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Metallic films are important in various applications, such as electric devices where it can act as contacts. In electrical devices, the substrate typically consists of silicon dioxide (SiO2) which is a temperature-sensitive substrate. Therefore, plasma enhanced chemical vapor deposition (PECVD) are better suited than thermally activated chemical vapor deposition (CVD). Depositing metallic films with PECVD demands co-reactants that act as reducing agents. However, these are not well-studied and do not always have the power enough to perform the reduction reaction for metals. Recently it has been concluded that electrons can act as reducing agents in the deposition of first row transition metallic films in a PECVD process. By supplying a positive bias to the substrate, the electrons got attracted to the surface of the substrate, which facilitated metal growth. The study concluded that metal growth only occurred at conductive -and semiconductive substrates and that the substrate bias and plasma power affected the metal growth. The process is however not well understood, which causes a knowledge gap, signifying that studies of the surface chemistry are needed. Here a new modified analytical method to study the surface chemistry in the newly developed process mentioned above is presented. The analytical method consists of an electrically modified quartz crystal microbalance (QCM) with gold electrodes as a conductive substrate. This allows the electron current to run through the QCM during the measurement. By supplying a DC-voltage to the front electrode it gets readily biased (negative and positive) and by placing a capacitor in the circuit, it connects the AC-circuit (oscillator circuit) and the DC-circuit (DC-voltage bias circuit). At the same time, it blocks the DC-current from going back to the oscillator but allows the high-frequency signal to pass from the QCM. The results in this thesis concluded that the QCM can be electrically modified to allow an electron flux to the QCM while using it as a substrate when electrons are used as reducing agents. Scanning electron microscopy (SEM) of a QCM crystal revealed that a 2 µm film had been deposited while SEM coupled with energy dispersive X-ray spectroscopy (EDS) showed that the film indeed contained iron. Further analysis was made by high-resolution X-ray photoelectron spectroscopy (HR-XPS) to find the elemental composition of the film, which revealed that the thin film contained 41 at.% iron. In addition, this study investigated if the QCM could be used to study CVD processes where electrons were used as reducing agents. The results indeed revealed that it is possible to study the surface chemistry where electrons are used as reducing agents with the electrically modified QCM to gain knowledge concerning film deposition. Initial results of the QCM showed that film growth could be studied when varying the plasma power between 5 W to 15 W and the QCM bias between -40 V to +40 V. The method generated easily accessible data concerning the process where electrons are used as reducing agents, which gained insight to the method that never has been disclosed before.

京都大学 / 新制・課程博士 / 博士(エネルギー科学) / 甲第24011号 / エネ博第447号 / 新制||エネ||84(附属図書館) / 京都大学大学院エネルギー科学研究科エネルギー応用科学専攻 / (主査)教授 平藤 哲司, 教授 土井 俊哉, 教授 藤本 仁 / 学位規則第4条第1項該当 / Doctor of Energy Science / Kyoto University / DFAM

A novel fiber optic structure, termed stochastic ordered hole fibers, has been developed that contains an ordered array of six hollow tubes surrounding a hollow core, combined with a nanoporous glass creating a unique fully three dimensional pore/fiber configuration. The objective of this study is to increase the functionality of these stochastic ordered hole fibers, as well as porous clad fibers, by integrating electronic device components such as conductors, and semiconductors, and optically active materials on and in the optical fiber pore structures. Conductive copper pathways were created on/in the solid core fibers using an electroless deposition technique. A chemical vapor deposition system was built in order to attempt the deposition of silicon in on the porous clad fibers. Additionally, conductive poly(3,4-ethylenedioxythiophene)- poly(styrene sulfonate) (PEDOT:PSS) and photoactive polymer blend poly(3- hexylthiophene) and 1-(3-methoxycarbonyl)-propyl-1-phenyl-)6,6)C61 (P3HT: PCBM) were deposited on the fibers using dip coating techniques. Quantum dots of Cadmium Selenide (CdSe) with particle sizes of ranging from 2- 10 nm were deposited in the stochastic ordered hole fibers. SEM and EDS analysis confirm that copper, polymer materials, and quantum dots were deposited in the pore structure and on the surface of the fibers. Finally, resistance measurements indicate that the electrolessly deposited copper coatings have sufficient conductivity to be used as metallic contacts or resistive heating elements. / Master of Science

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Graphene is one of the most important low dimensional materials. Ever since the inception of graphene, attempts to scale up production of graphene have never stopped. Chemical vapor deposition synthesis of graphene on copper is one of the most promising pathways. However, the poor quality of CVD-derived graphene has hindered synthetic graphene for large scale basic science and commercial applications. The lack of reproducibility of CVD graphene research, and the inferior quality of CVD graphene points to potential hidden variables and misunderstanding of the graphene CVD process. In this thesis, it is identified that trace oxygen is a key factor in determining the quality and growth trajectory for graphene grown by low-pressure CVD. By innovative design in the CVD system layout and meticulous control over the substrate quality, it is demonstrated that by eliminating oxygen below µTorr level in the growth chamber, high quality graphene comparable to exfoliated graphene can be obtained. The ultrahigh graphene quality is showcased by a combination of Raman spectroscopy, electrical transport measurement and various scanning probe techniques including scanning tunneling microscopy (STM) and atomic force microscopy (AFM). Moreover, a graphite-gated device encapsulated by hexagonal boron nitride (h-BN) shows well developed fractional quantum hall effect. Using the oxygen free CVD (OF-CVD) system as a platform, the effect of oxygen is revealed to be inducing etching effect at the µTorr limit. Addition of hydrogen delays the etching effect with reduced graphene growth rate. At high hydrogen concentrations, µTorr-level of oxygen is found to be inducing amorphous carbon contaminations to the graphene surface, at the same time, the quality of the resulting graphene deteriorates with increasing level of oxygen, as characterized by AFM, XPS, Raman spectroscopy and electrical transport measurements. OF-CVD enables unprecedented tunability of the graphene growth behavior in terms of growth rate and nucleation density. Controlled experiments reveal the individual effect of all experimental parameters such as temperature, and partial pressure of methane and hydrogen are studied. Their effect on the initial growth rate of graphene can be modeled by a compact model based on competitive adsorption of methane and hydrogen onto the copper surface. The mechanism of overall coverage-time evolution is further revealed by phase-field modeling. Collectively, the theoretical insights of the CVD process of graphene pave way for graphene synthesis by design. The underlying mechanism and principles provide insights for understanding and optimizing other 2D materials growth mediated by catalytic substrates.

There has been progress in the surface modification of low carbon steel in order to enhance its surface hardness. This study contributes to this by investigating the introduction of carbon nanotubes and amorphous carbon in the carburization of mild steel. In order to achieve the goal, carbon nanotubes were synthesized in a horizontal tubular reactor placed in a furnace also called the chemical vapor deposition process at a temperature of 700oC. Catalyst was produced from Iron nitrate Fe(NO3)3.9H2O and Cobalt nitrate Co(NO3)2.6H2O on CaCO3 support while acetylene C2H2 was used as the carbon source and nitrogen N2 was used as contaminant remover. The as-synthesized carbon nanotubes were purified using nitric acid HNO3 and characterized using scanning electron microscopy (SEM), thermo-gravimetric analysis (TGA) and fourier transform infrared spectroscopy (FTIR). It was found that as-synthesized carbon nanotubes had varying lengths with diameters between 42-52 nm from the SEM and the TGA showed the as-synthesized CNTs with a mass loss of 78% while purified CNTs had 85% with no damage done to the structures after using the one step acid treatment. The as-synthesized and purified carbon nanotubes were used in carburizing low carbon steel (AISI 1018) at two austenitic temperatures of 750oC and 800oC and varying periods of 10-50 minutes while amorphous carbon obtained by pulverizing coal was also used as comparison. The mild steel samples were carburized with carbon nanotubes and amorphous carbon in a laboratory muffle furnace with a defined number of boost and diffusion steps. The carburizing atmosphere consisted of heating up to the varying temperatures at a speed of 10oC/minute, heating under this condition at varying periods, performing a defined number of boost and diffusion processes at the varying temperatures and cooling to room temperatures under the same condition. The carburized surfaces were observed with the Olympus SC50 optical microscope and the hardness distribution of the carburized layer was inspected with a Vickers FM 700 micro-hardness tester. The as-synthesized and purified CNT samples showed higher hardness on the surface of the mild steel than the amorphous carbon. In the same vein, the change in the microstructures of vi the steel samples indicated that good and improved surface hardness was obtained in this work with the reinforcements but with purified CNT having the highest peak surface hardness value of 191.64 ± 4.16 GPa at 800oC, as-synthesized CNT with 177.88 ± 2.35 GPa and amorphous carbon with 160.702 ± 5.79 GPa which are higher compared to the values obtained at 750oC and that of the original substrate which had a surface hardness of 145.188 ± 2.66 GPa. The percentage hardness obtained for the reinforcement with the amorphous carbon, the CNT and the pCNT showed an increase of 5.47%, 10.04% and 15.77% respectively at 750oC when compared to that of the normal substrate carburized without reinforcements. Furthermore, at 800oC, the reinforcement with the amorphous carbon, the CNT and the pCNT show a percentage hardness increase of 7.04%, 14.68% and 22.05% when compared to that of the normal substrate carburized without reinforcements. Comparing the reinforcement potential of the amorphous carbon, the CNT and the pCNT at 750oC, the percentage hardness reveal that using pCNT displayed an increase of 10.89% over that of amorphous carbon and of 6.37% over that of CNT. In addition, the use of CNT as reinforcement at 750oC displayed a percentage hardness increase of 4.83% over that of the amorphous carbon carburized at the same temperature / Civil and Chemical Engineering / M. Tech. (Chemical Engineering)