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The focus of this research was to investigate the use of functionalized/non-functionalized multi walled carbon nanotubes (MWCNTs) as reinforcements for the Portland cement paste. The unique geometrical characteristics of the carbon nanotubes (CNTs), as well as its unique mechanical properties such as high strength, ductility and stiffness, were the vital motivation for this study. In this research, we combined this unique material (CNTs) with concrete which is the most used man-made material. When compared to other composite materials, a limited amount of research has been conducted on the CNTs/cement composites. In order to investigate how the aspect ratio of functionalized/non-functionalized MWCNTs affects the mechanical properties of cementitious composites, ten different mixes of the MWCNTs/cement composites were prepared and tested. The different batches had a fixed water/cement ratio of 0.4, and variations of MWCNTs length, concentration and surface treatment. The cement nanocomposites were cast in small-scale specimens (beams) for the three-point flexural testing. Four major mechanical properties were evaluated at ages of 7, 14, and 28 days from the casting day: the maximum flexural strength, ultimate strain capacity (ductility), modulus of elasticity, and modulus of toughness. The results for the different nanocomposite batches were compared with the plain cement (reference) batch. The mechanical testing results showed that at 28 days almost all of the MWCNTs composites increased the flexural strength of the cement nanocomposites. At 28 days, the long MWCNTs increased the flexural strength more than the short MWCNTs. In general, the ultimate strain (ductility) of the short MWCNTs nanocomposites was higher than the ultimate strain of the long MWCNTs nanocomposites. The flexural strength of short 0.2 percent MWNT and long 0.04 percent MWNT (OH) increased by 269 percent and 83 percent, respectively, compared to the plain cement sample at 28 days. The highest ductility at 28 days for the short 0.1 percent MWNT and the short 0.2 percent MWNT was 86 percent and 81 percent, respectively. Clear evidence was obtained from the SEM images for micro-crack bridging; many of the MWCNTs were stretching across the micro-cracks. In conclusion, CNTs as nano reinforcements, can effectively improve certain mechanical properties of the cement paste composites.

This study reports a novel and simple technique for successfully coating multi-walled carbon nanotubes (MWCNTs) on to the surface of carbon fibre (CF) fabric for the production of multi-scale CF-epoxy composites. Initially, epoxy composites with multi-scale reinforcement were produced by resin infusion (RI) using woven CF fabric coated with a dispersion of 1 wt. % MWCNTs in an epoxy binder of low molar mass. The effects of this reinforcement on the CF-epoxy interface with MWCNTs was studied in mode I and mode II interlaminar fracture toughness (ILFT) using double-cantilever beam (DCB) and 4 point end-notch flexure (4ENF) tests, respectively. Relative to an equivalent composite reinforced with non-coated CF reinforcement, the binder/MWCNTs coating increased significantly the ILFT of the CF-epoxy composite; in mode I by 105% and in mode II by 50%. This increase in ILFT was attributed to two main effects: Firstly, the binder alone (without MWCNTs), which has a much lower glass transition temperature (Tg) than that the matrix (45 vs. 140 °C), hindered crack propagation and increased the ILFT of the epoxy matrix by 25% for mode I and 15% for mode II; Secondly, the energy absorbing mechanisms of MWCNTs during fracture particularly pull-out and crack bridging. However the Tg of the matrix epoxy of the multi-scale composites was reduced to 118 °C compared to 140 °C, for the unmodified composite, due to phase mixing with the low Tg binder. For RI processing, the CF volume fraction of the composites prepared using coated CF was ≈50% compare to at ≈55% for the composite with non-coated CF. Curing agents were added to the binder, which not only increased the Tg from ≈50 °C to ≈100 °C, but also increased the Tg of the matrix epoxy of the multi-scale composites to 154 °C. Relative to an equivalent composite reinforced with non-coated CF reinforcement, the curable-binder/MWCNTs coating increased the ILFT of the CF-epoxy composite; in mode I by 120% and in mode II by 90%. A hybrid RI-hot press (HP) process was used to prepare CF-epoxy composites from coated fabrics with CF volume fractions of ≈55%. The damping curves for the HP-composites consisted of a β-peak, due to the formation of a third mixed phase, in addition to a γ-peak (assigned to the Tg of the binder) and an α-peak (assigned to the Tg of matrix epoxy). The β-peak, and the uniformly distributed nodular particles observed on the fracture surface of the matrix, by SEM, for HP-composites, are indicative of the formation of mixed-phase particles due to reaction induced phase separation (RIPS). Relative to an equivalent RI-composite, the curable-binder/MWCNTs treatment increased the ILFT of the CF-epoxy multi-scale composite; in mode I by 134% and in mode II by 15% for HP-composites. Impact test results showed that HP-composites absorbed more energy, due to CF fracture, compared to equivalent RI composites, which showed larger delamination areas after 5 J and 10 J impact. The out-of-plane electrical conductivity and thermal conductivity of the HP-composite with CF coated with curable-binder/MWCNTs was increased by ≈38% and ≈50%, respectively, compared to the composite with non-coated CF, indicating formation of MWCNTs networks in the matrix rich areas of the multi-scale composite.

Growth confinement techniques for multi walled carbon nanotubes on Au/SiO2 surfaces was studied and incorporated into a gas sensor design. A device framework was conceived and a sensor was built to achieve this structure. The fabrication results were analyzed using scanning electron microscopy which confirmed the achievement of highly site-selective growth of carbon nanotubes, exclusively between the interdigitated electrodes. The sensor was then evaluated for its capacitance and conductance response when exposed to NO2 gas. Variation in sensitivities with frequency and flow rate were analyzed. A mathematical model was derived for such a device structure and the predictions of the model were compared with experimental results.

L’utilisation des combustibles fossiles (énergies non renouvelables) est responsable de l’augmentation de la concentration en gaz à effet de serre dans l’atmosphère. Parmi les solutions de remplacement envisagées, l’hydrogène apparaît comme le vecteur énergétique le plus séduisant. Son stockage dans des intermétalliques permet d’obtenir des capacités massiques et volumiques (e.g. 140 g/L) supérieures à celles obtenues en voie liquide ou sous pression (respectivement 71 et 40 g/L). Dans les accumulateurs Nickel-Métal Hydrure (Ni-MH), l’électrode négative est constituée d’un composé intermétallique qui absorbe l’hydrogène de façon réversible dans des conditions normales de pression et de température. Ce travail de thèse vise d’une part, à synthétiser les alliages Mg2Ni1-xMnx (x =0, 0.125, 0.25, 0.375) et les alliages Mg2-xAlxNi (x = 0, 0.25) avec ou sans nanotubes de carbone (MWCNTs) par mécanosynthèse et d’autre part, d’étudier les effets des substitutions/additions sur la composition et la microstructure des alliages Mg2Ni afin d’améliorer leurs propriétés de stockage d’hydrogène.Les résultats obtenus montrent que les capacités de décharge des alliages Mg2Ni1-xMnx(x = 0, 0.125, 0.25, 0.375) augmentent avec le temps de broyage. Pour l’alliage Mg2Ni0.625Mn0.375 broyé durant 48 h, nous avons mis en évidence la formation d’une nouvelle phase Mg3MnNi2 qui est relativement stable. Par conséquent, Mg3MnNi2 est capable d’améliorer de manière significative la stabilité des cycles tout en maintenant une capacité de décharge relativement élevée.Les résultats obtenus par la théorie de la fonctionnelle de la densité (DFT) en utilisant le programme CASTEP montrent d’une part, que les paramètres de maille et les coordinations atomiques sont en parfait accord avec les résultats expérimentaux. D’autre part, que la stabilité des phases décroit graduellement selon l’ordre suivant : Mg2Ni sans aucune substitution >Mg3MnNi2 > Mg2Ni avec substitution par Mn.L’addition de nanotubes de carbone et de Al ont des effets synergétiques sur la capacité de stockage d’hydrogène électrochimique dans le cas des alliages Mg2-xAlxNi (x = 0, 0.25) + 5 wt.% MWCNTs. / The use of fossil fuels (non-renewable energy) is responsible for increasing the concentration of greenhouse gases in the atmosphere. Among the considered alternatives, hydrogen is seen as the most attractive energy vector. The storage in intermetallics makes it possible to obtain mass and volume capacities (e.g. 140 g/L) higher than those obtained by liquid form or under pressure (respectively 71 and 40 g/L). The negative electrode of Nickel-Metal Hydride (NiMH) batteries, is constituted by an intermetallic compound which is able to reversibly absorb hydrogen under normal conditions. In this work, on the one hand, Mg2Ni1-xMnx(x=0, 0.125, 0.25, 0.375) and Mg2-xAlxNi (x = 0, 0.25) electrode alloys with and without multiwalled carbon nanotubes (MWCNTs) have been prepared by Mechanical Alloying. On the other hand, influence of the partial elements substitution on the microstructure and electrochemical hydrogen storage properties of Mg2Ni-type alloy has been studied.The results show that the discharge capacities of Mg2Ni1-xMnx (x =0, 0.125, 0.25, 0.375) alloys increase with the prolongation of milling time. The new phase Mg3MnNi2 is formed only when x=0.375 after 48 h of milling. Mg3MnNi2 phase is relatively stable during charge/discharge cycles and therefore can significantly enhance the cycle stability under simultaneously maintaining a high discharge capacity.Based on the calculated results of first principles, the lattice parameters and atomic coordinates are in good agreement with the experimental results and the stability of phases gradually decreases along the sequence pure Mg2Ni phase > Mg3MnNi2 phase > Mn-substitution doped Mg2Ni phase.When Al and MWCNTs are added simultaneously, the highest discharge capacity is obtained for Mg1.75Al0.25Ni-MWCNTs composite, which implies that MWCNTs and Al have synergistic effects on electrochemical hydrogen storage capacity of milled alloys.

The focus of this dissertation is to utilize chemical functionalization as a probe to investigate the reactivity of N-doped multiwalled carbon nanotubes (N-MWCNTs). The surface of N-MWCNTs, being a set of potentially reactive graphene edges, provides a large number of reactive sites for chemical modification, so considerable changes in chemical and physical properties can be envisaged. We observed that both reduction (dissolving metal reduction/alkylation) and oxidation (H2SO4/HNO3 and H2SO4/KMnO4 mixtures) of N-MWCNTs lead to formation of interesting spiral channels and spiraled carbon nanoribbons. A variety of techniques, including TGA, SEM, TEM, XRD and surface area measurements were used to analyze these new textural changes. We have developed methods to demonstrate that specific chemistry has occurred on these new structures. To this end, we introduced metal-binding ligands that could be used as probes in imaging and spectroscopic techniques including TEM, STEM, EDX, and EELS. A proposal for the underlying structure of N-MWCNTs responsible for the formation of the new textures is presented. We have investigated the performance of our materials as potential negative electrodes for rechargeable lithium ion batteries.

The present research work aims to develop a new heat transfer fluid by combining multiwalled carbon nanotubes (MWCNT) and microencapsulated phase change materials (MPCMs). Stable nanofluids have been prepared using different sizes of multiwalled carbon nanotubes and their properties like thermal conductivity and viscosity have been measured. Microencapsulated phase change material slurries containing microcapsules of octadecane have been purchased from Thies Technology Inc. Tests have been conducted to determine the durability and viscosity of the MPCM slurries. Heat transfer experiments have been conducted to determine the heat transfer coefficients and pressure drop of the MWCNT nanofluids and MPCM slurries under turbulent flow and constant heat flux conditions. The MPCM slurry and the MWCNT nanofluid have been combined to form a new heat transfer fluid. Heat transfer tests have been conducted to determine the heat transfer coefficient and the pressure drop of the new fluid under turbulent flow and constant heat flux conditions. The potential use of this fluid in convective heat transfer applications has also been discussed. The heat transfer results of the MPCM slurry containing octadecane microcapsules was in good agreement with the published literature. The thermal conductivity enhancement obtained for MWCNTs with diameter (60-100 nm) and length (0.5-40?m) was 8.11%. The maximum percentage enhancement (compared to water) obtained in the heat transfer coefficient of the MWCNT nanofluid was in the range of 20-25%. The blend of MPCMs and MWCNTs was highly viscous and displayed a shear thinning behavior. Due to its high viscosity, the flow became laminar and the heat transfer performance was lowered. It was interesting to observe that the value of the maximum local heat transfer coefficient achieved in the case of the blend (laminar flow), was comparable to that obtained in the case of the MPCM slurry (turbulent flow). The pressure drop of the blend was lower than that of the MWCNT nanofluid.

A STUDY OF LIGNIN DEPOLYMERIZATION BY SELECTIVE CLEAVAGE OF THE Cα-Cβ LINKAGES IN LIGNIN MODEL COMPOUNDS VIA BAEYER-VILLIGER OXIDATION Lignin is amorphous aromatic polymer derived from plants and is a potential source of fuels and bulk chemicals. Herein, we present a survey of reagents for selective stepwise oxidation of lignin model compounds. Specifically, we have targeted the oxidative cleavage of Cα-Cβ bonds as a means to depolymerize lignin and obtain useful aromatic compounds. In this work, we prepared several lignin model compounds that possess structures, characteristic reactivity, and linkages closely related to the parent lignin polymer. We observed that selective oxidation of benzylic hydroxyl groups using TEMPO/O2, followed by Baeyer-Villiger oxidation of the resulting ketones using H2O2, successfully cleaves the Cα-Cβ linkage in the model compounds. This process was also applied to depolymerization of Organosolv lignin. The deconstructed lignin was analyzed by a number of techniques, including ATR-IR, GPC, and 31P NMR of suitably derivatized samples. AN INVESTIGATION OF THE CHANNELING REACTION IN NITROGEN-DOPED MULTIWALLED CARBON NANOTUBES (N-MWCNTS) The reduction of nitrogen-doped multiwalled carbon nanotubes (N-MWCNTs) with Li/NH3 results in deep longitudinal cuts in the nanotubes structure. As the N-MWCNTs are anisotropic, we were able to investigate whether the unzipping process proceeds with equal efficiency from the tip end or from the root (catalyst) end of the N-MWCNT structure. To accomplish this we prepared polymer filled aligned arrays of N-MWCNTs, then exposed one or the other end. Through this approach we were able to shield the sidewalls and either end of the nanotubes from the Li/NH3 solution We have found that when the top end of the N-MWCNTs array was exposed to the reaction mixture, very few nanotubes suffered significant ‘unzipping’. However, when the root (substrate) side of the array is exposed to the reaction mixture, we observe the features characteristic of nanotubes with longitudinal cuts. Our finding provides some insight into the mechanism of the unzipping process, and provides evidence that the unzipping process has a directional preference-unzipping from the root end towards the tip end. And may provide a method for selective functionalization of the interior of tubes and create a new form of nanotube- based porous membrane.

Electrically conductive adhesives (ECA) are discussed and studied with everincreasing interest as an environmentally friendly alternative to solder interconnection in microelectronics circuit packaging. They are used to attach surface mount devices (SMD), Integrated Circuits (IC) and Flip chips in electronic assembly. The use of ECAs brings some benefits like flexibility, mild processing conditions and process simplicity. Multi walled carbon nanotubes (MWCNT) are used instead of metal fillers because of their novel properties such as light weight, high aspect ratio, corrosion resistant, reduced processing temperature, lead free, good electrical conduction and mechanical strength. The purpose of the present work is to investigate the aging behavior of MWCNT filled adhesives based on anhydride cured epoxy systems and their dependence on loading. Composites with different loadings of MWNT in epoxy and epoxy: heloxy are prepared and then stencil printed onto different surface finished boards like gold, silver and tin to prepare contact resistance samples and onto aluminum oxide boards to prepare volume resistivity samples. These samples are kept at room temperature for about 90 days and then placed in a temperature chamber to observe the behavior of these samples after accelerated aging. The readings are taken for as prepared samples, after 45 days, after 90 days and after accelerated aging. The results are summarized and different trends are observed for different loadings of MWNT, different combinations of epoxy: heloxy and for different surface finished boards.

Multi-walled carbon nanotubes (MWCNTs) and integrated MWCNTs/ SiO2 nanoparticles (NPs) were loaded as additives into nanocomposite polyvinylidene fluoride (PVDF) membranes fabricated via phase inversion methods, and the effects of these additives on the structure and vacuum membrane distillation (VMD) performance of the membranes have been studied. With an appropriate amount of MWCNTs (2 wt.% to PVDF) blended into the membrane, VMD performance of membrane was improved significantly due to higher membrane porosity, contact angle and surface roughness without extreme compromise of liquid entry pressure of water (LEPw), which could reach up to 72 psi. Further integration of MWCNTs with a small amount of SiO2 nanoparticles (NPs) showed a synergic effect resulting in further improvement of VMD flux due primarily to the increase in surface pore size. When the amount of SiO2 NPs additive was large, the effects of NPs dominates the VMD performance. However, the asymmetric structure of PVDF membrane disappears, which exercises an unfavourable effect on VMD performance. All fabricated membranes exhibited a great desalination potential with extremely high salt rejection (>99.98%). The incorporation of MWCNTs did not improve the tensile properties of the membrane.