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.

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.

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.

The management of posterior vitreous detachment by an optometrist

Acute posterior vitreous detachment (PVD) is the most common cause of retinal detachment. The management of this condition can be variable and often undue reliance is placed upon associated signs and symptoms which can be a poor indicator of pathology. Optometrists undertake a number of extended roles, however involvement in vitreo-retinal sub-specialities appears to be limited. One objective was to directly compare an optometrist and ophthalmologist in the assessment of patients with PVD, for this a high level of agreement was found (95% sensitivity, 99% specificity, 0.94 kappa). A review of 1107 patients diagnosed with acute PVD that were re-evaluated in a PVD clinic a few weeks later was undertaken to determine whether such reviews are necessary. One-fifth of patients were found to have conditions undiagnosed at the initial assessment, overall 4% of patients had retinal breaks when examined in the PVD clinic and a total of 7% required further intervention. The sensitivity of fundus examination with +90D and 3-mirror lenses was 85-88% for detecting retinal breaks and 7-85% for pigment in the anterior vitreous for the presence of retinal breaks. Therefore patients with acute PVD should be examined by indirect ophthalmoscopy with indentation at the onset of PVD and 4-6 weeks later. The treatment of retinal breaks with laser retinopexy is performed by ophthalmologists with a primary success rate 54-85%. In a pioneering development, an optometrist undertaking this role achieved a comparable primary success rate (79%). Mid-vitreous opacities associated with PVD are described, and noted in 100% of eyes with PVD. The recognition of this sign is important in the diagnosis of PVD and retinal breaks. The importance of diagnostic imaging is also demonstrated, however the timing in relation to onset may be vital.

Electro and Magneto-Electropolished Surface Micro-Patterning on Binary and Ternary Nitinol

In this study, an Atomic Force Microscopy (AFM) roughness analysis was performed on non-commercial Nitinol alloys with Electropolished (EP) and Magneto-Electropolished (MEP) surface treatments and commercially available stents by measuring Root-Mean-Square (RMS) , Average Roughness (Ra), and Surface Area (SA) values at various dimensional areas on the alloy surfaces, ranging from (800 x 800 nm) to (115 x 115µm), and (800 x 800 nm) to (40 x 40 µm) on the commercial stents. Results showed that NiTi-Ta 10 wt% with an EP surface treatment yielded the highest overall roughness, while the NiTi-Cu 10 wt% alloy had the lowest roughness when analyzed over (115 x 115 µm). Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) analysis revealed unique surface morphologies for surface treated alloys, as well as an aggregation of ternary elements Cr and Cu at grain boundaries in MEP and EP surface treated alloys, and non-surface treated alloys. Such surface micro-patterning on ternary Nitinol alloys could increase cellular adhesion and accelerate surface endothelialization of endovascular stents, thus reducing the likelihood of in-stent restenosis and provide insight into hemodynamic flow regimes and the corrosion behavior of an implantable device influenced from such surface micro-patterns.

An energy based nanomechnical properties evaluation method for cementitious materials

Advances in multiscale material modeling of structural concrete have created an upsurge of interest in the accurate evaluation of mechanical properties and volume fractions of its nano constituents. The task is accomplished by analyzing the response of a material to indentation, obtained as an outcome of a nanoindentation experiment, using a procedure called the Oliver and Pharr (OP) method. Despite its widespread use, the accuracy of this method is often questioned when it is applied to the data from heterogeneous materials or from the materials that show pile-up and sink-in during indentation, which necessitates the development of an alternative method. ^ In this study, a model is developed within the framework defined by contact mechanics to compute the nanomechanical properties of a material from its indentation response. Unlike the OP method, indentation energies are employed in the form of dimensionless constants to evaluate model parameters. Analysis of the load-displacement data pertaining to a wide range of materials revealed that the energy constants may be used to determine the indenter tip bluntness, hardness and initial unloading stiffness of the material. The proposed model has two main advantages: (1) it does not require the computation of the contact area, a source of error in the existing method; and (2) it incorporates the effect of peak indentation load, dwelling period and indenter tip bluntness on the measured mechanical properties explicitly. ^ Indentation tests are also carried out on samples from cement paste to validate the energy based model developed herein by determining the elastic modulus and hardness of different phases of the paste. As a consequence, it has been found that the model computes the mechanical properties in close agreement with that obtained by the OP method; a discrepancy, though insignificant, is observed more in the case of C-S-H than in the anhydrous phase. Nevertheless, the proposed method is computationally efficient, and thus it is highly suitable when the grid indentation technique is required to be performed. In addition, several empirical relations are developed that are found to be crucial in understanding the nanomechanical behavior of cementitious materials.^

A model of school managerial control : the systematic analysis of managerial behaviors, processes, and indicators

The theoretical construct of control has been defined as necessary (Etzioni, 1965), ubiquitous (Vickers, 1967), and on-going (E. Langer, 1983). Empirical measures, however, have not adequately given meaning to this potent construct, especially within complex organizations such as schools. Four stages of theory-development and empirical testing of school building managerial control using principals and teachers working within the nation's fourth largest district are presented in this dissertation as follows: (1) a review and synthesis of social science theories of control across the literatures of organizational theory, political science, sociology, psychology, and philosophy; (2) a systematic analysis of school managerial activities performed at the building level within the context of curricular and instructional tasks; (3) the development of a survey questionnaire to measure school building managerial control; and (4) initial tests of construct validity including inter-item reliability statistics, principal components analyses, and multivariate tests of significance. The social science synthesis provided support of four managerial control processes: standards, information, assessment, and incentives. The systematic analysis of school managerial activities led to further categorization between structural frequency of behaviors and discretionary qualities of behaviors across each of the control processes and the curricular and instructional tasks. Teacher survey responses (N=486) reported a significant difference between these two dimensions of control, structural frequency and discretionary qualities, for standards, information, and assessments, but not for incentives. The descriptive model of school managerial control suggests that (1) teachers perceive structural and discretionary managerial behaviors under information and incentives more clearly than activities representing standards or assessments, (2) standards are primarily structural while assessments are primarily qualitative, (3) teacher satisfaction is most closely related to the equitable distribution of incentives, (4) each of the structural managerial behaviors has a qualitative effect on teachers, and that (5) certain qualities of managerial behaviors are perceived by teachers as distinctly discretionary, apart from school structure. The variables of teacher tenure and school effectiveness reported significant effects on school managerial control processes, while instructional levels (elementary, junior, and senior) and individual school differences were not found to be significant for the construct of school managerial control.

Densificação e microestrutura de um compósito Mo-Cu preparado a partir de um pó de heptamolibidato de amônia e cobre

The Cu-Mo system is a composite used in the electrical industry as material for electrical contact and resistance welding electrode as well as the heat sink and microwave absorber in microelectronic devices. The use of this material in such applications is due to the excellent properties of thermal and electrical conductivity and the possibility of adjustment of its coefficient of thermal expansion to meet those of materials used as substrates in the semiconductor micoreletrônic industry. Powder metallurgy through the processes of milling, pressing shaping and sintering is a viable technique for consolidation of such material. However, the mutual insolubility of both phases and the low wettability of liquid Cu on Mo impede its densification. However, the mutual insolubility of both phases and the low wettability of liquid Cu on Mo impede its densification. The mechanical alloying is a technique for preparation of powders used to produce nanocrystalline composite powder with amorphous phase or extended solid solution, which increases the sinterability immiscible systems such as the Mo-Cu. This paper investigates the influence of ammonium heptamolybdate (HMA) and the mechanical alloying in the preparation of a composite powder HMA-20% Cu and the effect of this preparation on densification and structure of MoCu composite produced. HMA and Cu powders in the proportion of 20% by weight of Cu were prepared by the techniques of mechanical mixing and mechanical alloying in a planetary mill. These were milled for 50 hours. To observe the evolution of the characteristics of the particles, powder samples were taken after 2, 10, 15, 20, 30 and 40 hours of milling. Cylindrical samples 5 to 8 mm in diameter and 3 to 4 mm thickness were obtained by pressing at 200 MPa to the mixed powders so as to ground. These samples were sintered at 1200 ° C for 60 minutes under an atmosphere of H2. To determine the effect of heating rate on the structure of the material during the decomposition and reduction of HMA, rates of 2, 5 and 10 ° C / min were used .. The post and the structures of the sintered samples were characterized by SEM and EDS. The density of the green and sintered bodies was measured using the geometric method (weight / volume). Vickers microhardness with a load of 1 N for 15 s were performed on sintered structures. The density of the sintered structures 10 ° C / min. reached 99% of theoretical density, how the density of sintered structures to 2 ° C / min. reached only 90% of the theoretical density

Estudo de um compósito Nb-15%pCu obtidos por moagem de alta energia e sinterizados por fase líquida

There is great difficulty in forming a composite refractory metal niobium with copper. This is due to the fact that Nb-Cu system is almost mutually immiscible and may be neglected solubility between them. These properties hinder or prevent obtaining homogeneous and high-density structures, conventionally prepared. This study aims to analyze the use of high-energy milling process (MAE) to implement these natural difficulties, with regard to the densification of the sintered bodies. The MAE and the press were used in the preparation of powders, to obtain a fine and homogeneous distribution of the grain size. Four loads Nb and Cu powders containing 15% by weight of Cu were then milled for MAE in a planetary type ball mill under various milling times and speeds. The results obtained by MAE were analyzed by scanning electron microscopy (SEM), according to the parameters of time and grinding speed. The samples were compacted under pressure of 200 MPa, were then sintered in liquid phase in a vacuum furnace at temperatures of 1100 ° C / 60 min and 1200 ° C / 60 min. Then it was used to characterize diffraction of X-rays to identify the phases. The microstructures of the sintered samples were observed and evaluated using scanning electron microscopy (SEM). Vickers Microhardness tests were performed, obtaining higher values for the sintered bodies in the largest of the post milling times and the larger grinding speeds. It was found that the liquid phase sintering of the samples that were processed by MAE produced at the end of a homogeneous and densified structure in 77,4% relative to the value of the theoretical density of the composite

Efeito da moagem de alta energia na densificação e microestrutura do compósito AI2O3-Cu

The Cu-Al2O3 composite ceramic combines the phase of alumina, which is extremely hard and durable, yet very brittle, to metallic copper phase high ductility and high fracture toughness. These characteristics make this material a strong candidate for use as a cutting tool. Al2O3-Cu composite powders nanocrystalline and high homogeneity can be produced by high energy milling, as well as dense and better mechanical structures can be obtained by liquid phase sintering. This work investigates the effect of high-energy milling the dispersion phase Al2O3, Cu, and the influence of the content of Cu in the formation of Cu-Al2O3 composite particles. A planetary mill Pulverisatte 7 high energy was used to perform the experiments grinding. Al2O3 powder and Cu in the proportion of 5, 10 and 15% by weight of Cu were placed in a container for grinding with balls of hard metal and ethyl alcohol. A mass ratio of balls to powder of 1:5 was used. All powders were milled to 100 hours, and powder samples were collected after 2, 10, 20, 50 and 70 hours of grinding. Composite powders with compact cylindrical shape of 8 mm diameter were pressed and sintered in uniaxial matrix resistive furnace to 1200, 1300 to 1350 °C for 60 minutes under an atmosphere of argon and hydrogen. The heating rate used was 10°C/min. The powders and structures of the sintered bodies were characterized by XRD, SEM and EDS. Analysis TG, DSC and particle size were also used to characterize the milled powders, as well as dilatometry was used to observe the contraction of the sintered bodies. The density of the green and sintered bodies was measured using the geometric method (mass / volume). Vickers microhardness with a load of 500 g for 10 s were performed on sintered structures. The Cu-Al2O3 composite with 5% copper density reached 61% of theoretical density and a hardness of 129 HV when sintered at 1300 ° C for 1h. In contrast, lower densities (59 and 51% of the theoretical density) and hardness (110 HV and 105) were achieved when the copper content increases to 10 and 15%.

Estudo do comportamento da sinterização de compactos de cavacos de um aço SAE 1050 obtidos sob alta pressão

From an economic standpoint, the powder metallurgy (P/M) is a technique widely used for the production of small parts. It is possible, through the P/M and prior comminution of solid waste such as ferrous chips, produce highly dense sintered parts and of interest to the automotive, electronics and aerospace industries. However, without prior comminution the chip, the production of bodies with a density equal to theoretical density by conventional sintering techniques require the use of additives or significantly higher temperatures than 1250ºC. An alternative route to the production of sintered bodies with high density compaction from ferrous chips (≤ 850 microns) and solid phase sintering is a compression technique under high pressure (HP). In this work, different compaction pressures to produce a sintered chip of SAE 1050 carbon steel were used. Specifically, the objective was to investigate them, the effect of high pressure compression in the behavior of densification of the sintered samples. Therefore, samples of the chips from the SAE 1050 carbon steel were uniaxially cold compacted at 500 and 2000 MPa, respectively. The green compacts obtained were sintered under carbon atmosphere at 1100 and 1200°C for 90 minutes. The heating rate used was 20°C/min. The starting materials and the sintered bodies were characterized by optical microscopy, SEM, XRD, density measurements (geometric: mass/volume, and pycnometry) and microhardness measurements Vickers and Rockwell hardness. The results showed that the compact produced under 2000 MPa presented relative density values between 93% and 100% of theoretical density and microhardness between 150 HV and 180 HV, respectively. In contrast, compressed under 500 MPa showed a very heterogeneous microstructure, density value below 80% of theoretical density and structural conditions of inadequate specimens for carrying out the hardness and microhardness measurements. The results indicate that use of the high pressure of ferrous chips compression is a promising route to improve the sinterability conditions of this type of material, because in addition to promoting greater compression of the starting material, the external tension acts together with surface tension, functioning as the motive power for sintering process. Additionally, extremely high pressures allow plastic deformation of the material, providing an intimate and extended contact of the particles and eliminating cracks and pores. This tends to reduce the time and / or temperature required for good sintering, avoiding excessive grain growth without the use of additives. Moreover, higher pressures lead to fracture the grains in fragile or ductile materials highly hardened, which provides a starting powder for sintering, thinner, without the risk of contamination present when previous methods are used comminution of the powder.

Estudo de duas pseudoligas de Nb-Cu obtidas pela rota da metalurgia do pó

The Nb-Cu pseudoalloys present themselves as potential substitutes for the alloys from a well known system and already commercially applied, as the W-Cu alloys, used in applications such as heat sinks, electrical contacts and coils for the generation of high magnetic fields. Because it is an immiscible system, where there is mutual insolubility and low wettability of the liquid Cu on the Nb surface, the processing route used in this work was the Powder Metallurgy. Two Nb alloys were used, with additions of 10% and 20% in weight of Cu, and times of 20, 30 and 40 hours for the high energy milling of the starting powders. The milling evolution of the powders is presented through the characterization techniques, such as the LASER diffraction for particle size, XRD, SEM, EDS, DSC, dilatometry, TEM and chemical analysis. After the milling, portions of the loads were submitted to the annealing heat treatment. The process used for the samples consolidation was the hot pressing, which has been applied both on some milled powders samples, as on the annealed powders. Subsequent heat treatments were performed in the samples at temperatures of 1000ºC (solid phase) and 1100ºC (in the Cu liquid phase). All sets of consolidated samples, and also the two sets of the heat treated, were analyzed by XRD, SEM, EDS, density and Vickers microhardness. Moreover, other Nb powder samples with 10% and 20% in weight of Cu obtained by simple mechanical mixing, were consolidated, thermally treated and characterized with the same techniques applied to the others, and the results were compared among themselves. Despite the difficulty of consolidation and densification of the two pseudoalloys of the Nb-Cu system of this study, on the route that passes through the HEM, samples were obtained with densities around 90% of the theoretical density. And, on the processing route of which were only mixed, the values reached up to 97%. Therefore, in this work are also emphasized the processes that made possible these results.

Evaluation of degree of conversion and hardness of dental composites photo-activated with different light guide tips

Objective: The aim of this study was to evaluate the degree of conversion and hardness of different composite resins, photo-activated for 40 s with two different light guide tips, fiber optic and polymer. Methods: Five specimens were made for each group evaluated. The percentage of unreacted carbon double bonds (% C═C) was determined from the ratio of absorbance intensities of aliphatic C═C (peak at 1637 cm−1) against internal standard before and after curing of the specimen: aromatic C-C (peak at 1610 cm−1). The Vickers hardness measurements were performed in a universal testing machine. A 50 gf load was used and the indenter with a dwell time of 30 seconds. The degree of conversion and hardness mean values were analyzed separately by ANOVA and Tukey’s test, with a significance level set at 5%. Results: The mean values of degree of conversion for the polymer and fiber optic light guide tip were statistically different (P<.001). The hardness mean values were statistically different among the light guide tips (P<.001), but also there was difference between top and bottom surfaces (P<.001). Conclusions: The results showed that the resins photo-activated with the fiber optic light guide tip promoted higher values for degree of conversion and hardness.

Estudo da evolução das tensões residuais através da difratometria de raios x em aço rolamento submetido a esforços cíclicos

The micro-deformations caused by cyclic loading origins the variation of the distances between atoms of the crystal lattice producing the irreversible component. In order to study and understand the microstructural behavior of the material this paper investigated the influence suffered by residual stresses in thrust rolling bearing races fabricated in AISI 52100 steel, after tests by cyclic rolling contact in a tribometer at 1m/s under two contact pressures (500 MPa and 1400 MPa) in dry and boundary lubrication conditions. Procedures of tests thermo-acustically isolated were developed for monitoring the contact temperature and sound pressure level signals to establish a comparison between the residual stress measurements, micro-hardness Vickers and micrographic registers searching an indication of wear evolution. The sin²ψ method by X-ray diffraction technique was used to quantify the residual stresses. Three raceway zones were selected for the evaluation of wear and surface morphology after predetermined cycling, comparing with their new condition ("as received"). Micro-hardness and residual stress measurements showed significant changes after the tests and it was possible to observe the relationship between the increase of sound pressure level and the residual stress for dry and lubricated conditions.

Estudo da evolução das tensões residuais através da difratometria de raios x em aço rolamento submetido a esforços cíclicos

The micro-deformations caused by cyclic loading origins the variation of the distances between atoms of the crystal lattice producing the irreversible component. In order to study and understand the microstructural behavior of the material this paper investigated the influence suffered by residual stresses in thrust rolling bearing races fabricated in AISI 52100 steel, after tests by cyclic rolling contact in a tribometer at 1m/s under two contact pressures (500 MPa and 1400 MPa) in dry and boundary lubrication conditions. Procedures of tests thermo-acustically isolated were developed for monitoring the contact temperature and sound pressure level signals to establish a comparison between the residual stress measurements, micro-hardness Vickers and micrographic registers searching an indication of wear evolution. The sin²ψ method by X-ray diffraction technique was used to quantify the residual stresses. Three raceway zones were selected for the evaluation of wear and surface morphology after predetermined cycling, comparing with their new condition ("as received"). Micro-hardness and residual stress measurements showed significant changes after the tests and it was possible to observe the relationship between the increase of sound pressure level and the residual stress for dry and lubricated conditions.