The main purpose of this thesis is to improve the fundamental knowledge of non-isothermal tempering of martensite phase and its effects on the reduction in hardness (softening) with respect the base metal occurring at the heat affected zone (HAZ) of resistance spot welded dual-phase (DP) steels. This thesis also aims at understanding the influence of HAZ-softening on the joint performance of various DP steel grades. The tempering of martensite occurring at the sub-critical HAZ (SC-HAZ) of resistance spot welded DP600, DP780 and DP980 steels has been systematically evaluated by microhardness testing through Vickers indentation and the degree of tempering has been correlated to the HAZ-softening. From the joint performance analysis of similar and dissimilar steel grade combinations assessed through standardized testing methods, three important issues have been targeted: a) the joint strength (maximum load to failure), b) the location of failure (failure mode), and c) the physical characteristic of the weld that determines certain type of failure (weld nugget size). In addition, a partial tensile test has been conducted in order to evaluate the initiation of failure in dissimilar steel grade combinations. It has been shown that HAZ-softening lowered the weld size at which transition from interfacial to pullout failure mode takes place along with increased load-bearing capacity and higher energy absorption. Thus, it is concluded from mechanical testing that HAZ-softening benefits the lap-shear tensile joint performance of resistance spot welded DP steels by facilitating pullout failures through failure initiation at the SC-HAZ (tempered region). Instrumented nanoindentation testing was employed to further investigate HAZ-softening along the SC-HAZ by evaluating individual phases of ferrite matrix and tempered martensite islands. Although the ferrite matrix presented a slight reduction in hardness at nanoscale, higher reduction in hardness (softening) resulted for tempered martensite; thus confirming that tempered martensite is the major contributor to softening at micro-scale. A comparison between nanohardness and microhardness testing made at different distances from the line of lower critical temperature of transformation (Ac1) allowed revealing the actual extension of the SC-HAZ. In this regard, good correlation was obtained between nanohardness results along the SC-HAZ and the microstructural changes analyzed by electron microscopy (i.e., the tempering of martensite occurring at various distances far from Ac1 was correlated to low temperature tempering of dual phase steels). An in-depth analysis of the tempering of martensite phase at high temperature in DP steel subjected non-isothermal conditions i.e., rapid heating, extremely short time at peak temperature and rapid cooling (resistance spot welding), has been carried out mainly through analytical transmission electron microscopy (TEM). In addition, an isothermal tempering condition (i.e., slow heating and long time at peak temperature) in DP steel has been evaluated for complementing the analysis. Both non-isothermal and isothermal conditions have been correlated to the softening behaviour. TEM analysis of the base metal in the DP steel indicated that the morphology of the martensite phase is dependent on its carbon content, and its tempering characteristics are similar to that of equal carbon containing martensitic steel. The isothermally tempered structure is characterized by coarsening and spheroidization of cementite (θ) and complete recovery of the martensite laths; whereas precipitation of fine quasi-spherical intralath θ-carbides, coarser plate-like interlath θ-carbides, decomposition of retained austenite into elongated θ-carbides, and partial recovery of the lath structure were observed after non-isothermal tempering of DP steel. This difference in tempering behaviour is attributed to synergistic effect of delay in cementite precipitation due to higher heating rate, and insufficient time for diffusion of carbon that delays the third stage of tempering process (cementite coarsening and recrystalization) during non-isothermal. The finer size and the plate-like morphology of the precipitated carbides along with the partial recovery of the lath structure observed after non-isothermal tempering strongly influenced the softening behaviour of DP steel. The chemical analysis of θ-carbides through extraction replicas for three different DP steels revealed that the chemistry of the carbides is inherited from the parent DP steel during non-isothermal tempering at high temperature confirming that non-isothermal tempering DP steel is predominantly controlled by carbon diffusion.

Diamond-liked carbon (DLC) film is an important material and has many application in industry. Recently doping impurity into the DLC to change the properties of DLC thin film is a research topic attracted scientists. In this thesis, DLC films were deposited by plasma-enhanced chemical vapor deposition (PECVD) on the Si wafer and glass. Acetylene was used as the source of carbon, and nitrogen was doped in DLC need too dopants of grow N2 and NH3. The growth mechanism and differences of the nitrogen doped DLC films were studied by methods of NK measurement, SEM and nano indentation. The analysis of nano indentation showed that the hardness and Young¡¦s Module decreased with increasing N2 flow rate. However, for increased NH3 a flow rate, the hardness and Young¡¦s Module of DLC were increased. The characteristic peaks of nitrogen doped DLC in the FTIR transmittance spectra were studied, sp2 C=H bond(2945 cm-1), sp3 C-H bond(2910 cm-1), and also the C¡ÝN (2200cm-1)and C=N bond(1625cm-1) are observed in DLC. The results of FTIR shows nitrogen was doped into DLC successfully. The DLC thin films thickness was determined by the NK analysis, and it is found the deposition rate of DLC was increased with the increasing flow rate of N2. However, for increased NH3 flow rate, the DLC deposition rate was decreased. From SEM, micrographs the NH3 doped DLC yielded rough morphology. The surface of N2 doped DLC thin film, revealed smoother. A growth mechanism of diamond with different dopant was proposed and explained the properties of DLC thin film with different deposition condition.When N2 was used as dopant source, the N2+ ions were induced by plasma and attracted upward due to the RF self-bias voltage. Therefore ,the surface of thin film was not bombarded due to N2+ ions. On contrast, when the NH3 was used as dopant source, the NH2- ions were produced and distracted downward by the RF self-bias voltage. And then the surface of the thin film was etched by the NH2- ions. Form the XPS analysis, the composition of sp3 C-C(285.4 eV) and sp3 C-N (287.7 eV)were decreased with increased N2 flow rate.However, the composition of sp3 C-C and SP3 C-N were increased with decreasing the NH3 flow rate. The composition of nitrogen in the DLC film increased with higher N2 flow rate. The number of sp2 bond was increased and the hardness was decreased with higher amount of nitrogen in the DLC film. This result is consistent with the nano indentation,FTIR analysis and explained by the ionic transportation growth mechanism model.

Molecular dynamics (MD) simulations are applied to elucidate the anisotropic characteristics in the material responses for crystallographic nickel substrates with (100), (110) and (111) surface orientations during nanoindentation. The strain energy of the substrate exerted by the tip is stored by the formation of the homogeneous nucleation, and is dissipated by the dislocation sliding of the {111} plane. The steep variations of the indentation curve from the local peak to the local minimums are affected by the numbers of slip angle of {111} sliding plane. The pile-up patterns of the three nickel substrates prove that the crystalline nickel materials demonstrate the pile-up phenomenon from nanoindentation on the nanoscale. The three crystallographic nickel substrates exhibit differing amounts of pile-up dislocation spreading at different crystallographic orientations. The effects of surface orientation in material properties of F.C.C. nickel material on the nanoscale are observable through the slip angle numbers of {111} sliding planes which influence hardness values, as well as the cohesive energy of different crystallographic surfaces that indicate Young¡¦s modulus. Furthermore, the multiscale simulations are performed on the (100) monocrystal nickel substrate by using nanoindentation, compensating for MD limitation of a large specimen simulation without significant increase in the size of the problem. This study examines the accuracy of the coupling method for the multiscale model by means of the indentation curve and the deformation profile. Nanoindentation-induced mechanical deformation in GaN thin films prepared by metal-organic chemical-vapor deposition (MOCVD) was investigated using the Berkovich diamond tip in combining with the cross-sectional transmission electron microscopy (XTEM). By using the focused ion beam (FIB) milling to accurately position the cross-section of the indented region, the XTEM results demonstrate that the major plastic deformation was taking place through the propagation of dislocations. The present observations are in support of attributing the pop-ins appeared in the load-displacement curves to the massive dislocation activities occurring underneath the indenter during loading cycle. The absence of indentation-induced new phases might have been due to the stress relaxation via substrate and is also consistent with the fact that no discontinuity was found upon unloading.

La pyrolyse d'un polymère précurseur permet de réaliser des dépôts céramiques. Comparé aux méthodes classiques (CVD, PVD), le principe est simple mais la réalisation pose des problèmes importants. On ne parvient pas à élaborer de cette façon des revêtements d'une épaisseur supérieure à environ 0,5 micromètres non fissurés et adhérents. L'objectif de cette étude est la compréhension des phénomènes de fissuration spontanée lors de la transformation par pyrolyse d'un film mince de polysilazane en céramique « SiCN ».<br />Dans un premier temps, l'analyse du comportement de dépôts pyrolysés sous différentes atmosphères est effectuée avec un dispositif de micro-pyrolyse spécialement développé pour cette étude. Il permet d'observer en microscopie optique la surface du dépôt en continu pendant le traitement thermique. Nous mettons ainsi en évidence plusieurs phénomènes pendant le chauffage. En particulier, nous montrons que la fissuration des dépôts se produit pendant la montée en température, vers 580°C sous azote ou sous argon. Des caractérisations chimiques montrent que, dans ces conditions, les dépôts sont du type SiCNO avec une couche oxydée (SiO2) en surface (épaisseur 100 nm environ).<br />Des modélisations mécaniques issues de la littérature, puis la construction d'un modèle monodimensionnel simple nous permettent de décrire la fissuration et le décollement des dépôts de manière plus quantitative.<br />La dernière partie de ce travail consiste en la détermination des paramètres principaux qui gouvernent cette fissuration. La caractérisation mécanique des dépôts à différents stades de la transformation du précurseur est effectuée par nanodureté. Nous montrons que la fissuration des dépôts coïncide avec un brutal accroissement des propriétés mécaniques du matériau (dureté et module d'Young) entre 550°C et 650°C, couplé à une augmentation importante du retrait à ces températures. Nous en déduisons que la fissuration résulte de la transition polymère/céramique.

In this work the author presents simulation procedures (mathematical models) with the aim to help determining and analysing the mechanical properties of coating-substrate-systems and finding an “optimal” coating structure which should protect the compound from inelastic deformation under a given range of load conditions. Such procedures may be used as a tool to minimise the search field for experimental work. For this purpose one would need a mathematical model which allows one to calculate the complete elastic field with all its displacement and stress components within a multilayer film on a substrate under given mechanical loading and intrinsic stress conditions. Due to copyright restrictions the author is not allowed to publish the Part II of his habilitation thesis at this place. It concerns the references in meta data. / In der Arbeit werden mathematische Modelle zur Berechnung der mechanischen Eigenschaften geschichtet aufgebauter Materialien unter unterschiedlichsten Lastbedingungen (Kontakt- und intrinsische Beanspruchung) vorgestellt und diskutiert. Auf Grund von Schutzrechtsbestimmungen ist eine Veröffentlichung der in der Habilitation angegebenen Literatur im Teil II an dieser Stelle nicht möglich. Der interessierte Leser wird gebeten die Arbeiten in den entsprechenden Journalen einzusehen. Dies betrifft die in den Metadaten angegebenen Veröffentlichungen des Autors.

Diamond and diamond-like carbon films, with their exceptionally good mechanical, chemical, and optical properties, are the best materials as protective hard coatings for electronic devices and cutting tools. The biocompatibility of these materials makes it suitable for bone implants. The wide range applications of these films are hindered because of the high compressive stresses developed during the deposition. Use of carbide and nitride interfacial layers has emerged as one of the methods to reduce the compressive stresses.The present research focuses on the study of different materials as the interfacial layers for diamond and tetrahedral amorphous carbon films. For tetrahedral amorphous carbon AlN, Ta, TiN, TiC, TaN and W were investigated as the interlayer materials. The interlayer was deposited at different substrate temperatures to study the temperature induced changes in the residual stress. The tetrahedral amorphous carbon with TiN interlayer deposited at 300°C and 600°C exhibited a maximum reduction in the stress.TiN and TiC were deposited as interlayer for the diamond films on Ti-6Al-4V alloy. TiC has improved the adhesion of diamond with the substrate and exhibited less compressive stresses compared to TiN.

In this project we studied the formation of nanoripples in calcite and InP single crystals by continuous scanning using the nanoindenter in the ambient environment and by Argon ion irradiation under ultra high vacuum conditions, respectively. Formation of tip induced nanowear ripples is studied on a freshly cleaved calcite single crystal as a function of scanning frequency and contact load of the diamond tip. At lower loads, initiation of the ripples takes place at the bottom of the surface slope at 3 Hz scanning frequency, which continue to propagate as scanning progresses. The orientation of these ripple structures is perpendicular to the scan direction. As the number of scans increases, ripples fully develop, and their height and periodicity increase with the number of scans by merging ripples together. At 6 mu N normal load, tip induced wear occurred as the tip started removing the ripple structures with increased number of scan cycles. As the contact load increased further, a ripple structure was not initiated and only tip induced wear occurred on the surface. At 1 Hz frequency material removal takes place as the tip moves back and forth and material slides towards the scan edges. Material removal rate increased with contact load and it is observed that the number of scans required to create a new surface is inversely proportional to the contact load. Possible mechanisms responsible for the formation of ripples at higher frequencies are attributed to the slope of the surface, piezo hysteresis,system dynamics or a combination of effects. Single crystal calcite hardness of 2.8 GPa and elastic modulus of 80 GPa were measured using nanoindentation. Evolution of nanostructures on the InP surface due to ion bombardment has been studied with scanning tunneling microscopy in UHV environment. InP crystal surfaces were irradiated by Argon ion incident beam with 3 KeV energy at an incident angle of 75 degrees. Self-organization of the surface was studied by varying the ion fluence from 7.7E13 to 4.6E17 ions per square centimeter. The observed nanoripple morphologies have been explained based on the concept of interplay between roughening and smoothing processes. Wavelength of the nanostructures linearly increases with the logarithm of the fluence. The rms roughness is approximately linear with the logarithm of the fluence. Nanoindentation experiments were performed on InP surface before and after ion bombardment to determine variation in hardness and elastic modulus. Surface of irradiated InP has higher H and E values as the surface become amorphized after Ar+ ion bombardment.

The main purpose of this thesis is to improve the fundamental knowledge of non-isothermal tempering of martensite phase and its effects on the reduction in hardness (softening) with respect the base metal occurring at the heat affected zone (HAZ) of resistance spot welded dual-phase (DP) steels. This thesis also aims at understanding the influence of HAZ-softening on the joint performance of various DP steel grades. The tempering of martensite occurring at the sub-critical HAZ (SC-HAZ) of resistance spot welded DP600, DP780 and DP980 steels has been systematically evaluated by microhardness testing through Vickers indentation and the degree of tempering has been correlated to the HAZ-softening. From the joint performance analysis of similar and dissimilar steel grade combinations assessed through standardized testing methods, three important issues have been targeted: a) the joint strength (maximum load to failure), b) the location of failure (failure mode), and c) the physical characteristic of the weld that determines certain type of failure (weld nugget size). In addition, a partial tensile test has been conducted in order to evaluate the initiation of failure in dissimilar steel grade combinations. It has been shown that HAZ-softening lowered the weld size at which transition from interfacial to pullout failure mode takes place along with increased load-bearing capacity and higher energy absorption. Thus, it is concluded from mechanical testing that HAZ-softening benefits the lap-shear tensile joint performance of resistance spot welded DP steels by facilitating pullout failures through failure initiation at the SC-HAZ (tempered region). Instrumented nanoindentation testing was employed to further investigate HAZ-softening along the SC-HAZ by evaluating individual phases of ferrite matrix and tempered martensite islands. Although the ferrite matrix presented a slight reduction in hardness at nanoscale, higher reduction in hardness (softening) resulted for tempered martensite; thus confirming that tempered martensite is the major contributor to softening at micro-scale. A comparison between nanohardness and microhardness testing made at different distances from the line of lower critical temperature of transformation (Ac1) allowed revealing the actual extension of the SC-HAZ. In this regard, good correlation was obtained between nanohardness results along the SC-HAZ and the microstructural changes analyzed by electron microscopy (i.e., the tempering of martensite occurring at various distances far from Ac1 was correlated to low temperature tempering of dual phase steels). An in-depth analysis of the tempering of martensite phase at high temperature in DP steel subjected non-isothermal conditions i.e., rapid heating, extremely short time at peak temperature and rapid cooling (resistance spot welding), has been carried out mainly through analytical transmission electron microscopy (TEM). In addition, an isothermal tempering condition (i.e., slow heating and long time at peak temperature) in DP steel has been evaluated for complementing the analysis. Both non-isothermal and isothermal conditions have been correlated to the softening behaviour. TEM analysis of the base metal in the DP steel indicated that the morphology of the martensite phase is dependent on its carbon content, and its tempering characteristics are similar to that of equal carbon containing martensitic steel. The isothermally tempered structure is characterized by coarsening and spheroidization of cementite (θ) and complete recovery of the martensite laths; whereas precipitation of fine quasi-spherical intralath θ-carbides, coarser plate-like interlath θ-carbides, decomposition of retained austenite into elongated θ-carbides, and partial recovery of the lath structure were observed after non-isothermal tempering of DP steel. This difference in tempering behaviour is attributed to synergistic effect of delay in cementite precipitation due to higher heating rate, and insufficient time for diffusion of carbon that delays the third stage of tempering process (cementite coarsening and recrystalization) during non-isothermal. The finer size and the plate-like morphology of the precipitated carbides along with the partial recovery of the lath structure observed after non-isothermal tempering strongly influenced the softening behaviour of DP steel. The chemical analysis of θ-carbides through extraction replicas for three different DP steels revealed that the chemistry of the carbides is inherited from the parent DP steel during non-isothermal tempering at high temperature confirming that non-isothermal tempering DP steel is predominantly controlled by carbon diffusion.

Recent studies of fcc metals with dense twins (~10 nm spacing) have revealed impressive mechanical properties, along with improved ductility and electrical conductivity in comparison to nanocrystalline metals with similar feature sizes. Many important fcc metals could benefit from these “nanotwinned” microstructures, however, not all fcc metals readily form such twins. The tendency of fcc metals to form twin boundaries is related to the twin boundary energy; those with low twin boundary energy, such as silver (Ag), easily form twins. Increasing twin boundary energy interferes with twin formation, to the point that in metals with high twin boundary energy, like aluminum (Al), twins are quite rare. This thesis focuses on the synthesis of nanotwinned Ag and Al via physical vapor deposition. Nanotwinned Ag is readily fabricated, however, a template approach had to be developed to induce twins in Al. The microstructures and their relationships to observed mechanical properties are also discussed. Grain boundaries interfere with dislocation transmission by posing a slip system discontinuity between grains. Twin boundaries are a special class of grain boundaries in which the grains on either side of the boundary are related by mirror symmetry. Twin boundaries inhibit dislocation transmission, providing strength in the same manner as grain boundaries. However, their symmetrical structure reduces the free volume and grain boundary energy. Accordingly, coherent twin boundaries are often more energetically stable than grain boundaries, and their coherency allows plasticity mechanisms to remain active under conditions where such mechanisms may be inhibited at grain boundaries. Hence, twin boundaries may provide a metal with unique combinations of high strength and good ductility, conductivity, and thermal stability.

Osteoporosis is a disease characterized by reduced bone mass and reduced bone quality. This deterioration manifests itself in osteoporotic fractures at skeletal sites containing large proportions of cancellous bone (ie. forearm, hip, spine). Given the costs associated with these fractures, improvements in our ability to model and predict the behaviour of cancellous bone would be of great financial and social benefit to society. This thesis makes contributions in three areas within the much larger goal of developing a comprehensive model for describing the mechanical behaviour of cancellous bone. Since the accuracy of model predictions can only be as good as the test data against which it is compared, the effect of experimental artifacts introduced by specimen geometry is examined for cored samples. The apparent elastic modulus of cancellous bone is found to be relatively insensitive to specimen (or gauge) length, such that it can be reduced below the recommended 2:1 aspect ratio without introducing detectable artifact. Conversely, apparent modulus is found to be much more sensitive to specimen diameter. The role of water is also examined. Dehydration at room temperature was found to increase the apparent elastic modulus by roughly 14%. This net increase results from the competing effects of an increased tissue modulus and a decreased bone volume fraction due to shrinkage. Finally, preliminary work is presented which attempts to relate micro-CT voxel intensity and locally measured nanoindentation moduli, in order to provide an experimental basis for assigning heterogeneous material properties to finite element method (FEM) models. / Thesis (Ph.D, Mechanical and Materials Engineering) -- Queen's University, 2009-04-24 14:28:17.772