Métallurgie
Surface performances of Ti-6Al-4V substrates coated PVD multilayered filmsin biological environments
Multilayered and nanostructured coatings of Ti based alloys (oxides and nitrides) are elaborated and tested for increasing protective properties such as corrosion and wear resistances. A pin-on-disc tribometer was used to evaluate the wear resistance in Hank's solution against bovine bone. Corrosion behavior in Hank's solution was determined by potentiodynamic and electrochemical impedance spectroscopy techniques. Besides, the specimen surfaces were characterized by Atomic Force Microscopy (AFM), Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) microanalyses. The results showed that optimal tribological properties were obtained in the case of coatings having TiN as top layer. The main wear mechanism was abrasive third bodywear. In vitro corrosion tests at 37 °C showed that the better corrosion resistance was obtained when TiN was the top layer. However all of them exhibited good tribological properties, good corrosion resistance and then may be promising options for biomedical applications. Voir les détails
Mots clés : PVD coatings, oxides, Nitrides, Biomaterials, tribology, corrosion
Effets des éléments (vanadium et niobium) sur la structure et le comportement à la corrosion de l’acier inoxydable austénitique de type AISI309
Les aciers inoxydables austénitiques sont utilisés dans des environnements agressifs couvrant de larges domaines tels que le secteur alimentaire, chimique et nucléaire. Par ailleurs, ils doivent présenter des propriétés d’emploi adéquates et une durée de vie optimale. Ainsi, plusieurs méthodes sont employées afin d’améliorer ces propriétés à savoir l’addition des éléments chimiques, le traitement thermique et le traitement de surface. Cette étude porte sur l'influence de l'addition du vanadium et du niobium sur la variation de la microstructure, l’évolution des propriétés mécaniques et le comportement électrochimique d’un acier inoxydable austénitique de type AISI309. Un traitement de mise en solution a été appliqué sur l’acier inoxydable de base et l’acier inoxydable allié au vanadium et au niobium à une température de 1100°C pendant trois heures suivi d’un refroidissement rapide à l’eau. Ce traitement a été suivi d’un revenu à différentes températures suivi d'un refroidissement à l’air. La caractérisation microstructurale a été effectuée par microscopie optique, MEB, EDS, DRX, DSC. Afin, d’évaluer la résistance à l’usure des matériaux étudiés, une caractérisation mécanique des échantillons étudiés a été réalisée au moyen des mesures de dureté et des essais d’usure par frottement. De plus, pour examiner le comportement à la corrosion, des tests potentiodynamiques et des mesures d’impédances électrochimiques (EIS) ont été réalisés dans deux milieux HCl et H2SO4. L'inhibition à la corrosion de l'acier inoxydable austénitique de type AISI309 avec et sans ajout de vanadium et de niobium par 2,2’-Bipyridyl dans H2SO4 a été étudiée en utilisant la polarisation potentiodynamique (Tafel), la polarisation linéaire (LRP) et la spectroscopie d'impédance électrochimique (SIE). D’après les résultats expérimentaux il a été constaté la présence d’une précipitation des carbures de niobium et de vanadium de type MC (VC, NbC) au détriment d’une précipitation intergranulaire de carbures riches en chrome, ainsi qu’une amélioration des propriétés mécaniques tels que la résistance à l’usure et la dureté suite à l’ajout des éléments d’alliage (vanadium et du niobium) avec et sans traitements thermiques. Par conséquent, l’addition du vanadium et du niobium a contribué à l’amélioration du comportement à la corrosion dans les milieux envisagés ainsi que l’efficacité inhibitrice de l’acier étudié en présence d’inhibiteur (2,2’-Bipyridyl). Voir les détails
Mots clés : AISI309, Cr23C6, Vanadium, niobium, 2, 2'-bipyridyle, corrosion, microstructure, propriétés mécaniques, comportement électrochimique, dureté, usure par frottement
Contribution à la modélisation du processus de refroidissement secondaire d’acier coulée en continue
Dans l’industrie sidérurgique, la coulée continue est le procédé qui se situe entre l’élaboration d’acier et le laminage. Ce procédé a pris, depuis 30 ans, une place de plus en plus importante dans la filière de production en raison des avantages par rapport à la technique traditionnelle de coulée en lingots ; économie d’énergie et de main d’œuvre, meilleur rendement et amélioration de la qualité du produit, ainsi l’amélioration du rendement métallique de la coulée et la possibilité de couler des produits de plus faible section, directement adaptés aux laminoirs finisseurs. La coulée continue permet de transformer le métal liquide en métal solide en des formes simples, et de façon continue. Un des soucis majeurs dans l’industrie de l’acier est l’amélioration de la qualité finale du produit. Certes, le produit final présente parfois des défauts, qui sont difficiles à détecter pendant la fabrication ; la plupart du temps, ils ne sont détectés que dans les phases finales de fabrication. L’objectif de ce travail consiste à fournir un modèle numérique du refroidissement secondaire permettant de prédire l’évolution du débit de refroidissement secondaire en fonction de la vitesse de coulée dans chaque zone des nuances de l’acier. Voir les détails
Mots clés : Modélisation thermomécanique, coulée continue, refroidissement secondaire, acier, Défaut.
Arc Voltage Signals-Based Flicker Effect Analysis Using SampEn Multi-scale Entropy Algorithm
Real-time monitoring in the steel and metallurgical production sector is of great importance. To ensurecompetitiveness, the industrial process will have to innovate and evolve towards better quality. Therefore, the monitoring of the voltage signal in Electric Arc Furnace (EAF) has a vital role in keeping a nominal operation of electrical components in order to achieve high performance. A new monitoring method based on multi-scale Sample Entropy (SampEn) (MSE) algorithm for EAF voltage flicker is proposed. In the proposed method, different percentages of flicker effect analysis are presented. The current voltage characteristic of the EAF in conjunction with MSE and comparison of observed values with those predicted from a Cassie and Mayr model built using nominally healthy data are analysed. In order to achieve the classification procedure, five extracted features are used to adapt the subtractive clustering network for each state of the flicker effect and the performance of the classifier during the training is given with success. Voir les détails
Mots clés : Electric Arc Furnace (EAF), Power quality, Voltage flicker, Voltage unbalance, SampEn Multi-scale entropy algorithm, subtractive clustering
Effect of solution treatment on the microstructure, micromechanical properties, and kinetic parameters of the β → α phase transformation during continuous cooling of Ti-6Al-4V titanium alloy
The aim of this study is to examine the effect of solution treatment temperature (STT) on the microstructure, the micromechanical properties, and the kinetic parameters of the β → α phase transformation during continuous cooling of the dual phase titanium alloy Ti-6Al-4V. Increasing the STT from 1050 °C to 1200 °C delays the formation of the α phase during cooling and increases the value of its activation energy. The microstructural analysis reveals the emergence of αW platelets from protuberances on the αGB / αW interface. The investigation of the morphology of the αW platelets reveals the presence of ledges on their longest side showing a sharp extremity. The micromechanical properties determined by nanoindentation and microhardness tests are almost insensitive to the cooling rate but are strongly affected by the STT; the higher the STT, the lower the overall microhardness of the Ti-6Al-4V alloy. In addition, the STT affects the microhardness and the Young’s modulus of both α and β phases differently; when the STT increases, the microhardness and the Young’s modulus of the α phase decrease whereas those of the β phase increase. Voir les détails
Mots clés : Ti-6Al-4V, solution treatment, ledge mechanism, interface instability, Nanoindentation, partitioning
Isothermal and non-isothermal precipitation kinetics in Al–Mg–Si-(Ag) alloy
In the present work, isothermal and non-isothermal precipitation kinetics in a 6063 aluminium alloy containing a small silver (Ag) addition have been investigated using Vickers microhardness and Differential Scanning Calorimetry (DSC) measurements respectively. Isothermal kinetics analysis showed that β'' phase precipitation obeyed the Johnson-Mehl-Avrami (JMA) model. The DSC analysis revealed that Ag addition modified the precipitation sequence in the investigated 6063 aluminium alloy through the formation of an additional metastable pre-β'' phase. An approach based on the additivity concept has been applied to the heating DSC diagrams to investigate the β'' phase precipitation. The obtained Avrami exponent values from this approach led to suggest that the β'' phase precipitation proceeded through two processes during continuous heating. The Avrami exponent value obtained at the final stage of the transformation was consistent with that obtained from the isothermal analysis, whereas the corresponding activation energy was higher than the one calculated from the isothermal analysis and Kissinger's method. It was also established that the precipitation kinetics of the β'' phase was enhanced by the formation of the precursor phase pre-β''. Voir les détails
Mots clés : 6063 aluminium alloy, Ag addition, Precipitation kinetics, JMA model, Additivity concept
Surface peformances of PVD ZrN coatings in biological environments
Zirconium nitride (ZrN) thin films were deposited by reactive RF magnetron sputtering on Ti-6Al-4V and Si (100) substrates for potential use in biomedical applications. The tribological behaviour was evaluated against bovine bone in dry condition using a pin-on-disc apparatus. Abrasion is the primary wear mechanism observed in ZrN/bone contact. The corrosion properties were determined through two electrochemical techniques: potentiodynamic polarization and electrochemical impedance spectroscopy. The coatings with reduced oxygen content provided: (i) good resistance against corrosion when exposed to physiological solution and (ii) better anti-bioadhesion against Staphylococcus aureus bacteria. Voir les détails
Mots clés : PVD coating, ZrN, wear, corrosion, bioadhesion
ETUDE ÉLECTROCHIMIQUE COMPARATIVE D’UN ALLIAGE (TiNi) ÉLABORÉ, AVEC UN IMPLANT DENTAIRE EN MILIEU SIMULÉ
Good mechanical compatibility with cellular tissue and corrosion resistance, as well as excellent biocompatibility in body fluids, are required for titanium-based alloys to be materials of choice for biomedical applications such as orthopedic implants and dental. The present thesis aims to obtain TiNi binary alloys developed by vacuum induction, as a possible alternative for dental applications. The TiNi alloys developed as part of this thesis work contain Ni contents ranging from 40 to 60%. The choice of this composition was made, first to check the influence of the Ni content on the formation of the structure and the morphology of the phases and secondly the repercussions of this structure on the final properties of the alloy to know; the mechanical properties, tribological and electrochemical and bioactivity. TA6V4 alloy is used for comparison.For this purpose, the chemical composition of the TiNi alloys and the microstructural evolution was determined by scanning electron microscopy (SEM) coupled to the EDS. The formation and growth of the phases was followed by X-ray diffraction. Instrumented hardness measurements were made to assess the hardness and Young's modulus of the alloys. The coefficient of friction of the TiNi alloys and the wear rate were determined by dry sliding at different loads. The electrochemical characterization in Hank's solution and artificial saliva has been studied by stationary techniques and by EIS at different immersion times. The tribocorrosion behavior was performed in artificial saliva to understand the tribocorrosion mechanisms of TiNi and TA6V4 alloys. The bioactivity tests were performed in the SBF solution after 21 days of immersion. The SEM / EDS and RX results show that the two alloys Ti50Ni50 and Ti40Ni60 have a TiNi type matrix (NiTi), and Ti2Ni and Ni2Ti type precipitated phases. The revealed microstructure for the Ti60Ni40 alloy is a Ti2Ni-based matrix comprising the NiTi intermetallic. This same alloy had the lowest Young's modulus, while the Ti40Ni60 alloy had superior superelasticity, than the other titanium alloys (Ti50Ni50, Ti60Ni40 and TA6V4).All TiNi alloys exhibit better tribological behavior compared to the TA6V4 alloy which results in high wear resistance and low wear. Abrasive and adhesive wear mechanisms have been identified as degradation mechanisms for TiNi and TA6V4 alloys, with the predominant adhesive mechanism for TiNi alloys. The Nyquist and Bode impedance diagrams for all TiNi and TA6V4 alloys show capacitive loops with two time constants, indicating that the passive film is formed of two layers namely, a compact passive internal barrier layer and a porous outer layer. The electrochemical study revealed that all alloys have a passive character. The corrosion resistance of the TA6V4 alloy is greater than that exhibited by the various TiNi alloys. TiNi alloys showed hydroxyapatite formation under in vitro bioactivity conditions of SBF. Voir les détails
Mots clés : Titanium alloys, Young module, superelasticity, wear behavior, corrosion resistance, impedance, bioactivity.
Effet de la cinétique de précipitation sur la résistance à la corrosion de l’acier inoxydable duplex 2205 et de l’alliage d’aluminium 2000
This thesis is subdivided into two main parts. First, the influence of the microstructure of the AA2214-T6 aluminum alloy on the morphologies and electrochemical properties of anodic alumina oxide films was investigated. (AAO) formed, and then to see if the heat treatment T4 brought to the AA2214 alloy brought improvements in term of the morphologies of (AAO) and in term of resistance to the corrosion of the anodic alumina oxide films .Secondly, we orientate this work to correlate the pitting potential (Epit) evolution with the kinetics of σ phase precipitation in the 2205 duplex stainless steel aged at 850°C after solution treatment at 1150°C. The potentiodynamic polarization curves indicate a reduction of the pitting corrosion resistance with the aging time, which is revealed by a decrease in the Epit values from 0.65 to 0.40 VSCE. Thus, Epit values are used to determine the kinetics parameters of the σ phase precipitation. The experimental transformed fraction agrees well with the one calculated by using the modified Kolmogorov–Johnson–Mehl–Avrami equation with an impingement parameter c = 0.6. Voir les détails
Mots clés : Kinetics, KJMA, Pitting corrosion, Potentiodynamic polarization, sigma phase precipitation, Aluminum alloy, (AAO) anodic alumina oxide, porous structure, T4, EIS
Risk of Contamination of the Littoral lands by the mill scale in Annaba City-Algeria
A significant amount of scale is produced during casting of ingots and processing of hot-rolled products. In the El Hadjar steel complex, during the various rolling operations, the amount of scale produced is approximately 0.1% of the annual production of the rolling mills. The quality of the thin sheet during rolling is affected by the behavior of the iron oxide layers formed on their surfaces. For this reason, acids and oils are used for the descaling of slabs and billets by means of pressurized water. The calamine, contaminated by these various acids and used oils, is rejected and stored involuntarily on important areas and pollutes soil and groundwater. Micrographic observations as well as x-ray diffraction analysis have shown that calamine consists mainly of iron oxides. Hematite and magnetite become the main components for oxidation times greater than 1 hour. Characterization tests have shown that calamine is dense (ρ = 4.8 g/cm3), its particle size is variable depending on the degree of oxidation (from 0.5 to 10 mm). Simultaneous thermal analysis showed that an increase in mass of the calamine sample with a release of heat. Studies are underway for the physico-chemical characterization of the soils of the storage areas. Voir les détails
Mots clés : Scale, Risks, soil, thermal analysis, granulometry, X-ray diffraction