The performance advances of radar-guided missiles have created a need for radome materials with improved strength, toughness, and thermal shock capabilities. Zirconium phosphate bonded silicon nitride (Zr-PBSN), which has a low and thermally stable dielectric constant, high rain erosion resistance and a low-cost processing method, has been developed for radome applications in advanced tactical missiles. Pressureless sintering reduces processing costs, but is untried for radome manufacturing. The tendency for catastrophic failure requires that each radome fabricated with this material/method be inspected for defects prior to use. Visible, thermographic and ultrasonic nondestructive evaluation (NDE) methods have been tested with Zr-PBSN discs containing fabricated flaws likely to be present in a radome. Ultrasonic C-scanning using a 0.25" diameter, 15 MHz focused transducer with a pulse-echo configuration was clearly superior at detecting cracks, delaminations, impurities, voids and porosity variation. A method for determining local porosity via the longitudinal elastic wave velocity was developed and can be incorporated into an ultrasonic scanning system. A system that uses a computer to perform all motion control, data acquisition, and data manipulation, but requiring a skilled operator for scan setup and interpretation of the data has been proposed. / Master of Science

Ternary indium aluminum nitride (InXAl1-XN) semiconductor is an attractive material with a wide-range bandgap energy varied from ultraviolet (Eg(AlN): 6.2 eV) to near infrared (Eg(InN): 0.7 eV). With tuning composition, it can be widely used to many optoelectronic device applications. In this thesis, I have studied InXAl1-XN film deposited on Si (111) substrate using natural and isotopically enriched nitrogen as reactive gas by reactive magnetron sputter epitaxy (MSE). Four series of experiments were performed, which are I. InAlN presputtering, II. InAlN sputter deposition, III. InAlN direct deposition, and IV. InAlN direct deposition using isotopically enriched nitrogen. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EDX). The θ-2θ XRD scan confirms that the designed composition x = 0.17 of InXAl1-XN film was obtained. TEM images shows that an amorphous interlayer with a thickness ranging from 1.2 nm to 1.5 nm was formed between Si substrate and InXAl1-XN film. However, high-resolution TEM shows that the interlayer actually contains partial crystalline structures. EDX line profile indicates that the chemical composition of the amorphous interlayer is silicon nitride (SiNX). By comparing d-spacing measurement of partial crystalline structures with EDX line profile, it reveals that partial SiNX crystal is formed in the interlayer. Nonetheless, the samples (IAD01, IAD02, IAD03, IAD04), grown without presputtering procedure, contain both crystalline SiNX and InXAl1-XN embedded in the amorphous interlayer. It means that SiNX and InXAl1-XN film can be directly grown on the substrate in the beginning of deposition. Moreover, the samples (IAD01, IAD03), quenched directly after deposition, have less crystalline structures in the interlayer then the samples (IAD02, IAD04), maintained at 800℃ for 20 min.

The objective of this dissertation is to understand the structural and optoelectronic properties of group III-nitride materials grown by High-Pressure Metal Organic Chemical Vapor Deposition (HP-MOCVD) and Migration Enhanced Plasma Assisted MOCVD by FTIR reflectance spectroscopy, Raman spectroscopy, X-ray diffraction, and Atomic Force Microscopy. The influence of the substrates/templates (Sapphire, AlN, Ga-polar GaN, N-polar GaN, n-GaN, and p-GaN) on the free carrier concentration, carrier mobility, short-range crystalline ordering, and surface morphology of the InN layers grown on HP-MOCVD were investigated using those techniques. The lowest carrier concentration of 7.1×1018 cm-3 with mobility of 660 cm2V-1s-1 was found in the InN film on AlN template, by FTIR reflectance spectra analysis. Furthermore, in addition to the bulk layer, an intermediate InN layers with different optoelectronic properties were identified in these samples. The best local crystalline order was observed in the InN/AlN/Sapphire by the Raman E2 high analysis. The smoothest InN surface was observed on the InN film on p-GaN template. The influence of reactor pressures (2.5–18.5 bar) on the long-range crystalline order, in plane structural quality, local crystalline order, free carrier concentration, and carrier mobility of the InN epilayers deposited on GaN/sapphire by HP-MOCVD has also been studied using those methods. Within the studied process parameter space, the best material properties were achieved at a reactor pressure of 12.5 bar and a group-V/III ratio of 2500 with a free carrier concentration of 1.5x1018 cm-3, a mobility in the bulk InN layer of 270 cm2 V-1s-1 and the Raman (E2 high) FWHM of 10.3 cm-1. The crystalline properties, probed by XRD 2θ–ω scans have shown an improvement with the increasing reactor pressure. The effect of an AlN buffer layer on the free carrier concentration, carrier mobility, local crystalline order, and surface morphology of InN layers grown by Migration-Enhanced Plasma Assisted MOCVD were also investigated. Here, the AlN nucleation layer was varied to assess the physical properties of the InN layers. This study was focused on optimization of the AlN nucleation layer (e.g. temporal precursor exposure, nitrogen plasma exposure, and plasma power) and its effect on the InN layer properties.

In the past decade, GaN-based nitrides have had a considerable impact in solid state lighting and high speed high power devices. InGaN-based LEDs have been widely used for all types of displays in TVs, computers, cell phones, etc. More and more high power LEDs have also been introduced in general lighting market. Once widely used, such LEDs could lead to the decrease of worldwide electrical consumption for lighting by more than 50% and reduce total electricity consumption by > 10%. However, there are still challenges for current state-of-the art InGaN-based LEDs, including ‘efficiency droop’ issues that cause output power quenching at high current injection levels (> 100 A/cm2). In this dissertation, approaches were investigated to address the major issues related to state-of-the-art nitride LEDs, in particular related to (1) efficiency droop investigations on m-plane and c-plane LEDs: enhanced matrix elements in m-plane LEDs and smaller hole effective mass favors the hole transport across the active region so that m-plane LEDs exhibit 30% higher quantum efficiency and negligible efficiency droop at high injection levels compared to c-plane counterparts; (2) engineering of InGaN active layers for achieving high quantum efficiency and minimal efficiency droop: lower and thinner InGaN barrier enhance hole transport as well as improves the quantum efficiencies at injection levels; (3) double-heterostructure (DH) active regions: various thicknesses were also investigated in order to understand the electron and hole recombination mechanism. We also present that using multi-thin DH active regions is a superior approach to enhance the quantum efficiency compared with simply increasing the single DH thickness or the number of quantum wells (QWs, 2 nm-thick) in multi-QW (MQW) LED structures due to the better material quality and higher density of states. Additionally, increased thickness of stair-case electron injectors (SEIs) has been demonstrated to greatly mitigate electron overflow without sacrificing material quality of the active regions. Finally, approaches to enhance light extraction efficiency including using Ga doped ZnO as the p-GaN contact layer to improve light extraction as well as current spreading was introduced.

Abstract This thesis studies the factors that govern transverse cracking during continuous casting of low carbon, niobium microalloyed and boron microalloyed steels. Crack susceptibility in the thick slab, billet and thin slab casting processes are compared by using typical conditions in laboratory hot ductility tests. There is limited published literature on hot ductility in aluminium-killed and siliconkilled boron microalloyed steels and the proposed mechanisms of failure by transverse cracking are contradictory. Few published papers specifically compare hot ductility behaviour of any steels between thick slab, billet and thin slab continuous casting processes. Thus, the basis of this research is to assess the influence of casting parameters and compositional variations on hot ductility behaviour in low carbon steels, niobium microalloyed steels, aluminium-killed boron microalloyed steels and silicon-killed, boron microalloyed steels. The typical temperature ranges, cooling rate and strain rate conditions of the continuous casting processes were used in reheated and in situ melted hot tensile tests performed on steel specimens. Solidification, transformation and precipitation temperatures were calculated using solubility equations and modelled using the Thermo-CalcTM thermodynamics program. Scanning electron microscopy and transmission electron microscopy were used to determine the modes of failure in the tested specimens. In the low carbon steels, hot ductility was improved by increasing the strain rate; by calcium treatment, which minimises copper sulphide and iron sulphide formation; and by maintaining a nickel to copper ratio of 1:1. It was shown that thin slab casting conditions provided the best hot ductility results for the low carbon steels. All the niobium steels showed poor ductility in the single-phase austenite temperature region, indicating that intergranular precipitation of fine niobium carbonitrides was the cause of the poor ductility. It was shown that the hot ductility was greatly improved by calcium treatment, by decreasing the cooling rate and by increasing the strain rate. Slow iv thin slab and thick slab casting conditions provided the best hot ductility results for the niobium steels. Hot ductility was substantially improved in the aluminium-killed boron steels by increasing the boron to nitrogen ratio from 0.19 to 0.75. The results showed that, at cooling rates generally associated with thick slab, bloom and slow thin slab casting, a boron to nitrogen ratio of ≥0.47 was sufficient to avoid a ductility trough altogether. However, under conditions typically experienced in fast thin slab and billet casting, a boron to nitrogen ratio of 0.75 was required to provide good hot ductility. The mechanism of the ductility improvement with increasing boron to nitrogen ratio was found to be enhanced precipitation of boron nitride, leading to a decrease in nitrogen available for aluminium nitride precipitation. In the silicon-killed boron steels, it was found that the boron to nitrogen ratio had the overriding influence on hot ductility and hence on crack susceptibility. Excellent hot ductility was found for boron to nitrogen ratios above 1. Additionally, analysis of industrial casting data showed that the scrap percentage due to transverse cracking increased significantly at manganese to sulphur ratios below fourteen. An exponential decay relationship between the manganese to sulphur ratio and the average scrap percentage due to transverse cracking was determined as a tool to predict scrap levels in the casting plant.

Ces dernières années les semi-conducteurs à base de InGaN sont devenus attractifs pour des applications d'éclairage. Les sources blanches à base de LED sont de plus en plus utilisées en raison de leur petite taille, leur longue durée de vie et leur faible consommation d'énergie. Malheureusement les LED utilisées dans ces dispositifs subissent une perte de rendement quantique externe quand leur courant d'alimentation augmente. Ceci se traduit par un décalage du maximum d'émission ainsi qu'un élargissement spectral. Ces variations d'émission impactent la conversion de lumière bleue en lumière blanche, ce qui diminue l'efficacité du procédé. Une méthode alternative pour obtenir de la lumière blanche en travaillant à forte puissance serait l'utilisation de diodes laser (DL) à la place des LED. Contrairement aux LED, elles sont moins affectées par les pertes d'efficacité. La puissance lumineuse et le rendement quantique externe des diodes laser augmentent linéairement avec le courant d'alimentation, ce qui maintient la stabilité de la lumière blanche produite. / In past few years InGaN-based semiconductors have attracted much more attention for application in solid-state lighting sources. Recently, their usage is constantly increasing on worldwide market. High-brightness white LEDs have been used due to their size, long life and energy saving. However, LEDs used in light sources suffer from a loss in external quantum efficiency as an operating current increases. This loss may lead to a shift in peak emission wavelength and broadening of emission spectrum. Laser diodes, in contrary to LEDs, do not suffer this loss. The output power increases linearly with injection current. Moreover, they can reach higher luminosity, for the same power, than LEDs. Additionally, laser-based devices can be operated in reflection mode, allowing for the phosphor to be placed on a reflection substrate that may also act as a heat sink to effectively dissipate heat away from the phosphor.

Thin film coatings are used to improve the properties of components and products in such diverse areas as tool coatings, wear resistant biological coatings, miniature integrated electronics, micro-mechanical systems and coatings for optical devices. This thesis focuses on understanding the development of intrinsic stress and microstructure in coatings of the technologically important materials of aluminium nitride (AlN) and titanium vanadium nitride (TiVN) deposited by filtered cathodic arc deposition. Thin films of AlN are fabricated under a variety of substrate bias regimes and at different deposition rates. Constant substrate bias was found to have a significant effect on the stress and microstructure of AlN thin films. At low bias voltages, films form with low stress and no preferred orientation. At a bias voltage of -200 V, the films exhibited the highest compressive stress and contained crystals preferentially oriented with their c axis in the plane of the film. At the highest bias of -350 V, the film forms with low stress yet continue to contain crystallites with their c axis constrained to lie in the plane of the film. These microstructure changes with bias are explained in terms of an energy minimisation model. The application of a pulsed high voltage bias to a substrate was found to have a strong effect on the reduction of intrinsic stress within AlN thin films. A model has been formulated that predicts the stress in terms of the applied voltage and pulsing rate, in terms of treated volumes known as thermal spikes. The greater the bias voltage and the higher the pulse rate, the greater the reduction in intrinsic stress. At high pulsing and bias rates, a strong preference for the c axis to align perpendicular to the substrate is seen. This observation is explained by dynamical effects of the incident ions on the growing film, encouraging channelling and preferential sputtering. For the first time, the effect of the rate of growth on AlN films deposited with high voltage pulsed bias was investigated and found to significantly change the stress and microstructure. The formation of films with highly tensile stress, highly compressive stress and nano-composites of AlN films containing Al clusters were seen. These observations are explained in terms of four distinct growth regions. At low rates, surface diffusion and shadowing causes highly porous structures with tensile stress; increased rates produced Al rich films of low stress; increasing the growth rate further led to a dense AlN film under compressive stress and the highest rates produce dense, low stress, AlN due to increased levels of thermal annealing. Finally this thesis analyses the feasibility of forming ternary alloys of high quality TiVN thin films using a dual cathode filtered cathodic arc. The synthesised films show exceptional hardness (greater than either titanium nitride or vanadium nitride), excellent mixing of the three elements and interesting optical properties. An optimum concentration of 23% V content was found to give the highest stress and hardness.

In this work novel solid-state neutron detectors based on Gallium Nitride (GaN) have been produced and characterized. GaN is a radiation hard semiconductor which is commonly used in commercial optoelectronic devices. The important design consideration for producing GaN-based neutron detectors have been examined, and device simulations performed. Scintillators and p-i-n diode-type neutron detectors have been grown by metalorganic chemical vapor deposition (MOCVD) and characterized. GaN was found to be intrinsically neutron sensitive through the Nitrogen-14 (n, p) reaction. Neutron conversion layers which produce secondary ionizing radiation were also produced and evaluated. GaN scintillator response was found to scale highly linearly with nuclear reactor power, indicating that GaN-based detectors are suitable for use in the nuclear power industry. This work is the first demonstration of using GaN for neutron detection. This is a novel application for a mature semiconductor material. The results presented here provide a proof-of-concept for solid-state GaN-based neutron detectors which offer many potential advantages over the current state-of-the-art, including lower cost, lower power operation, and mechanical robustness. At present Helium-3 proportional counters are the preferred technology for neutron detection, however this isotope is extremely rare, and there is a global shortage. Meanwhile demand for neutron detectors from the nuclear power, particle physics, and homeland security sectors requires development of novel neutron detectors which are which are functional, cost-effective, and deployable.

A wide variety of group III-Nitride-based photonic and electronic devices have opened a new era in the field of semiconductor research in the past ten years. The direct and large bandgap nature, intrinsic high carrier mobility, and the capability of forming heterostructures allow them to dominate photonic and electronic device market such as light emitters, photodiodes, or high-speed/high-power electronic devices. Avalanche photodiodes (APDs) based on group III-Nitrides materials are of interest due to potential capabilities for low dark current densities, high sensitivities and high optical gains in the ultraviolet (UV) spectral region. Wide-bandgap GaN-based APDs are excellent candidates for short-wavelength photodetectors because they have the capability for cut-off wavelengths in the UV spectral region (λ < 290 nm). These intrinsically solar-blind UV APDs will not require filters to operate in the solar-blind spectral regime of λ < 290 nm. For the growth of GaN-based heteroepitaxial layers on lattice-mismatched substrates, a high density of defects is usually introduced during the growth; thereby, causing a device failure by premature microplasma, which has been a major issue for GaN-based APDs. The extensive research on epitaxial growth and optimization of Al_x Ga _1-x N (0 ≤ x ≤ 1) grown on low dislocation density native bulk III-N substrates have brought UV APDs into realization. GaN and AlGaN UV <i> p-i-n </i> APDs demonstrated first and record-high true avalanche gain of > 10,000 and 50, respectively. The large stable optical gains are attributed to the improved crystalline quality of epitaxial layers grown on low dislocation density bulk substrates. GaN <i>p-i-n </i> rectifiers have brought much research interest due to its superior physical properties. The AIN-free full-vertical GaN<i> p-i-n </i> rectifiers on<i> n </i>- type 6H-SiC substrates by employing a conducting AIGaN:Si buffer layer provides the advantages of the reduction of sidewall damage from plasma etching and lower forward resistance due to the reduction of current crowding at the bottom<i> n </i> -type layer. The AlGaN:Si nucleation layer was proven to provide excellent electrical properties while also acting as a good buffer role for subsequent GaN growth. The reverse breakdown voltage for a relatively thin 2.5 μm-thick<i> i </i>-region was found to be over -400V.

This thesis describes the development of III-Nitride materials for light emitting applications. The goals of this research were to create and optimize a green light emitting diode (LED) and laser diode (LD). Metalorganic chemical vapor deposition (MOCVD) was the technique used to grow the epitaxial structures for these devices. The active regions of III-Nitride based LEDs are composed of InₓGa₁₋ₓN, the bandgap of which can be tuned to attain the desired wavelength depending on the percent composition of Indium. An issue with this design is that the optimal growth temperature of InGaN is lower than that of GaN, making the growth temperature of the top p-layers critical to the device performance. Thus, an InGaN:Mg layer was used as the hole injection and p-contact layers for a green led, which can be grown at a lower temperature than GaN:Mg in order to maintain the integrity of the active region. However, the use of InGaN comes with its own set of drawbacks, specifically the formation of V-defects. Several methods were investigated to suppress these defects such as graded p-layers, short period supper lattices, and native GaN substrates. As a result, LEDs emitting at ~532 nm were realized. The epitaxial structure for a III-Nitride LD is more complicated than that of an LED, and so it faces many of the same technical challenges and then some. Strain engineering and defect reduction were the primary focuses of optimization in this study. Superlattice based cladding layers, native GaN substrates, InGaN waveguides, and doping optimization were all utilized to lower the probability of defect formation. This thesis reports on the realization of a 454 nm LD, with higher wavelength devices to follow the same developmental path.