L'alliage N19 est un superalliage base nickel, élaboré par métallurgie des poudres, qui a été développé récemment en vue d'une application pour disques de turbine aéronautique. L'objectif de cette étude est d'optimiser la microstructure de cet alliage en agissant sur les paramètres de traitements thermiques pour améliorer les propriétés mécaniques de l'alliage. Une bonne compréhension des relations entre les paramètres de traitements thermiques et la microstructure, d'une part, et, des relations entre la microstructure et les propriétés mécaniques, d'autre part, est donc nécessaire. De nombreux traitements thermiques ont été appliqués à l'alliage N19 pour évaluer l'effet de la température de mise en solution, des conditions de refroidissement et de la température de revenu sur la taille de grains, et sur la taille et la distribution des précipités gamma prime. L'observation des microstructures en microscopie électronique à balayage et en transmission a permis d'évaluer l'effet des différentes étapes du traitement thermique sur les caractéristiques microstructurales de l'alliage. L'effet de ces modifications microstructurales sur la vitesse de propagation de fissure en fatigue-fluage à 650°C a été étudié. Les résultats de ces essais de propagation de fissure en fatigue-fluage ont été analysés à l'aide d'essais de comportement en fatigue-relaxation. Une synthèse des différentes propriétés mécaniques de l'alliage en fonction des paramètres de traitements thermiques et des caractéristiques microstructurales a été proposée. / The N19 alloy is a powder metallurgy nickel-based superalloy which has recently been developed for aircraft engine turbine disks. The aim of this study is to optimize the N19 microstructure through the adjustment of the heat treatment parameters in order to enhance the mechanical properties of this alloy. A good understanding of the relationships between the heat treatment parameters and the microstructure, and between the microstructure and the mechanical properties is required. Numerous heat treatments were applied to the alloy to investigate the effect of the solutionizing temperature, the cooling path, and the ageing temperature on the grain size, and on the gamma prime precipitates size and distribution. The observation of the microstructures using scanning electron microscopy and transmission electron microscopy supports the analysis of the heat treatment parameters effects on the microstructural features of the alloy. The effect of the microstructural modifications on the creep fatigue crack growth rate at 650°C was studied. The results of the creep fatigue crack growth tests were analyzed using cyclic stress-relaxation tests. A synthesis of the various mechanical properties of the alloy according to the heat treatment parameters and microstructural features is proposed.

Nanotubular structures from a new family of misfit compounds LnS–TaS₂ with (Ln = La, Ce, Nd, Ho, Er) and LaSe–TaSe₂ (some of them not known hitherto) are reported. Stress relaxation originating from the lattice mismatch between the alternating LnS(Se) and TaS₂(Se) layers, combined with seaming of the dangling bonds in the rim, leads to the formation of a variety of nanotubular structures. Their structures are studied via scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy (STEM) and selected area electron diffraction (SAED). Tubules exhibiting a single folding vector for the LnS(Se) as well as TaS₂(Se) layers were often found. The small values of the c-axis periodicities are indicative of a strong interaction between the two constituent layers which was also supported by Raman spectroscopy and theoretical calculations.

No description available.

The aim of the presented work was to deposit cubic boron nitride thin films by magnetron sputtering under simultaneous stress relaxation by ion implantation. An in situ instrument based on laser deflectometry on cantilever structures and in situ ellipsometry, was used for in situ stress measurements. The characteristic evolution of the instantaneous stress during the layered growth of cBN films observed in IBAD experiments, could be reproduced for magnetron sputter deposition. To achieve simultaneous stress relaxation by ion implantation, a complex bipolar pulsed substrate bias source was constructed. This power supply enables the growth of cBN thin films under low energy ion irradiation (up to 200 eV) and, for the first time, the simultaneous implantation of ions with an energy of up to 8 keV during high voltage pulses. It was demonstrated that the instantaneous stress in cBN thin films can be released down to -1.1 GPa by simultaneous ion bombardment during the high voltage pulses. A simultaneous stress relaxation during growth is possible in the total investigated ion energy range between 2.5 and 8 keV. These are the lowest ion energies reported for the stress relaxation in cBN. Since such a substrate bias power supply is easy to integrate in existing process lines, this result is important for industrial deposition of thin films, not only for cubic boron nitride films. It was found that the amount of stress relaxation depends on the number of atomic displacements (displacements per atom: dpa) that are induced by the high energy ion bombardment and is therefore dependent on the ion energy and the high energy ion flux. In practise, this means that the stress relaxation is controlled by the product of the pulse voltage and the pulse duty cycle or frequency. The cantilever bending measurements were complemented on microscopic scale by x-ray diffraction (XRD). The analysis of the cBN (111) lattice distances revealed a pronounced biaxial compressive state of stress in a non-relaxed cBN film with d(111) being larger in out-of-plane than in in-plane direction. Post deposition annealing at 900 ° C of a sample with an ion induced damage of 1.2 dpa, resulted in a complete relaxation of the lattice with equal in-plane and out-of-plane lattice parameters. In the case of medium-energy ion bombardment, the in-plane and out-of-plane lattice parameters approach the value of the annealed sample with increasing ion damage. This is a clear evidence for stress relaxation within the cBN lattice. The stability of cBN under ion bombardment was investigated by IR spectroscopy and XRD. The crystalline cBN was found to be very stable against ion irradiation. However a short-range ordered, sp3/sp2 - mixed phase may exist in the films, which could be preferably converted to a sp2 -phase at high damage values. From the analysis of the near surface region by XANES, it can be concluded the stress relaxation by the energetic ion bombardment is less at the surface than in the bulk film. This is explained with the dynamic profile of the ion induced damage, that reaches the stationary bulk value in 15-20 nm depth, whereas it is decreasing towards the surface. This fits with the results that the stress relaxation is dependent on the amount of ion induced damage. Comparing the results from substrate curvature measurement, XRD, XANES, and IR spectroscopy possible mechanisms of stress relaxation are discussed. Concluding the results, it can be stated that using simultaneous ion implantation for stress relaxation during the deposition it is possible to produce BN films with a high amount of the cubic phase and with very low residual stress.

No description available.

[pt] Neste trabalho é feito um estudo experimental da relaxação de uma fibra sintética de alta resistência, conhecida como Kevlar 49, empregada na fabricação de cabos que podem ser usados como cabos de protensão. O objetivo é obter uma equação para o cálculo da relaxação e verificar a influência de um condicionamento mecânico (aplicação e remoção de uma tensão). Foram realizados ensaios em seis amostras da fibra sob cinco níveis de tensão, equivalentes a 10%, 20%, 30%, 40% e 50% da tensão de ruptura do material. Os ensaios foram realizados com a temperatura e umidade relativa do ar controlados na faixa de 21oC + 2oC e 77% + 7% respectivamente. O tempo de duração de cada ensaio foi de 72 horas. Os resultados revelaram que as curvas de relaxação são lineares quando plotadas numa escala logarítmica do tempo e que o coeficiente de relaxação é bem representado por uma função potencial e depende da tensão aplicada. Em adição revelaram que um condicionamento mecânico não altera o comportamento da fibra. / [en] High-strength aramid fibers have been used in the production of a variety of cables and ropes which have found several applications as structural members in bridges and other types of structures. For such applications, a sound knowledge of the time dependent material properties is highly important. An experimental investigation on the stress relaxation behavior of a high-strength aramid fiber was carried out, with the purpose of studying the viscoelastic properties of the material and the effect of a mechanical conditioning (application and removal of stress prior to testing) on these properties. The fiber used in this investigation is commercially known as Kevlar 49. The tests were conducted at five different stress levels, at constant temperature and moisture. The results showed that the fiber has a non-linear viscoelastic behavior and that the effect of the mechanical conditioning isn´t important. An equation for the prediction of the stress relaxation is presented. / [es] En este trabajo se realiza un estudio experimental de la relajamiento de una fibra sintética de alta resistencia, conocida como Kevlar 49, empleada en la fabricación de cables que pueden ser usados como cables de protensión. El objetivo es obtener una ecuación para el cálculo dela relajamiento y verificar la influencia de un condicionamento mecánico. Fueron realizados ensayos en seis muestras de la fibra bajo cinco niveles de tensión, equivalentes a 10%, 20%, 30%, 40% y 50% de la tensión de ruptura del material. Los ensayos fueron realizados con la temperatura y la humedad relativa del aire controlados en la faja de 21oC + 2oC y 77% + 7% respectivamente. El tiempo de duración de cada ensayo fue de 72 horas. Los resultados revelaron que las curvas de relajamiento son lineales cuando se utiliza una escala logarítmica para el tiempo y que el coeficiente de relajamiento está bien representado por una función potencial, que depende de la tensión aplicada. Adicionalmente, los ensayos revelaron que un condicionamento mecánico no altera el comportamiento de la fibra.

The damage development and strength of ply-level scaled carbon/epoxy composite laminates having stacking sequence of [+Tn/-Tn/902n]s where constraint ply angle, T, was 0, 15, 30, 45, 60, and 75 degrees, and size was scaled as n=1,2,3, and 4, is reported in Part I. X-radiography was used to monitor damage developments. First-ply failure stress, and tensile strength were recorded. First-ply failure of the midplane 90 deg. plies depended on the stiffness of constraint plies, and size. All 24 cases were predicted using Zhang's shear-lag model and data generated from cross-ply tests. Laminate strength was controlled by the initiation of a triangular-shaped local delamination of the surface angle plies. This delamination was predicted using O'Brien's strain energy release rate model for delamination of surface angle plies. For each ply angle, the smallest laminate was used to predict delamination (and strength) of the other sizes. The in-situ tensile strength of the 0 deg. plies within different cross-ply, and quasi-isotropic laminates of varying size and stacking sequence is reported in Part II. No size effect was observed in the strength of 0 deg. plies for those lay-ups having failure confined to the gauge section. Laminates exhibiting a size-strength relationship, had grip region failures for the larger sizes. A statistically significant set of 3-point bend tests of unidirectional beams were used to provide parameters for a Weibull model, to re-examine relationship between ultimate strength of 0 deg. plies and specimen volume. The maximum stress in the 0 deg. plies in bending, and the tensile strength of the 0 deg. plies (from valid tests only) was the same. Weibull theory predicted loss of strength which was not observed in the experiments. An effort to model the durability and life of quasi-isotropic E-glass/913 epoxy composite laminates under steady load and in an acidic environment is reported in Part III. Stress-rupture tests of unidirectional coupons immersed in a weak hydrochloric acid solution was conducted to determine their stress-life response. Creep tests were conducted on unidirectional coupons parallel and transverse to the fibers, and on ±45°. layups to characterize the lamina stress- and time-dependent compliances. These data were used in a composite stress-rupture life model, based on the critical element modeling philosophy of Reifsnider, to predict the life of two ply-level thickness-scaled quasi-isotropic laminates. / Ph. D.

Die vorliegende Arbeit verfolgt das Ziel, Cu(Ag)-Dünnschichten als potentiellen Werkstoff für Leiterbahnen in der Mikroelektronik zu untersuchen. Für die Beurteilung dieses Materialsystems wurden vier Schwerpunkte bezüglich der Schichtcharakterisierung definiert: Herstellung, Gefüge, thermomechanische Eigenschaften, Elektromigrationsresistenz. Grundlage sämtlicher Untersuchungen ist eine geeignete Probenpräparation. In Anlehnung an Technologien, die zur Zeit bei der Herstellung von reinen Cu-Leiterbahnen Anwendung finden, erfolgte die Beschichtung der Cu(Ag)-Schichten (Dicke bis 1 µm) galvanisch aus einem schwefelsauren Elektrolyten unter Additiveinsatz auf thermisch oxidierten Siliziumwafern. Hierbei war nicht nur die Abscheidung von ganzflächigen Dünnschichten, sondern auch die Beschichtung auf strukturierte Substrate von Interesse. Die erzeugten Schichtproben werden in ihren Gefügeeigenschaften, vergleichend zu reinen Kupferschichten, charakterisiert. Hierzu zählen Korngrößen und -orientierungen, thermisches Gefügeverhalten, Einbau, Verteilung und Segregation von Silber und Fremdstoffen sowie die elektrischen Eigenschaften. Von grundsätzlicher Bedeutung für das Elektromigrationsverhalten und damit für die Zuverlässigkeit und das Leistungsvermögen sind die thermomechanischen Eigenschaften. Diese werden an ausgedehnten Schichten mit der Substratkrümmungsmessung bis zu Temperaturen von 500°C beschrieben. Die Diskussion des mechanischen Schichtverhaltens umfasst sowohl thermische als auch temporale Charakteristika. Die Untersuchungen geben einen Einblick in die wirkenden Mechanismen des Stofftransports und des Spannungsabbaus. Den Abschluss der Arbeit stellen erste Experimente zum Elektromigrationsverhalten der Cu(Ag)-Dünnschichten dar. Den Kern dieser Analysen bilden Messungen an sog. Blech-Strukturen (Materialdriftexperimente). Hierbei werden geeignete Technologien für die mikrotechnologische Herstellung von derartigen Cu(Ag)-Strukturen vorgestellt. Anhand erster Messungen wird das Elektromigrationsverhalten von Cu(Ag)-Metallisierungen in seinen Grundcharakteristika beschrieben.

No description available.

Die vorliegende Arbeit verfolgt das Ziel, Cu(Ag)-Dünnschichten als potentiellen Werkstoff für Leiterbahnen in der Mikroelektronik zu untersuchen. Für die Beurteilung dieses Materialsystems wurden vier Schwerpunkte bezüglich der Schichtcharakterisierung definiert: Herstellung, Gefüge, thermomechanische Eigenschaften, Elektromigrationsresistenz. Grundlage sämtlicher Untersuchungen ist eine geeignete Probenpräparation. In Anlehnung an Technologien, die zur Zeit bei der Herstellung von reinen Cu-Leiterbahnen Anwendung finden, erfolgte die Beschichtung der Cu(Ag)-Schichten (Dicke bis 1 µm) galvanisch aus einem schwefelsauren Elektrolyten unter Additiveinsatz auf thermisch oxidierten Siliziumwafern. Hierbei war nicht nur die Abscheidung von ganzflächigen Dünnschichten, sondern auch die Beschichtung auf strukturierte Substrate von Interesse. Die erzeugten Schichtproben werden in ihren Gefügeeigenschaften, vergleichend zu reinen Kupferschichten, charakterisiert. Hierzu zählen Korngrößen und -orientierungen, thermisches Gefügeverhalten, Einbau, Verteilung und Segregation von Silber und Fremdstoffen sowie die elektrischen Eigenschaften. Von grundsätzlicher Bedeutung für das Elektromigrationsverhalten und damit für die Zuverlässigkeit und das Leistungsvermögen sind die thermomechanischen Eigenschaften. Diese werden an ausgedehnten Schichten mit der Substratkrümmungsmessung bis zu Temperaturen von 500°C beschrieben. Die Diskussion des mechanischen Schichtverhaltens umfasst sowohl thermische als auch temporale Charakteristika. Die Untersuchungen geben einen Einblick in die wirkenden Mechanismen des Stofftransports und des Spannungsabbaus. Den Abschluss der Arbeit stellen erste Experimente zum Elektromigrationsverhalten der Cu(Ag)-Dünnschichten dar. Den Kern dieser Analysen bilden Messungen an sog. Blech-Strukturen (Materialdriftexperimente). Hierbei werden geeignete Technologien für die mikrotechnologische Herstellung von derartigen Cu(Ag)-Strukturen vorgestellt. Anhand erster Messungen wird das Elektromigrationsverhalten von Cu(Ag)-Metallisierungen in seinen Grundcharakteristika beschrieben.