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The 6th EEIGM Conference on Advanced Materials Research (AMR 2011) was held at the European School of Materials Engineering (EEIGM) on the 7–8 November 2011 in Nancy, France. This biennial conference organized by the EEIGM is a wonderful opportunity for all scientists involved in the EEIGM programme, in the 'Erasmus Mundus' Advanced Materials Science and Engineering Master programme (AMASE) and the 'Erasmus Mundus' Doctoral Programme in Materials Science and Engineering (DocMASE), to present their research in the various fields of Materials Science and Engineering. This conference is also open to other universities who have strong links with the EEIGM and provides a forum for the exchange of ideas, co-operation and future orientations by means of regular presentations, posters and a round-table discussion. This edition of the conference included a round-table discussion on composite materials within the Interreg IVA project '+Composite'.

Following the publication of the proceedings of AMR 2009 in Volume 5 of this journal, it is with great pleasure that we present this selection of articles to the readers of IOP Conference Series: Materials Science and Engineering. Once again it represents the interdisciplinary nature of Materials Science and Engineering, covering basic and applicative research on organic and composite materials, metallic materials and ceramics, and characterization methods.

The editors are indebted to all the reviewers for reviewing the papers at very short notice. Special thanks are offered to the sponsors of the conference including EEIGM-Université de Lorraine, AMASE, DocMASE, Grand Nancy, Ville de Nancy, Region Lorraine, Fédération Jacques Villermaux, Conseil Général de Meurthe et Moselle, Casden and '+Composite'.

Zoubir Ayadi, David Horwat and Brigitte Jamart

All papers published in this volume of IOP Conference Series: Materials Science and Engineering have been peer reviewed through processes administered by the proceedings Editors. Reviews were conducted by expert referees to the professional and scientific standards expected of a proceedings journal published by IOP Publishing.

Fiber/matrix interface debond growth is one of the main mechanisms of damage evolution in unidirectional (UD) polymer composites. Because for polymer composites the fiber strain to failure is smaller than for the matrix multiple fiber breaks occur at random positions when high mechanical stress is applied to the composite. The energy released due to each fiber break is usually larger than necessary for the creation of a fiber break therefore a partial debonding of fiber/matrix interface is typically observed. Thus the stiffness reduction of UD composite is contributed both from the fiber breaks and from the interface debonds. The aim of this paper is to analyze the debond growth in carbon fiber/epoxy and glass fiber/epoxy UD composites using fracture mechanics principles by calculation of energy release rate G_II. A 3-D FEM model is developed for calculation of energy release rate for fiber/matrix interface debonds at different locations in the composite including the composite surface region where the stress state differs from the one in the bulk composite. In the model individual partially debonded fiber is surrounded by matrix region and embedded in a homogenized composite.

Composite laminates during service undergo complex combinations of thermal and mechanical loading leading to microdamage accumulation in the plies. The most common damage mode and the one examined in this work is intralaminar cracking in layers. The crack opening displacement (COD) and the crack sliding displacement (CSD) during loading reduce the average stress in the damaged layer, thus reducing the laminate stiffness.

These parameters depend on material properties of the damaged layer and surrounding layers, on layer orientation and thickness. Previously these parameters have been calculated using finite element method (FEM) assuming linear elastic material with idealized geometry of cracks. To validate these assumptions experimentally the displacement field on the surface of a [90/0/90] carbon fiber/epoxy laminate specimens with multiple intralaminar cracks in the surface layer is studied and the COD dependence on the applied mechanical load is measured. The specimen full-field displacement measurement is carried out using ESPI (Electronic Speckle Pattern Interferometry). The displacement jumps corresponding to cracks are clearly visible and can be used to determine the opening displacement along the cracks. The effect of crack interaction on the COD at high crack density is also investigated.

The most common damage mode and the one examined in this work is the formation of intralaminar cracks in layers of laminates. These cracks can occur when the composite structure is subjected to mechanical and/or thermal loading and eventually lead to degradation of thermo-elastic properties. In the present work, the shear modulus reduction due to cracking is studied. Mathematical models exist in literature for the simple case of cross-ply laminates. The in-plane shear modulus of a damaged laminate is only considered in a few studies. In the current work, the shear modulus reduction in cross-plies will be analysed based on the principle of minimization of complementary energy. Hashin investigated the in-plane shear modulus reduction of cross-ply laminates with cracks in inside 90-layer using this variational approach and assuming that the in-plane shear stress in layers does not depend on the thickness coordinate. In the present study, a more detailed and accurate approach for stress estimation is followed using shape functions for this dependence with parameters obtained by minimization. The results for complementary energy are then compared with the respective from literature and finally an expression for shear modulus degradation is derived.

The degradation of the elastic properties of composite laminates with intralaminar cracks is caused by reduced stress in the damaged layer which is mainly due to two parameters: the crack opening displacement (COD) and the crack sliding displacement (CSD). In this paper these parameters are measured experimentally providing laminate stiffness reduction models with valuable information for validation of used assumptions and for defining limits of their application. In particular, the displacement field on the edges of a [0/ +70₄/ −70₄]_s glass fiber/epoxy laminate specimens with multiple intralaminar cracks is studied and the COD and CSD dependence on the applied mechanical load is measured. The specimen full-field displacement measurement is carried out using ESPI (Electronic Speckle Pattern Interferometry). By studying the displacement discontinuities, the crack face displacements were measured. A comparison between the COD and the CSD (for the same crack) is performed.

Non Crimp Fabrics (NCF) are promising new generation composite materials. They are now being used in some sections of composite industry, for example in wind turbine blades and boat hulls. The aerospace industry also shows an increasing interest in this material, thanks to the low cost of its manufacturing process. NCFs are special types of textile composites, made of layers of parallel fiber bundles oriented in different directions and separated by resin. Due to the manufacturing process the fiber bundles are not perfectly straight. They show a certain degree of waviness which decreases the stiffness and the strength of the material. The heterogeneous mesostructure affects the mechanical properties of the material and the failure mechanisms. This was studied using both numerical and experimental methods. In our experimental approach, a carbon fiber/epoxy resin laminate with uniform fiber distribution was manufactured by voluntarily introducing waviness to simulate the NCF composites. The displacement map was studied against the thickness of a sample loaded in tension, using ESPI (Electronic Speckle Pattern Interferometry). This can give us a primary idea of the micro damage initiation and the cracks' shapes.

The behaviour of highly non-linear cellulosic fibers and their composite is characterized. Micro-mechanisms occurring in these materials are identified. Mechanical properties of regenerated cellulose fibers and composites are obtained using simple tensile test. Material visco-plastic and visco-elastic properties are analyzed using creep tests. Two bio-based resins are used in this study – Tribest and EpoBioX. The glass and flax fiber composites are used as reference materials to compare with Cordenka fiber laminates.

Cellulose nanowhiskers separated from two different industrial residues, sludge from cellulose production (CNW_SL) and lignin residue from ethanol production (CNW_ER), were compared in order to evaluate their characteristics and their potential as a source for the production of cellulose nanowhiskers (CNWs). It was found that CNW_SL and CNW_ER suspensions exhibited flow birefringence when they were studied through cross-polarized filters. Transmission electron microscopy (TEM) study showed that the CNW_SL were longer (377 nm) than CNW_ER (301 nm). It was also demonstrated that most CNW_SL had nanowhiskers between 375-449 nm and CNW_ER between 300-374 nm. The UV/Vis spectroscopy showed a stronger interference in the UV and visible region for the CNW_SL films. The crystallinity, obtained by X-ray analysis, was higher for CNW_SL (86%) than for CNW_ER (78%). Finally, the thermal stability appeared to be slightly higher for the CNW_ER than for CNW_SL. Both studied residues seem to be suitable sources for large-scale production of CNWs.

Biopolymers have received in recent years an increasing interest for their potential applications in the field of biomedical engineering. Among the natural polymers that have been experimented, chitosan is probably the most promising in view of its exceptional biological properties. Several techniques may be employed to sterilize chitosan-based materials. The aim of our study was to compare the effect of common sterilization treatments on the degradation of chitosan-based materials in various physical states: solutions, hydrogels and solid flakes. Four sterilization methods were compared: gamma irradiation, beta irradiation, exposure to ethylene oxide and saturated water steam sterilization (autoclaving). Exposure to gamma or beta irradiation was shown to induce an important degradation of chitosan, regardless of its physical state. The chemical structure of chitosan flakes was preserved after ethylene oxide sterilization, but this technique has a limited use for materials in the dry state. Saturated water steam sterilization of chitosan solutions led to an important depolymerization. Nevertheless, steam sterilization of chitosan flakes bagged or dispersed in water was found to preserve better the molecular weight of the polymer. Hence, the sterilization of chitosan flakes dispersed in water would represent an alternative step for the preparation of sterilized chitosan solutions. Alternatively, autoclaving chitosan physical hydrogels did not significantly modify the macromolecular structure of the polymer. Thus, this method is one of the most convenient procedures for the sterilization of physical chitosan hydrogels after their preparation.

Polycarbonate foams reinforced with 0,5 wt% of graphene were obtained by firstly melt-mixing the polycarbonate and graphene in an internal mixer, compression-moulding the melt-compounded grinded material and lastly dissolving CO₂ inside a high pressure vessel. The CO₂ desorption behaviour in the unfilled polycarbonate and nanocomposite was studied in terms of the CO₂ saturation concentration and desorption diffusion coefficient, with the graphene-filled nanocomposite displaying a higher CO₂ loss rate when compared to the neat polycarbonate. The cellular structure of the foams was found to be highly dependent on the saturation/foaming temperature, with smaller cell sizes being obtained with decreasing the temperature. Another parameter that had an important influence was the residual pressure, with higher residual pressure values resulting in foams with more uniform and regular cells.

The main scope of this work was to develop a processing method to homogeneously distribute graphite nanoplatelets (GNP) within an ultra-high molecular weight polyethylene (UHMWPE) matrix. After this step, we estimated the toughness of the new nanocomposite material. Combining a sonication step, a micro-extrusion step and a hot-pressing step, we did not reach an optimal distribution state of the nanofillers. Nevertheless, the toughness of the nanocomposites evaluated by Charpy tester was higher than that of the reference UHMWPE (only processed by hot-pressing). We also found that our new processing procedure applied to neat UHMWPE leads to the higher toughness than that of the nanocomposite. Micro-extrusion appears as a promising processing tool for neat UHMWPE.

The plastic deformation accumulated during fatigue testing can induce the transformation of austenite to martensite in metastable austenitic stainless steels. To analyze this issue, a metastable austenitic stainless steel grade AISI 301 LN was studied in two different conditions, i.e. annealed and cold rolled. In the first case, the steel was fully austenitic, whereas cold rolled material had almost 30% of martensite. High cycle fatigue tests at a stress ratio of 0.8 were carried out on flat specimens from both steel conditions. Several characterization techniques, including optical microscopy, X-ray diffraction (XRD) and electron back scattered diffraction (EBSD), were used to detect and quantify the martensite induced by the cyclic deformation.

The weldability of materials is still a poorly understood concept; a quantitative assessment remains elusive. The variables associated with welding are reduced here into two groups - processing parameters and material properties - from which two characteristic indices are defined and used as the basis of weldability charts. For the case of constructional steels, a carbon equivalent characterises both heat affected zone hardenability and the maximum hardness developed after solid state phase transformations. The welding process is characterised by its energy input. A mathematical model is used to establish relationships between the indices, which are displayed on charts as contours of microstructure and hardness.

Mechanical alloying in air atmosphere lead to interaction of an initial material with the oxygen with formation of strengthening oxide particles. It allows creating the dispersion strengthened composite materials. The possibility of obtaining the composite materials based on Al-Mg-Li alloys by mechanical alloying is shown. It was found that the most intense oxidation of the material held within the first hour of milling. Microstructure evolution and mechanical properties of composite materials is investigated.

The only operation of heat treatment of 6XXX alloys before extrusion is homogenizing annealing. The presence of needle particles of β-Al₅FeSi in a billet for extrusion negatively affects the limit extrusion rate and surface quality of extruded products. Passage of the phase transformation of ferrous phases is the main limiting factor in the length of homogenizing annealing. In this work the method of quantitative phase transformation analysis is proposed for estimation the completeness of the homogenizing annealing.

Solid Metal Induced Embrittlement (SMIE) is caused by a specific combination of two solid metals in intimate contact. Cadmium, gold, silver and copper are known to cause SMIE in certain titanium alloys. Solid copper is used in welding electrodes and fixtures in various manufacturing processes for titanium parts within the aerospace industry. In the case of resistance welding, titanium alloys are in intimate contact with solid copper, since the electrodes resistively heat the titanium part under pressure during the welding process. No previous published work that investigates the risk of using copper electrodes for welding of titanium alloys is available in the literature, but an initial study using U-bend testing indicates that solid copper in contact with Ti-8Al-1V-1Mo and Ti-6Al-2Sn-4Zr-2Mo could lead to SMIE. Therefore, in the present study, resistance welded Ti-8Al-1V-1Mo and Ti-6Al-2Sn-4Zr-2Mo have been evaluated to investigate the influence of copper electrodes on these alloys. Furthermore, resistance welded specimens sputtered with copper and gold to promote SMIE have also been evaluated. No SMIE was found in the resistance welded specimens, which may be explained by the short interaction time that the copper electrodes are in intimate contact with the titanium alloy, and/or the magnitude of residual stresses after welding, which may be too low to initiate SMIE.

The surface mechanical properties of different types of advanced zirconia ceramics have been assessed after being subjected to hydrothermal degradation. Three different types of zirconia were considered: standard tetragonal polycrystalline zirconia doped with 3 % molar yttria (3Y-TZP) produced by conventional sintering; 3Y-TZP produced by spark-plasma sintering (3Y-TZP(SPS)) and a Ce-TZP/Al₂O₃ nanocomposite. Hydrothermal ageing was assessed by using X-ray diffraction. Berkovich nanoindentation was performed before and after the materials being exposed to 131 °C water vapour in autoclave, in order to assess changes in the surface hardness and Young modulus. It is shown that, while standard 3Y-TZP suffers a substantial decay of the surface mechanical properties with hydrothermal exposure, this is not the case for 3Y-TZP(SPS) and the Ce-TZP/Al₂O₃ materials. On the contrary, the later maintained their surface integrity during hydrothermal exposure. The results are explained in terms of microstructure and chemical composition.

Tetragonal Zirconia Polycrystals stabilized with 3% mol. content of yttria (3Y-TZP) has excellent properties in terms of strength and fracture toughness. These properties are mostly imputable to the transformation toughening mechanism, by which the doped metastable tetragonal phase of zirconia transforms to monoclinic under applied stress ahead of a crack. This phenomenon is accompanied by a volume expansion of 5%, and increases the resistance to crack growth, thus leading to higher toughness and strength. An important drawback of this material is represented by the Low Temperature Degradation (LTD or aging), which consists in the progressive tetragonal-to-monoclinic phase transformation by the influence of water. This work focuses on the improvement of 3Y-TZP aging behavior in order to develop a novel dental post, by means of the addition of ceria from the surface. This was achieved through the impregnation of the pre-sintered samples with a solution containing Cerium, followed by sintering. Various pre-sintering temperatures were studied in terms of microstructure, mechanical properties and aging resistance. The novel zirconia dental posts developed in this work are much more resistant to LTD as compared to the base material with no loss in mechanical properties.

The aim of this study was to compare the thermal behaviour of clays containing illite and kaolinite in various proportions. The clays contained small amounts of K and Fe, which act as fluxing agents. In order to investigate the phase formations during heating, the samples were examined in a differential scanning calorimeter at temperatures up to 1300°C. The thermal expansion of the samples was determined by dilatometer measurements from room temperature up to 1150°C. Phases were identified using x-ray diffraction and scanning electron microscopy.

In all samples, most of the kaolinite was transformed into metakaolinite during heating up to 650°C, while illite remained unchanged up to 950°C. There was no influence of K and Fe on dehydroxylation. Metakaolinite formed at temperatures above 950°C leading to a Si-Al spinel. Furthermore, mullite was formed in the temperature interval 1050-1150°C. In this temperature range, the mechanism of mullite formation depended on the amount of K and Fe in the samples, changing the temperature of formation of mullite. It was observed by x-ray diffraction that most of the illite was transformed into a Si-Al spinel phase at 1050°C, and during further heating transformed into mullite. An increased amount of illite in the clays slightly decreased the melting temperature. The dilatometer measurements showed expansion and shrinkage for the dehydroxylation and spinel-phase formation, respectively.

The comparison between different methods used to compute the logarithmic decrement in high-resolution mechanical spectroscopy (HRMS) is analyzed. The performance of parametric OMI method (Optimization in Multiple Intervals) and interpolated discrete Fourier transform (IpDFT) methods are investigated as a function of the sampling frequency used to digitize free decaying oscillations in low-frequency resonant mechanical spectrometers. It is clearly demonstrated that a new Yoshida-Magalas (YM) method is the most powerful IpDFT-based method which outperforms the standard Yoshida (Y) method and other DFT-based methods. Four IpDFT methods and the OMI method are carefully analyzed as a function of the sampling frequency. The results presented in this work clearly show that the relative error in the estimation of the logarithmic decrement depends both on the length of free decaying signal and on the sampling frequency. The effect of the sampling frequency was not yet reported in the literature. The performance of different methods used in the computations of the logarithmic decrement can be listed in the following order: (1) the OMI, (2) the Yoshida-Magalas YM, (3) the Yoshida-Magalas YMC, and finally (4) the Yoshida Y.

In this paper, we compare the values of the resonant frequency f₀ of free decaying oscillations computed according to the parametric OMI method (Optimization in Multiple Intervals) and nonparametric DFT-based (discrete Fourier transform) methods as a function of the sampling frequency. The analysis is carried out for free decaying signals embedded in an experimental noise recorded for metallic samples in a low-frequency resonant mechanical spectrometer. The Yoshida method (Y), the Agrež method (A), and new interpolated discrete Fourier transform (IpDFT) methods, that is, the Yoshida-Magalas (YM) and (YM_C) methods developed by the authors are carefully compared for the resonant frequency f₀ = 1.12345 Hz and the logarithmic decrement, δ = 0.0005. Precise estimation of the resonant frequency (Youngs' modulus ∼ f₀²) for real experimental conditions, i.e., for exponentially damped harmonic signals embedded in an experimental noise, is a complex task. In this work, various computing methods are analyzed as a function of the sampling frequency used to digitize free decaying oscillations. The importance of computing techniques to obtain reliable and precise values of the resonant frequency (i.e. Young's modulus) in materials science is emphasized.

The in-plane effective thermal conductivity of free-standing Si thin films with periodic micropores was measured at -100 to 0 °C. The Si thin films with micropores were prepared from silicon-on-insulator (SOI) wafers by standard microfabrication processes. The dimensions of the free-standing Si thin films were 200μm×150μm×2 μm, with staggered 4 μm pores having an average pitch of 4 mm. The Si thin film serves both as a heater and thermometer. The average temperature rise of the thin film is a function of its in-plane thermal conductivity. The effective thermal conductivity was calculated using a simple one-dimensional heat conduction model. The measured thermal conductivity was much lower than that expected based on classical model evaluations. A significant phonon size effect was observed even in the microsized structures, and the mean free path for phonons is very long even at the room temperature.

In several magnetic Non-Destructive Testing (NDT) methods, the local measurement of the magnetic field inside the material is required. Moreover, looking at difficult part geometries, magnetic field sensors have to be small enough in order to reach the measuring position. The most-used magnetic field sensors are coils, Hall-effect sensors, flux gates and magnetoresistive sensors. However, regarding the industrial application, those sensors are often packaged and cannot be placed close enough to the measuring position.

As part of an ongoing research project funded by the German Ministry of Economics and Technology (BMWi), a new kind of magnetic field sensor was developed and used in order to measure the strength of remanent magnetic field spots. This so-called 'Point Probe' is based upon a needle-shaped ferromagnetic core having a primary coil as a magnetic field source and a secondary coil as an inductive pick-up. This contribution describes the details of the sensor design and its operating principle. The sensitivity of the measured signals for local magnetic fields is described. Finally, a method for nondestructive hardness estimation of materials by using the Point Probe is presented. The results show a high correlation between hardness and a new coercivity-dependent testing parameter.

This research focuses on space dust ranging from 100μm to 1mm. Space dust is mainly due to secondary space debris, which is called ejecta. The objective was to create an inexpensive space dust impacts detector using elemental materials. The detector is a glass/epoxy laminate printed circuit board with an area of 81cm² for a weight of 30g. The detector can estimate the number of impacts and can give an approximation of the space dust size. The detector will be mounted on Horyu II that will operate in polar orbit for one year. In this article the authors report: a) the production of ejecta, b) the ejecta experiments on solar array coupon, aluminium honeycomb and CFRP/aluminium honeycomb, c) the detector's working principle and d) the estimations of the minimum detectable size of debris and collision probability. The ejecta experiments demonstrated that the ejecta's mass is 7 to 46 times higher than the projectile's mass. For space dust in the range 100μm – 600μm in diameter, the collision probability was calculated to be 16.5 percent. The detector's capabilities to detect broken lines and to transmit the data to the on-board computer were also demonstrated. This in-situ space dust impacts detector is thus a very promising research area for its lightness, low cost and its ability to provide immediate data on space dust population.