Nanostructured smart materials as functional components of medical devices

The field of medical devices has experienced, more than others, technological advances, developments and innovations, thanks to the rapidly expanding scientific knowledge and collaboration between different disciplines such as biology, engineering and materials science. The design of functional components can be achieved by exploiting composite materials based on nanostructured smart materials, that due to the inherent characteristics of single constituents develop unique properties that make them suitable for different applications preserving excellent mechanical proprieties. For instance, recent developments have focused on the fabrication of piezoelectric devices with multiple biomedical functions, as actuation and sensing functions in one component for monitoring pressure signals. The present Ph.D. Thesis aims at investigating nanostructured smart materials embedded into a polymeric matrix to obtain a composite material that can be used as a functional component for medical devices. (i) Nanostructured piezoelectric material with self-sensing capability was successfully manufactured by using ceramic (i.e. lead zirconate titanate (PZT)) and (ii) polymeric (i.e. poly(vinylidene fluoride-trifluoro ethylene (PVDF-TRFE)) piezoelectric materials. PZT nanofibers were obtained by sol-gel electrospinning starting from synthetized PZT precursor solution. Synthesis, sol-gel electrospinning process, and thermal treatment were accurately controlled to obtain PZT nanofibers dimensionally stable with densely packed grains in the perovskite phase. To guarantee the impact resistance of the laminate, the morphology and size of the hosting filler were accurately designed by increasing the surface area to volume ratio. Moreover, to solve the issue relative to the mechanical discrepancy between rigid electronic materials/soft human tissues/different material of the device (iii) a nanostructured flexible composite material based on a network of Poly-L-lactic acid (PLLA) made of curled nanofibers that present a tuneable mechanical response as a function of the applied stress was successful fabricated.

Mechanical properties of Y-TPZ ceramics obtained by liquid phase sintering using bioglass as additive

Yttria stabilized tetragonal zirconia (Y-TZP) ceramics were sintered by liquid phase sintering at low temperatures using bioglass as sintering additive. ZrO2-bioglass ceramics were prepared by mixing a ZrO2 stabilized with 3 Mol%Y2O3 and different amounts of bioglass based on 3CaO center dot P2O5-MgO-SiO2 system. Mixtures were compacted by uniaxial cold pressing and sintered in air, at 1200 and 1300 degrees C for 120 min. The influence of the bioglass content on the densification, tetragonal phase stability, bending strength, hardness and fracture toughness was investigated. The ceramics sintered at 1300 degrees C and prepared by addition of 3% of bioglass, exhibited the highest strength of 435 MPa, hardness of 1170 HV and fracture toughness of 6.3 MPa m(1/2). These results are related to the low monoclinic phase content, high relative density and the presence of the thermal residual stress generated between the ZrO2-matrix and bioglass grain boundary, contributing to the activation of the toughening mechanisms. (c) 2007 Elsevier B.V. All rights reserved.

Composition and orientation effects on the final recrystallization texture of coarse-grained Nb-containing AISI 430 ferritic stainless steels

Composition and orientation effects on the final recrystallization texture of three coarse-grained Nb-containing AISI 430 ferritic stainless steels (FSSs) were investigated. Hot-bands of steels containing distinct amounts of niobium, carbon and nitrogen were annealed at 1250 degrees C for 2h to promote grain growth. In particular, the amounts of Nb in solid solution vary from one grade to another. For purposes of comparison, the texture evolution of a hot-band sheet annealed at 1030 degrees C for 1 min (finer grain structure) was also investigated. Subsequently, the four sheets were cold rolled up to 80% reduction and then annealed at 800 degrees C for 15 min. Texture was determined using X-ray diffraction and electron backscatter diffraction (EBSD). Noticeable differences regarding the final recrystallization texture and microstructure were observed in the four investigated grades. Results suggest that distinct nucleation mechanisms take place within these large grains leading to the development of different final recrystallization textures. (c) 2011 Elsevier B.V. All rights reserved.

Annealing effects on microstructure and coercive field of ferritic-martensitic ODS Eurofer steel

Oxide dispersion strengthened reduced-activation ferritic-martensitic steels are promising candidates for applications in future fusion power plants. Samples of a reduced activation ferritic-martensitic 9 wt.%Cr-oxide dispersion strengthened Eurofer steel were cold rolled to 80% reduction in thickness and annealed in vacuum for 1 h from 200 to 1350 degrees C to evaluate its thermal stability. Vickers microhardness testing and electron backscatter diffraction (EBSD) were used to characterize the microstructure. The microstructural changes were also followed by magnetic measurements, in particular the corresponding variation of the coercive field (H(c)), as a function of the annealing treatment. Results show that magnetic measurements were sensitive to detect the changes, in particular the martensitic transformation, in samples annealed above 850 degrees C (austenitic regime). (C) 2010 Elsevier B.V. All rights reserved.

EIS study of Ti-23Ta alloy in artificial saliva

Although titanium and Ti-6Al-4V alloy have been widely used as dental materials, possible undesirable effects such as cytotoxic reactions and neurological disorder due to metal release led to the development of more corrosion resistant and V and Al free titanium alloys, containing Nb, Zr, Mo and Ta atoxic elements. Fluoride containing products used in the prevention of plaque formation and dental caries can affect the stability of the passive oxide films formed on the Ti alloys. In this work, the corrosion behaviour of the new Ti-23Ta alloy has been evaluated in artificial saliva of different pH and fluoride concentration using electrochemical impedance spectroscopy. Electrochemical impedance spectroscopy study showed that the oxide film formed on the alloy in artificial saliva consists of an inner compact film and an outer porous layer. The corrosion resistance of Ti-23Ta alloy which is reduced by increasing F concentration or decreasing pH is related to the resistance of the inner compact layer. The presence of fluoride and low pH of the saliva enhance the porosity of the oxide film and its dissolution.

Selection of new glass-forming compositions in Al-La system using a combination of topological instability and thermodynamic criteria

A combination of an extension of the topological instability ""lambda criterion"" and a thermodynamic criterion were applied to the Al-La system, indicating the best range of compositions for glass formation. Alloy compositions in this range were prepared by melt-spinning and casting in an arc-melting furnace with a wedge-section copper mold. The GFA of these samples was evaluated by X-ray diffraction, differential scanning calorimetry and scanning electron microscopy. The results indicated that the gamma* parameter of compositions with high GFA is higher, corresponding to a range in which the lambda parameter is greater than 0.1, which are compositions far from Al solid solution. A new alloy was identified with the best GFA reported so far for this system, showing a maximum thickness of 286 mu m in a wedge-section copper mold. Crown Copyright (C) 2009 Published by Elsevier B.V. All rights reserved.

Properties of Y-TZP/Al(2)O(3) ceramic nanocomposites obtained by high-energy ball milling

In this work, the synthesis of Y(2)O(3) stabilized tetragonal zirconia polycrystals (Y-TZP)-alumina (Al(2)O(3)) powder mixture was performed by high-energy ball milling and the sintering behavior of this composite was investigated. In order to understand the phase transformations occurring during ball milling, samples were collected after different milling times, from 1 to 60 h. The milled powders were compacted by cold uniaxial pressing and sintered at 1400 and 1600 degrees C. Both powders and sintered samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry analysis (EDS) and mechanical properties. Fully dense samples were obtained after sintering at 1600 degrees C, while the samples sintered at 1400 degrees C presented a full density for powder mixtures milled for 30 and 60 h. Fracture toughness and Vickers hardnessvalues of the Y-T-ZP/Al(2)O(3) nanocomposite were improved due to dispersed Al(2)O(3) grains and reduced ZrO(2) grain size. Samples sintered at 1400 degrees C, based on powders milled for 60 h, presented high K(IC) and hardness values near to 8.0 Mpan(1/2) and 15 GPa, respectively (C) 2008 Elsevier B.V. All rights reserved

Bidimensional codes recorded on an oxide glass surface using a continuous wave CO(2) laser

Surface heat treatment in glasses and ceramics, using CO(2) lasers, has attracted the attention of several researchers around the world due to its impact in technological applications, such as lab-on-a-chip devices, diffraction gratings and microlenses. Microlens fabrication on a glass surface has been studied mainly due to its importance in optical devices (fiber coupling, CCD signal enhancement, etc). The goal of this work is to present a systematic study of the conditions for microlens fabrications, along with the viability of using microlens arrays, recorded on the glass surface, as bidimensional codes for product identification. This would allow the production of codes without any residues (like the fine powder generated by laser ablation) and resistance to an aggressive environment, such as sterilization processes. The microlens arrays were fabricated using a continuous wave CO(2) laser, focused on the surface of flat commercial soda-lime silicate glass substrates. The fabrication conditions were studied based on laser power, heating time and microlens profiles. A He-Ne laser was used as a light source in a qualitative experiment to test the viability of using the microlenses as bidimensional codes.

Analytical formulae for electromechanical effective properties of 3-1 longitudinally porous piezoelectric materials

A unidirectional fiber composite is considered here, the fibers of which are empty cylindrical holes periodically distributed in a transversely isotropic piezoelectric matrix, The empty-fiber cross-section is circular and the periodicity is the same in two directions at an angle pi/2 or pi/3. Closed-form formulae for all electromechanical effective properties of these 3-1 longitudinally periodic porous piezoelectric materials are presented. The derivation of such expressions is based on the asymptotic homogenization method as a limit of the effective properties of two-phase transversely isotropic parallel fiber-reinforced composites when the fibers properties tend to zero. The plane effective coefficients satisfy the corresponding Schulgasser-Benveniste-Dvorak universal type of relations, A new relation among the antiplane effective constants from the solutions of two antiplane strains and potential local problems is found. This relation is valid for arbitrary shapes of the empty-fiber cross-sections. Based on such a relation, and using recent numerical results for isotropic conductive composites, the antiplane effective properties are computed for different geometrical shapes of the empty-fiber cross-section. Comparisons with other analytical and numerical theories are presented. (c) 2008 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Impact of transition oxides on growth stresses and texture of alumina scales formed during oxidation of iron aluminides

The internal stresses and crystallographic texture in alpha-Al(2)O(3) scales grown on iron aluminides at 1100 degrees C were determined in situ using synchrotron X-ray diffraction. In the first hour of oxidation, alpha-Al(2)O(3) was formed by direct nucleation and by conversion from transition oxides (either theta-Al(2)O(3) or a mixed Fe-Al oxide). A sharp texture develops connected with the direct nucleation of alpha-Al(2)O(3), in contrast to the weaker texture observed in alpha-Al(2)O(3) originated by previous transformations, which also yielded tensile stresses in early oxidation stages. (C) 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Microstructure and mechanical properties of laser-welded joints of TWIP and TRIP steels

With the aim of investigating a laser-welded dissimilar joint of TWIP and TRIP steel sheets, the microstructure was characterized by means of OM, SEM, and EBSD to differentiate the fusion zone, heat-affected zone, and the base material. OIM was used to differentiate between ferritic, bainitic, and martensitic structures. Compositions were measured by means of optical emission spectrometry and EDX to evaluate the effect of manganese segregation. Microhardness measurements and tensile tests were performed to evaluate the mechanical properties of the joint. Residual stresses and XRD phase quantification were used to characterize the weld. Grain coarsening and martensitic areas were found in the fusion zone, and they had significant effects on the mechanical properties of the weld. The heat-affected zone of the TRIP steel and the corresponding base material showed considerable differences in the microstructure and properties. (C) 2009 Elsevier B.V. All rights reserved.

Thixocasting of an A356 alloy: Fluidity, porosity distribution and thermomechanical fatigue behavior

An extensive set of experiments was performed on a semi-solid A356 alloy in order to assess its flow behavior, mechanical properties, microstructural evolution and porosity level. Three different microstructural conditioning techniques (raw material preparation) were employed: deformation recrystallization, magnetohydrodynamic stirring and low temperature pouring. Measurement of microstructural parameters such as Al-alpha particle size, shape factor, contiguity and entrapped liquid showed a relative equivalency among the various conditioning techniques. It was found that the strongest influence on semi-solid slurry fluidity is exerted by the mould temperature. Tensile properties and porosity levels were measured on a demonstration part produced with different slurry ingate velocities. Results showed similar strength levels among all thixocast samples, a strong correlation between elongation and pore volume fraction and porosity levels much lower than the typical figure for permanent mould or die cast Al-Si alloys. Finally, thermomechanical fatigue tests results were much more favorable to the semi-solid material when compared with the conventionally cast alloy, a result attributed to lower porosity, spheroidal shape of the Al-alpha phase, and refined Si eutectic particles. alpha 2007 Elsevier B.V. All rights reserved.

Ultrasound, eddy current and magnetic Barkhausen noise as tools for sigma phase detection on a UNS S31803 duplex stainless steel

Sigma phase is a deleterious one which can be formed in duplex stainless steels during heat treatment or welding. Aiming to accompany this transformation, ferrite and sigma percentage and hardness were measured on samples of a UNS S31803 duplex stainless steel submitted to heat treatment. These results were compared to measurements obtained from ultrasound and eddy current techniques, i.e., velocity and impedance, respectively. Additionally, backscattered signals produced by wave propagation were acquired during ultrasonic inspection as well as magnetic Barkhausen noise during magnetic inspection. Both signal types were processed via a combination of detrended-fluctuation analysis (DFA) and principal component analysis (PCA). The techniques used were proven to be sensitive to changes in samples related to sigma phase formation due to heat treatment. Furthermore, there is an advantage using these methods since they are nondestructive. (C) 2010 Elsevier B.V. All rights reserved.

Chemical characterization of a high nitrogen stainless steel by optimized electron probe microanalysis

The distribution of Cr and N in a high-temperature gas-nitrided stainless steel was measured by using a scanning electron microscope-coupled wavelength-dispersive X-ray spectrometer and the results were related to the microhardness profile of the hardened case. The experimental spectrometric procedure was optimized to consistently measure N contents varying between 0.1 and 0.8 wt.% in martensite and between 18.3 and 21.6 wt.% in nitrides, as well as Cr contents ranging from 11.5 to 17.0 wt.%. (C) 2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.