quenched to ambient conditions. A total of 10 crystallographic orientations were examined on selected grains with a maximum load of 4 or 20 mN. We observed discontinuity in the load-displacement curve (pop-in) for the [2 5 over(1, -)] and [6 2 over(1, -)] grains subjected to a maximum load of 20 mN. The single-crystal hardness at high plastic deformation is quasi-isotropic with an average of 32 ± 1 GPa, similar to the polycrystalline hardness reported earlier; the theoretical hardness determined from the experiments is about 54 ± 3 GPa. These two hardnesses suggest that stishovite is one of the hardest oxides. The measured indentation moduli are close to the predictions at low load (minor plasticity) but are considerably lower at high load (high plasticity). Both indentation hardness and modulus decrease with increasing plasticity. Our results underscore the necessity of considering the degree of plastic deformation when interpreting hardness and elastic moduli from indentation experiments. © 2007 Elsevier B.V. All rights reserved.

Elastic and plastic properties of Mo3Si measured by nanoindentation

Single crystal Mo3Si specimens were grown and tested at room temperature using established nanoindentation techniques at various crystallographic orientations. The indentation modulus and hardness were obtained for loads that were large enough to determine bulk properties, yet small enough to avoid cracking in the specimens. From the indentation modulus results, anisotropic elastic constants were determined. As load was initially increased to approximately 1.5 mN, the hardness exhibited a sudden drop that corresponded to a jump in displacement. The resolved shear stress that was determined from initial yielding was 10-15% of the shear modulus, but 3 to 4 times the value obtained from the bulk hardness. Non-contact atomic force microscopy images in the vicinity of indents revealed features consistent with {100}(010) slip.

A decade of silicone hydrogel development:surface properties, mechanical properties, and ocular compatibility

Since the initial launch of silicone hydrogel lenses, there has been a considerable broadening in the range of available commercial material properties. The very mobile silicon–oxygen bonds convey distinctive surface and mechanical properties on silicone hydrogels, in which advantages of enhanced oxygen permeability, reduced protein deposition, and modest frictional interaction are balanced by increased lipid and elastic response. There are now some 15 silicone hydrogel material variants available to practitioners; arguably, the changes that have taken place have been strongly influenced by feedback based on clinical experience. Water content is one of the most influential properties, and the decade has seen a progressive rise from lotrafilcon-A (24%) to efrofilcon-A (74%). Moduli have decreased over the same period from 1.4 to 0.3 MPa, but not solely as a result of changes in water content. Surface properties do not correlate directly with water content, and ingenious approaches have been used to achieve desirable improvements (e.g., greater lubricity and lower contact angle hysteresis). This is demonstrated by comparing the hysteresis value of the earliest (lotrafilcon-A, >40°) and most recent (delefilcon-A, <10°) coated silicone hydrogels. Although wettability is important, it is not of itself a good predictor of ocular response because this involves a much wider range of physicochemical and biochemical factors. The interference of the lens with ocular dynamics is complex leading separately to tissue–material interactions involving anterior and posterior lens surfaces. The biochemical consequences of these interactions may hold the key to a greater understanding of ocular incompatibility and end of day discomfort.

Mechanical properties and the evolution of matrix molecules in PTFE upon irradiation with MeV alpha particles

The morphology, chemical composition, and mechanical properties in the surface region of α-irradiated polytetrafluoroethylene (PTFE) have been examined and compared to unirradiated specimens. Samples were irradiated with 5.5 MeV 4He2+ ions from a tandem accelerator to doses between 1 × 106 and 5 × 1010 Rad. Static time-of-flight secondary ion mass spectrometry (ToF-SIMS), using a 20 keV C60+ source, was employed to probe chemical changes as a function of a dose. Chemical images and high resolution spectra were collected and analyzed to reveal the effects of a particle radiation on the chemical structure. Residual gas analysis (RGA) was utilized to monitor the evolution of volatile species during vacuum irradiation of the samples. Scanning electron microscopy (SEM) was used to observe the morphological variation of samples with increasing a particle dose, and nanoindentation was engaged to determine the hardness and elastic modulus as a function of a dose. The data show that PTFE nominally retains its innate chemical structure and morphology at a doses <109 Rad. At α doses ≥109 Rad the polymer matrix experiences increased chemical degradation and morphological roughening which are accompanied by increased hardness and declining elasticity. At  α doses >1010 Rad the polymer matrix suffers severe chemical degradation and material loss. Chemical degradation is observed in ToF-SIMS by detection of ions that are indicative of fragmentation, unsaturation, and functionalization of molecules in the PTFE matrix. The mass spectra also expose the subtle trends of crosslinking within the α-irradiated polymer matrix. ToF-SIMS images support the assertion that chemical degradation is the result of a particle irradiation and show morphological roughening of the sample with increased a dose. High resolution SEM images more clearly illustrate the morphological roughening and the mass loss that accompanies high doses of a particles. RGA confirms the supposition that the outcome of chemical degradation in the PTFE matrix with continuing irradiation is evolution of volatile species resulting in morphological roughening and mass loss. Finally, we reveal and discuss relationships between chemical structure and mechanical properties such as hardness and elastic modulus.

Three-dimensional finite element analysis of the effects of anisotropy on bone mechanical properties measured by nanoindentation

A three-dimensional finite element analysis (FEA) model with elastic-plastic anisotropy was built to investigate the effects of anisotropy on nanoindentation measurements for cortical bone. The FEA model has demonstrated a capability to capture the cortical bone material response under the indentation process. By comparison with the contact area obtained from monitoring the contact profile in FEA simulations, the Oliver-Pharr method was found to underpredict or overpredict the contact area due to the effects of anisotropy. The amount of error (less than 10% for cortical bone) depended on the indentation orientation. The indentation modulus results obtained from FEA simulations at different surface orientations showed a trend similar to experimental results and were also similar to moduli calculated from a mathematical model. The Oliver-Pharr method has been shown to be useful for providing first-order approximations in the analysis of anisotropic mechanical properties of cortical bone, although the indentation modulus is influenced by anisotropy.

Tensile properties of as fabricated, aged, and stretched SiC whisker and particle reinforced 2009 aluminium alloy

Tensile tests were carried out using specimens of 2009 aluminium alloy reinforced by either SiC whiskers or particles. The size distributions of the whiskers and particles in the matrix were obtained by image analysis. It was found that failure was a result of uniform void nucleation and coalescence in the as fabricated composites, or a result of fast crack propagation initiated by a flaw developed at clusters of SiC in the aged or stretched and aged composites. The strengths of the as fabricated composites were estimated based on the results of image analysis using continuum mechanics and dislocation theories. The estimation indicated that the tensile strengths are largely contributed to by composite strengthening, supplemented by residual dislocation strengthening and work hardening. Owing to the flaw controlled failure, the tensile strengths of the aged or stretched and aged composites were independent of aging time, aging temperature, and the amount of stretching. The elastic moduli of the composites were estimated using the Halpin-Tsai model and a good correlation was found between the measured and estimated moduli. © 1996 The Institute of Materials.

Effect of thermal and mechanical processing on tensile properties of powder formed 2124 aluminium and 2124 Al-SiC p metal matrix composite

The aging responses of 2124 Al-SiC p metal matrix composite (MMC) and unreinforced matrix alloy are studied and related to variations in tensile properties. The MMC is aged from Wo starting conditions: (i) stretched and naturally aged and (ii) re-solution treated. Accelerated aging occurs in both MMC conditions compared with unreinforced alloy. Tensile strengths and elastic moduli are improved in the MMC compared with the alloy, but ductility is reduced. Stretched MMC exhibits higher strength but lower ductility and modulus than re-solutioned MMC. The re-solutioned MMC fails by microvoid coalescence in low aging conditions, and by void nucleation and shear in high aging conditions. Failure of the stretched MMC initiates at the surface at specimen shoulders, illustrating the increased notch sensitivity of this condition, and propagates via a zigzag shear fracture mode. Zigzag facet size increases on gross aging. Particle fracture occurs during tensile failure, but also before testing as a result of the manufacturing process. © 1995 The Institute of Materials.

Spin transition of 1D, 2D and 3D iron(II) complex polymers - the tug-of-war between elastic interaction and a shock-absorber effect

The structures of linear chain Fe(II) spin-crossover compounds of α,β- and α,ω-bis (tetrazol-1-yl)alkane type ligands are described in relation to their magnetic properties. The first threefold interlocked 3-D catenane Fe(II) spin-transition system, [μ-tris(1,4-bis(tetrazol-1-yl)butane-N1,N1′) iron(II)] bis(perchlorate), will be discussed. An analysis is made among the structures and the cooperativity of the spin-crossover behaviour of polynuclear Fe(II) spin-transition materials.

Anisotropic properties of human tibial cortical bone as measured by nanoindentation

The purpose of this study was to investigate the effects of elastic anisotropy on nanoindentation measurements in human tibial cortical bone. Nanoindentation was conducted in 12 different directions in three principal planes for both osteonic and interstitial lamellae. The experimental indentation modulus was found to vary with indentation direction and showed obvious anisotropy (oneway analysis of variance test, P < 0.0001). Because experimental indentation modulus in a specific direction is determined by all of the elastic constants of cortical bone, a complex theoretical model is required to analyze the experimental results. A recently developed analysis of indentation for the properties of anisotropic materials was used to quantitatively predict indentation modulus by using the stiffness matrix of human tibial cortical bone, which was obtained from previous ultrasound studies. After allowing for the effects of specimen preparation (dehydrated specimens in nanoindentation tests vs. moist specimens in ultrasound tests) and the structural properties of bone (different microcomponents with different mechanical properties), there were no statistically significant differences between the corrected experimental indentation modulus (Mexp) values and corresponding predicted indentation modulus (Mpre) values (two-tailed unpaired t-test, P < 0.5). The variation of Mpre values was found to exhibit the same trends as the corrected Mexp data. These results show that the effects of anisotropy on nanoindentation measurements can be quantitatively evaluated. © 2002 Orthopaedic Research Society. Published by Elsevier Science Ltd. All rights reserved.

Grewia gum 1:some mechanical and swelling properties of compact and film

Purpose: To study the mechanical and dynamic swelling properties of grewia gum, evaluate its compression behaviour and determine the effect of drying methods on its properties. Methods: Compacts (500 mg) of both freeze-dried and air-dried grewia gum were separately prepared by compression on a potassium bromide (KBr) press at different pressures and subjected to Heckel analysis. Swelling studies were performed using 200 mg compacts of the gum (freeze-dried or air-dried) compressed on a KBr press. The mechanical properties of the films of the gum prepared by casting 1 % dispersions of the gum were evaluated using Hounsfield tensiometer. The mechanical properties of grewia gum films were compared with films of pullulan and guar gum which were similarly prepared. The effect of temperature on the water uptake of the compacts was studied and the data subjected to Schott's analysis. Results: Drying conditions had no effect on the yield pressure of the gum compacts as both air-dried and freeze-dried fractions had a yield pressure of 322.6 MPa. The plots based on Schott's equation for the grewia gum samples showed that both samples (freeze-dried and air-dried) exhibited long swelling times. Grewia gum film had a tensile strength of 19.22±3.61 MPa which was similar to that of pullulan films (p > 0.05). It had an elastic modulus of 2.13±0.12 N/mm2 which was significantly lower (p < 0.05) than those of pullulan and guar gum with elastic moduli of 3.33±0.00 and 2.86±0.00 N/mm2, respectively. Conclusion: The type of drying method used does not have any effect on the degree of plasticity of grewia gum compacts. Grewia gum obtained by either drying method exhibited extended swelling duration. Matrix tablet formulations of the gum will likely swell slowly and promote sustained release of drug. © Pharmacotherapy Group, Faculty of Pharmacy, University of Benin, Benin City.