This dissertation describes the development of a label-free, electrochemical immunosensing platform integrated into a low-cost microfluidic system for the sensitive, selective and accurate detection of cortisol, a steroid hormone co-related with many physiological disorders. Abnormal levels of cortisol is indicative of conditions such as Cushing’s syndrome, Addison’s disease, adrenal insufficiencies and more recently post-traumatic stress disorder (PTSD). Electrochemical detection of immuno-complex formation is utilized for the sensitive detection of Cortisol using Anti-Cortisol antibodies immobilized on sensing electrodes. Electrochemical detection techniques such as cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) have been utilized for the characterization and sensing of the label-free detection of Cortisol. The utilization of nanomaterial’s as the immobilizing matrix for Anti-cortisol antibodies that leads to improved sensor response has been explored. A hybrid nano-composite of Polyanaline-Ag/AgO film has been fabricated onto Au substrate using electrophoretic deposition for the preparation of electrochemical immunosening of cortisol. Using a conventional 3-electrode electrochemical cell, a linear sensing range of 1pM to 1µM at a sensitivity of 66µA/M and detection limit of 0.64pg/mL has been demonstrated for detection of cortisol. Alternately, a self-assembled monolayer (SAM) of dithiobis(succinimidylpropionte) (DTSP) has been fabricated for the modification of sensing electrode to immobilize with Anti-Cortisol antibodies. To increase the sensitivity at lower detection limit and to develop a point-of-care sensing platform, the DTSP-SAM has been fabricated on micromachined interdigitated microelectrodes (µIDE). Detection of cortisol is demonstrated at a sensitivity of 20.7µA/M and detection limit of 10pg/mL for a linear sensing range of 10pM to 200nM using the µIDE’s. A simple, low-cost microfluidic system is designed using low-temperature co-fired ceramics (LTCC) technology for the integration of the electrochemical cortisol immunosensor and automation of the immunoassay. For the first time, the non-specific adsorption of analyte on LTCC has been characterized for microfluidic applications. The design, fabrication technique and fluidic characterization of the immunoassay are presented. The DTSP-SAM based electrochemical immunosensor on µIDE is integrated into the LTCC microfluidic system and cortisol detection is achieved in the microfluidic system in a fully automated assay. The fully automated microfluidic immunosensor hold great promise for accurate, sensitive detection of cortisol in point-of-care applications.

The Terahertz (1012 Hz) region of the electromagnetic spectrum covers the frequency range from roughly 300 GHz to 10 THz, which is in between the microwave and infrared regimes. The increasing interest in the development of ultra-compact, tunable room temperature Terahertz (THz) emitters with wide-range tunability has stimulated in-depth studies of different mechanisms of THz generation in the past decade due to its various potential applications such as biomedical diagnosis, security screening, chemical identification, life sciences and very high speed wireless communication. Despite the tremendous research and development efforts, all the available state-of-the-art THz emitters suffer from either being large, complex and costly, or operating at low temperatures, lacking tunability, having a very short spectral range and a low output power. Hence, the major objective of this research was to develop simple, inexpensive, compact, room temperature THz sources with wide-range tunability. We investigated THz radiation in a hybrid optical and THz micro-ring resonators system. For the first time, we were able to satisfy the DFG phase matching condition for the above-mentioned THz range in one single device geometry by employing a modal phase matching technique and using two separately designed resonators capable of oscillating at input optical waves and generated THz waves. In chapter 6, we proposed a novel plasmonic antenna geometry – the dimer rod-tapered antenna (DRTA), where we created a hot-spot in the nanogap between the dimer arms with a very large intensity enhancement of 4.1×105 at optical resonant wavelength. Then, we investigated DFG operation in the antenna geometry by incorporating a nonlinear nanodot in the hot-spot of the antenna and achieved continuously tunable enhanced THz radiation across 0.5-10 THz range. In chapter 8, we designed a multi-metallic resonators providing an ultrasharp toroidal response at THz frequency, then fabricated and experimentally demonstrated an efficient polarization dependent plasmonic toroid switch operating at THz frequency. In summary, we have successfully designed, analytically and numerically investigated novel THz emitters with the advantages of wide range tunability, compactness, room temperature operation, fast modulation and the possibility for monolithic integration, which are the most sought after properties in the new generation THz sources.

In this research the integration of nanostructures and micro-scale devices was investigated using silica nanowires to develop a simple yet robust nanomanufacturing technique for improving the detection parameters of chemical and biological sensors. This has been achieved with the use of a dielectric barrier layer, to restrict nanowire growth to site-specific locations which has removed the need for post growth processing, by making it possible to place nanostructures on pre-pattern substrates. Nanowires were synthesized using the Vapor-Liquid-Solid growth method. Process parameters (temperature and time) and manufacturing aspects (structural integrity and biocompatibility) were investigated. Silica nanowires were observed experimentally to determine how their physical and chemical properties could be tuned for integration into existing sensing structures. Growth kinetic experiments performed using gold and palladium catalysts at 1050 ˚C for 60 minutes in an open-tube furnace yielded dense and consistent silica nanowire growth. This consistent growth led to the development of growth model fitting, through use of the Maximum Likelihood Estimation (MLE) and Bayesian hierarchical modeling. Transmission electron microscopy studies revealed the nanowires to be amorphous and X-ray diffraction confirmed the composition to be SiO2 . Silica nanowires were monitored in epithelial breast cancer media using Impedance spectroscopy, to test biocompatibility, due to potential in vivo use as a diagnostic aid. It was found that palladium catalyzed silica nanowires were toxic to breast cancer cells, however, nanowires were inert at 1µg/mL concentrations. Additionally a method for direct nanowire integration was developed that allowed for silica nanowires to be grown directly into interdigitated sensing structures. This technique eliminates the need for physical nanowire transfer thus preserving nanowire structure and performance integrity and further reduces fabrication cost. Successful nanowire integration was physically verified using Scanning electron microscopy and confirmed electrically using Electrochemical Impedance Spectroscopy of immobilized Prostate Specific Antigens (PSA). The experiments performed above serve as a guideline to addressing the metallurgic challenges in nanoscale integration of materials with varying composition and to understanding the effects of nanomaterials on biological structures that come in contact with the human body.

The Terahertz region of the electromagnetic spectrum is the region between microwaves and infra-red, dubbed the terahertz 'gap' due to its relative underdevelopment in terms of technology. This region is marked by expensive and inconvenient sources that are bulky or that require cryogenic cooling for normal operation, therefore creating a need for cheap and easy to use terahertz sources. Carbon nanotubes have received considerable attention since their discovery due to their unique physical and electronic properties. Many applications have been proposed using especially Single-Walled Carbon Nanotubes (SWCNTs), and a number of commercial technologies exist. In this work, we have proposed to use SWCNTs as the basis for a cheap, compact and room temperature-operating Terahertz source. We have characterized the SWCNT source, and we present results on transport characteristics (I–V curves), radiation patterns, spectra, polarization as well as optical, SEM and AFM imaging. We show that the radiation spectrum is vi determined by integrated antennas coupled to the SWCNTs, and preliminary power calibration indicates that the radiated power exceeds the power predicated by the Nyquist formula.

Carbon nanotubes (CNTs) are promising nanomaterials for high frequency applications due to their unique physical characteristics. CNTs have a low heat capacity, low intrinsic capacitance, and incredibly fast thermal time constants. They can also exhibit ballistic transport at low bias, for both phonons and electrons, as evident by their fairly long mean free paths. However, despite the great potential they present, the RF behavior of these nanostructures is not completely understood. In order to explore this high frequency regime we studied the microwave (MW) and terahertz (THz) response of individual and bundled single wall nanotube based devices. This thesis is an experimental study which attempts to understand the high frequency characteristics of metallic single walled carbon nanotubes, and to develop an ultra-fast and sensitive direct THz detector. First, the appropriate high frequency detector background is introduced. CNTs previously measured behavior draws similarities to two types of detectors: diode and bolometer. Therefore, our CNT devices are geared towards those designs. Second the fabrication process of devices is reviewed. UV lithography is used to pattern THz coupling log periodic antennas, on top of which CNTs are deposited by using a dielectrophoretic process. Third, the fabricated devices are tested at DC, MW, and THz frequencies. All of these measurements are done as a function of temperature, power, and frequency. Finally, the physical processes that give rise to the diode and bolometric detections at MW and THz detection at different temperatures and under different bias regimes (i.e. low and high) are explained.

Parameter variations introduced by manufacturing imprecision are becoming more influential on circuit performance. This is especially the case in emerging nanoscale fabrics due to unconventional manufacturing steps (e.g., nano-imprint) and aggressive scaling. These parameter variations can lead to performance deterioration and consequently yield loss. Parameter variations are typically addressed pre-fabrication with circuit design targeting worst-case timing scenarios. However, this approach is pessimistic and much of performance benefits can be lost. By contrast, if parameter variations can be estimated post-manufacturing, adaptive techniques or reconfiguration could be used to provide more optimal level of tolerance. To estimate parameter variations during run-time, on-chip variation sensors are gaining in importance because of their easy implementation. In this thesis, we propose novel on-chip variation sensors to estimate variations in physical parameters for emerging nanoscale fabrics. Based on the characteristics of systematic and random variations, two separate sensors are designed to estimate the extent of systematic variations and the statistical distribution of random variations from measured fall and rise times in the sensors respectively. The proposed sensor designs are evaluated through HSPICE Monte Carlo simulations with known variation cases injected. Simulation results show that the estimation error of the systematic-variation sensor is less than 1.2% for all simulated cases; and for the random-variation sensor, the worst-case estimation error is 12.7% and the average estimation error is 8% for all simulations. In addition, to address the placement of on-chip sensors, we calculate sensor area and the effective range of systematic-variation sensor. Then using a processor designed in nanoscale fabrics as a target, an example for sensor placement is introduced. Based on the sensor placement, external noises that may affect the measured fall and rise times of outputs are identified. Through careful analysis, we find that these noises do not deteriorate the accuracy of the systematic-variation sensor, but affect the accuracy of the random-variation sensor. We believe that the proposed on-chip variation sensors in conjunction with post-fabrication compensation techniques would be able to improve system-level performance in nanoscale fabrics, which may be an efficient alternative to making worst-case assumptions on parameter variations in nanoscale designs.

This research reports on the fabrication and characterization of integrated dual nanometer-sized electrodes. The electrodes are made of closely spaced nanometer-sized platinum and gold achieved by inserting and pulling platinum wire in cylindrical glass pipette plated with gold. Cyclic voltammetry has been used to characterize the electrodes. Our results show that both electrodes can work individually and can accomplish generation/collection experiments. Factors that may affect the performance of the electrodes as well as formation mechanism of the gold film by electroless plating are discussed.

Metasurfaces are arrays of subwavelength meta-atoms that shape waves in a compact and planar form factor. During recent years, metasurfaces have gained a lot of attention due to their compact form factor, easy integration with other devices, multi functionality and straightforward fabrication using conventional CMOS techniques. To provide and evaluate an efficient metasurface, an optimized design, high resolution fabrication and accurate measurement is required. Analysis and design of metasurfaces require accurate methods for modeling their interactions with waves. Conventional modeling techniques assume that metasurfaces are locally periodic structures excited by plane waves, restricting their applicability to gradually varying metasurfaces that are illuminated with plane waves. In this work, we will first provide a novel technique that enables the development of accurate and general models for 1D metasurfaces. This approach can be easily extended to 2D metasurfaces. Due to the remarkable importance of accurate characterization of metasurfaces, we will provide a rigorous method to characterize 1D metasurfaces. Finally, we will provide an accurate approach to fabricate and characterize 2D metasrufaces.

<p>Gallium nitride (GaN) nanowires are high-performance materials with wide, direct bandgaps and superior electronic properties. Although their properties make them of great interest for next-generation technologies, widespread adoption has been limited by expensive production processes. Here, the results of growing GaN nanowires via DC magnetron sputtering at different temperatures and using different metal catalysts are reported.</p> <p>A new substrate heater was designed to minimize contamination from the heater filament and increase the substrate temperature window to in excess of 800°C. Sixteen-mm² (111) silicon samples had one-to-four nm of a metal catalyst deposited on them using evaporation. This metal catalyst layer (gold, platinum, or nickel) was employed to induce catalyst-assisted vapor-liquid-solid nanowire growth. GaN was deposited via a reactive nitrogen DC magnetron sputtering system. Surface morphology and composition were analyzed using both scanning and transmission electron microscopy. Energy-dispersive x-ray spectroscopy (EDS) and electron energy loss spectroscopy were used to measure the presence of gallium and nitrogen in the resulting nanowires, respectively.</p> <p>This furnace significantly reduced tungsten contamination to below the detectable levels of EDS. GaN nanowires were present on gold-catalyzed samples only in the gold-covered region of the silicon substrate exposed to a gallium flux. Nanowire morphology improved as temperature was elevated, but it did so at the cost of lower areal density. Conversely, platinum-coated samples yielded fewer nanowires than their gold-coated counterparts. Samples that had nickel deposited on them displayed the best GaN nanowire growths. They had the best surface morphologies, had negligible oxygen concentrations, and were single crystalline.</p> / Master of Applied Science (MASc)

Scanning-electron-beam lithography (SEBL) is the primary technology to generate arbitrary features at the nano-scale. However, pattern placement accuracy still remains poor compared to its resolution due to the open-loop nature of SEBL systems. Vibration, stray electromagnetic fields, deflection distortion and hysteresis, substrate charging, and other factors prevent the electron-beam from reaching its target position and one has no way to determine the actual beam position during patterning with conventional systems. To improve the pattern placement accuracy, spatial-phase-locked electron-beam lithography (SPLEBL) provides feedback control of electron-beam position by monitoring the secondary electron signal from electron-transparent fiducial grids on the substrate. While scanning the electron beam over the fiducial grids, the phase of the grid signal is analyzed to estimate the electron-beam position error; then the estimates are sent back to beam deflection system to correct the position error. In this way, closed-loop control is provided to ensure pattern placement accuracy. The implementation of spatial-phase-locking on high speed field-programmable gate array (FPGA) provides a low-cost method to create a nano-manufacturing platform with 1 nm precision and significantly improved throughput. Shot-to-shot, or pixel-to-pixel, dose variation during EBL is a significant practical and fundamental problem. Dose variations associated with charging, electron source instability, optical system drift, and ultimately shot noise in the beam itself conspire to increase critical dimension variability and line width roughness and to limit the throughput. It would be an important improvement to e-beam patterning technology if real-time feedback control of electron-dose were provided to improve pattern quality and throughput even beyond the shot noise limit. A novel approach is proposed in this document to achieve the real-time dose control based on the measurement of electron arrival at the sample to be patterned, rather than from the source or another point in the electron-optical system. A dose control algorithm, implementation on FPGA, and initial experiment results for the real-time feedback dose control on the e-beam patterning tool is also presented.