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High temperature polyarylene networks produced through the step-growth thermal cyclopolymerization of mono-ortho-diynylarene (MODA) and bis-ortho-diynylarene (BODA) monomers have been shown to produce high yielding glassy carbon once pyrolyzed at 1000 °C. In this study the homo- and co-polymerization of both monomers will be studied, and the effects of copolymer composition on the processability when applied to carbonization and carbon-carbon composites. The carbon products from these high temperature polymer matrices will also be characterized. MODA and BODA are prepared through a Sonogashira coupling reaction and are polymerized through a heat-initiated Bergman Cyclization reaction mechanism. This work seeks to show how BODA-MODA copolymers can attenuate current composite processing limitations, and improve mechanical properties while retaining high temperature properties including high carbon yields.

Carbon/Carbon (C/C) composite is defined as a carbon fiber reinforced carbon matrix. Since 1958 research has been carried out on the C/C composites. The main reason for the development of new C/C composites is the number of advantages it has to offer when compared with the regular materials. The areas where C/C composites are being used extensively are aerospace, military, etc. These C/C composites have better physical, mechanical, thermal properties when compared to steel. That is the reason C/C brakes made a huge impact in the aerospace industry. The main drawback associated with the C/C brakes which are used in aerospace applications is the oxidation of the composite at higher temperatures. Also other problem linked with the C/C brake is the migration of the inhibitors on to the friction surface of the brake which can eventually decrease the friction coefficient of the brake material. So, characterizing the commercially available Anti-Oxidant(A/O) system, developing a new A/O system which can not only provide better oxidation protection, but also an improved anti-oxidant migration resistance will be our main goal of this project.

Circular air-coupled ultrasonic testing (ACUT) setup for the inspection of commercial carbon-carbon composite aircraft brake disks was developed in Intelligent Measurement and Evaluation Laboratory (IMEL) at Southern Illinois University Carbondale (SIUC). The developed test setup utilizes Airstar single channel air-coupled equipment and has only manual A-scan and B-scan capability. The developed ACUT technique is unique compared to the commercial C-scan ultrasonic systems and is proficient, fast, economically feasible, and easy to implement method particularly for the inspection of carbon-carbon (C/C) composites aircraft brake disks. Prior to conducting air-coupled measurements, wobble analysis was carried out. This was important because significant wobbling in the test setup can lead to the interference of the reflected and the incident beam which would result to inaccurate ultrasonic measurements. The measured deviation due to wobbling, surface profile of the disk, design, and experimental error were relatively small. Therefore, these errors were neglected while performing ACUT measurements. For ACUT measurements, several through-transmitted amplitude signals were recorded within the C/C brake disks manually. The images were then reconstructed using Matlab based on the through-transmitted amplitude signals. Finally, a comparison was drawn between the reconstructed images and the C-scan images of the C/C brake disks obtained from the commercial Airstar C-scan ACUT system. Like commercial C-scan ACUT image results, reconstructed images were also able to detect all defects in the commercial C/C brake disks which served for the system verification and validation. In addition, defect, non-defect, and suspected areas within the C/C brake disks were quantified with air-coupled measurement. For this, light microscopy was conducted for every sample made from each C/C brake disks at lower magnification of 10X. It was concluded that it is very difficult to assess the crack or delamination situation based on a 2D micrograph of one depth. Also, it was concluded that an internal porosity and micro-cracks may not be only factors that can be related to defects. Finally, an intelligent systems approach, specifically, fuzzy logic and artificial neural network (ANN) methodologies were implemented for the automatic defect detection in commercial C/C aircraft brake disks by using air-coupled ultrasonic results. For this, a multi-layer perceptron (MLP) with two hidden layers and a scaled conjugate gradient back-propagation (BP) learning algorithm was used for the ANN training. The network training process was performed in an off-line mode using the ANN toolbox in Matlab. The network training was repeated until a steady state was reached, where there was no further change in the synaptic weights. The ANN provided plausible results in detecting the defect areas for different C/C brake disks. It was also demonstrated that the system was able to learn the rules without knowing any algorithm for automatic defect detection.

In recent times, composite materials have gained mainstay acceptance as a structural material of choice due to their tailorability and improved thermal, specific strength/stiffness and durability performance. Carbon-Carbon (C/C) composites are used for high temperature applications such as exit nozzles for rockets, leading edges for missiles, nose cones, brake pads etc. Mechanical property estimation of C/C composites is challenging due to their highly heterogeneous microstructure. Computed Tomography (CT) images (volumetric imaging) coupled with Scanning Electron Microscopy (SEM) reveal a highly heterogeneous microstructure comprised of woven C-fibers, amorphous C-matrix, irregularly shaped voids, cracks and other inclusions. The images also disclose structural hierarchy of the C/C composite at different length scales. Predicting the mechanical behavior of such complex hierarchical materials like C/C composites forms the motivation for the present work. A systematic study to predict the effective mechanical properties of C/C Composite using numerical homogenization has been undertaken in this work. The Micro-Meso-Macro (MMM) principle of ensemble averages for estimating the effective properties of the composite has been adopted. The hierarchical length scales in C/C composites has been identified as micro (single fiber with matrix), meso (fabric) and macro (laminate). Numerical homogenization along with periodic boundary conditions (PBCs) have been used to estimate the effective engineering properties of the material at different length scales. Concurrently, mechanical testing has also been carried out at macro (compression tests) and micro scale (using nano-indentation studies) to characterize the mechanical behavior of C/C composites.

<p dir="ltr">Fretting wear occurs when two contacting bodies under load are subjected to small amplitude oscillatory motion. Depending on the applied normal load, displacement amplitude, coefficient of friction and resulting shear force, two types of fretting wear regimes exist – (i) partial slip and (ii) gross slip. At displacement amplitudes higher than gross slip condition, sliding wear regime prevails. Fretting wear becomes dominant in machine components subject to vibrations such as bearings, dovetail joints, etc. whereas sliding wear is observed in brakes, piston-ring applications, etc. The work in this dissertation primarily focuses on characterizing the material response of various machine components subjected to fretting and sliding wear regimes.</p><p dir="ltr">At first, the friction and fretting wear behavior of inlet ring and spring clip components used in land-based gas turbines was investigated at elevated (<a href="" target="_blank">500°C</a>) temperature. In order to achieve this objective, a novel high-temperature fretting wear apparatus was designed and developed to simulate the conditions existing in a gas turbine. The test apparatus was used to investigate fretting wear of atmospheric plasma sprayed (APS) Cr₃C₂-NiCr (25% wt.), high-velocity oxy-fuel (HVOF) sprayed Cr₃C₂-NiCr (25% wt.), HVOF sprayed T-800 and APS sprayed PS400 coated inlet rings against HVOF-sprayed Cr₃C₂-NiCr (25% wt.) coated spring clip. The PS400 coated inlet rings demonstrated a significant reduction in friction and wear. A finite element (FE) framework was also developed to simulate fretting wear in HVOF-sprayed Cr₃C₂-NiCr composite cermet coating. The material microstructure was modelled using Voronoi tessellations with a log-normal distribution of grain size. Moreover, the individual material phases in the coating were randomly assigned to resemble the microstructure from an actual SEM micrograph. A damage mechanics based cohesive zone model with grain deletion algorithm was used to simulate debonding of the ceramic carbide phase from the matrix and resulting degradation from repeated fretting cycles. The specific wear rate obtained from the model for the existing material microstructure was benchmarked against experiments. Novel material microstructures were also modeled and demonstrated to show less scatter in wear rate.</p><p dir="ltr">Following, a three-dimensional (3D) continuum damage mechanics (CDM) FE model was developed to investigate the effects of fretting wear on rolling contact fatigue (RCF) of bearing steels. In order to determine the fretting scar geometry, a 3D arbitrary Lagrangian-Eulerian (ALE) adaptive mesh (AM) FE model was developed to simulate fretting wear between two elastic bodies for different initially pristine fretting pressures (0.5, 0.75 and 1 GPa) and friction coefficients (0.15, 0.175 and 0.25) resulting in stick zone to contact width ratios, c/a = 0.35, 0.55 and 0.75. The resulting wear profiles were subjected to various initially pristine RCF pressures (1, 2.2 and 3.4 GPa). The pressure profiles for RCF were determined by moving the contact over the fretted wear profiles in 21 steps. These pressure profiles were then used in the CDM-FE model to predict the RCF life of fretted surfaces. The results indicate that increased fretting pressure leads to more wear on the surface, thereby reducing RCF life. As the RCF pressure increases (P_RCF ≥ 2.2 GPa), the effect of fretting on RCF life decreases for all fretting pressures and c/a values, indicating that life is primarily governed by the RCF pressure. The results from CDM-FE model were used to develop a life equation for evaluating the L₁₀ life of fretted M-50 bearing steel for the range of tested conditions.</p><p dir="ltr">Lastly, the sliding wear characteristics of pitch and poly-acrylonitrile based carbon-carbon (C/C) composites were investigated in air and nitrogen environment by designing and developing a disc brake test rig. It was found that the temperature of the disc, the surrounding environment, the supplied energy flux as well as the type of composite play a critical role in determining whether C/C composites operate in normal wear or dusting wear regime. Further analysis of wear mechanisms revealed interface and matrix cracking with fiber breakage from tests in air environment, whereas in nitrogen environment, particulate and layered debris played a prominent role.</p>

Les composites carbone/carbone présentent de propriétés thermomécaniques à hautes températures qui les rendent particulièrement adaptés à l’ablation ou à la friction. Leur sensibilité à l’oxydation dès 400°C a conduit à envisager leur dopage en éléments réfractaires inoxydables ou à température d’oxydation élevée. Le procédé sol-gel a permis d’introduire environ 1 % volumique d’oxyde ou de nitrure de titane ou d’aluminium dans leur matrice. Les nitrures sont obtenus par nitruration carbothermique des films d’oxydes. Deux types de sols ont été utilisés : des sols « standard » et des sols enrichis en saccharose. Le saccharose est ajouté pour prévenir la consommation du pyrocarbone lors de la nitruration. Il a par ailleurs une influence sur l’avancement de la nitruration. Les composites chargés sont ensuite densifiés par voie gazeuse, ce qui induit des transformations de phases prévues par la thermodynamique : les films de nitrure de titane sont partiellement carburés (formation de carbonitrure), et les films d’oxyde de titane sont réduits (formation d’oxycarbure). Les dépôts à base d’aluminium sont plus stables et ne subissent aucune transformation. La diffusivité thermique des composites réalisés est faiblement impactée par les charges introduites, alors que les résistances en traction/compression sont sensiblement augmentées. Par ailleurs, une rigidification des composites est observée. Leur cinétique d’oxydation est ralentie. Les composites enrichis en alumine et nitrure d’aluminium présentent des vitesses de perte de masse divisées par 2 par rapport à la référence C/C. Toutes ces propriétés sont liées directement ou non à la composition des sols, et plus particulièrement à sa teneur en saccharose. Il a en effet été montré que les sols qui en contiennent ont tendance à gélifier en surface du composite, ce qui gêne la diffusion des gaz précurseurs au cœur du composite lors de la densification. La porosité finale s’en trouve modifiée. Cette dernière a une influence non négligeable sur le comportement en compression, la diffusivité thermique et la cinétique d’oxydation des composites élaborés. / Carbon/carbon composites exhibit excellent mechanical and thermal properties at high temperature that make them espe-cially suitable for ablation or friction pieces. Their sensitivity toward oxidation above 400°C has lead to the will of doping them with refractory ceramics that are nonoxidizable or with a high oxidation temperature. The sol-gel process allowed to introduce 1 % in volume of titanium or aluminum oxide or nitride in the matrix. Nitrides are obtained by carbothermal nitridation of the oxide films. Two types of sols were used: the “standard” ones and those with extra sucrose. Sucrose is added to prevent pyrocarbon consumption during the nitridation. Furthermore, it was shown that it has an impact on the nitridation rate. Charged composites are then densified by Chemical Vapor Infiltration, which induces phases transforma-tions that were predicted by thermodynamics: titanium nitride films are partially carburized (formation of titanium carbonitride) and titanium dioxide films are reduced (formation of titanium oxycarbide). Aluminum-based films are more stable and don’t undergo any transformation. Thermal diffusivity of the as-synthesized composites is not much modified by the addition of these ceramics while the tensile and compressive strength are slightly increased. By the way, composites are hardened. Their oxidation kinetics is slowed down. Aluminum-rich composites exhibit a weight loss divided by two compared to the C/C reference. All those properties are directly, or not, linked to the composition of the sols, in particular to their sucrose content. Indeed, it was shown that sucrose-containing sols rather jellify on the surface of the composite, thus preventing the diffusion of precursor gases to the heart of the pieces. The final porosity is then modified. The porosity has an important impact on the compressive strength, thermal diffusivity and oxidation kinetics of the synthesized composites.