Process control -- Computer programs.
Process control -- Data processing.
Biomass chemicals -- Extrusion.
Wood flour -- Extrusion.
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PublisherThe University of Arizona.
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Degree ProgramChemical Engineering
Degree GrantorUniversity of Arizona
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Processing High Purity Zirconium Diboride Ultra-High Temperature Ceramics: Small-to-Large Scale ProcessingCorral, Erica L.; Pham, David; Corral, Erica L.; Muralidharan, Krishna; Loy, Doug; Manga, Venkateswara R. (The University of Arizona., 2016)Next generation aerospace vehicles require thermal protection system (TPS) materials that are capable of withstanding the extreme aerothermal environment during hypersonic flight (>Mach 5 [>1700 m/s]). Ultra-high temperature ceramics (UHTC) such as zirconium diboride (ZrB₂) are candidate TPS materials due to their high-temperature thermal and mechanical properties and are often the basis for advanced composites for enhanced oxidation resistance. However, ZrB₂ matrix impurities in the form of boron trioxide (B₂O₃) and zirconium dioxide (ZrO₂) limit the high-temperature capabilities. Electric based sintering techniques, such as spark plasma sintering (SPS), that use joule heating have become the preferred densification method to process advanced ceramics due to its ability to produce high density parts with reduced densification times and limit grain growth. This study focuses on a combined experimental and thermodynamic assisted processing approach to enhance powder purity through a carbo- and borocarbo-thermal reduction of oxides using carbon (C) and boron carbide (B₄C). The amount of oxides on the powder surface are measured, the amount of additive required to remove oxides is calculated, and processing conditions (temperature, pressure, environment) are controlled to promote favorable thermodynamic reactions both during thermal processing in a tube furnace and SPS. Untreated ZrB₂ contains 0.18 wt%O after SPS. Additions of 0.75 wt%C is found to reduce powder surface oxides to 0.12 wt%O. A preliminary Zr-C-O computational thermodynamic model shows limited efficiency of carbon additions to completely remove oxygen due to the solubility of oxygen in zirconium carbide (ZrC) forming a zirconium oxycarbide (ZrCₓOᵧ). Scanning electron microscopy (SEM) and scanning transmission electron microscopy (STEM) with atomic scale elemental spectroscopy shows reduced oxygen content with amorphous Zr-B oxides and discreet ZrO₂ particle impurities in the microstructure. Processing ZrB₂ with minimal additions of B₄C (0.25 wt%) produces high purity parts after SPS with only 0.06 wt%O. STEM identifies unique “trash collector” oxides composed of manufacturer powder impurities of calcium, silver, and yttrium. A preliminary Zr-B-C-O thermodynamic model is used to show the potential reaction paths using B₄C that promotes oxide removal to produce high-purity ZrB₂ with fine grains (3.3 𝜇m) and superior mechanical properties (flexural strength of 660MPa) than the current state-of-the-art ZrB₂ ceramics. Due to the desirable properties produced using SPS, there is growing interest to advance processing techniques from lab-scale (20 mm discs) to large-scale (>100 mm). The advancement of SPS technologies has been stunted due to the limited power and load delivery of lab-scale furnaces. We use a large scale direct current sintering furnace (DCS) to address the challenges of producing industrially relevant sized parts. However, current-assisted sintering techniques, like SPS and DCS, are highly dependent on tooling resistances and the electrical conductivity of the sample, which influences the part uniformity through localized heating spots that are strongly dependent on the current flow path. We develop a coupled thermal-electrical finite element analysis model to investigate the development and effects of tooling and current density manipulation on an electrical conductor (ZrB₂) and an electrical insulator, silicon nitride (Si₃N₄), at the steady-state where material properties, temperature gradients and current/voltage input are constant. The model is built based on experimentally measured temperature gradients in the tooling for 20 mm discs and validated by producing 30 mm discs with similar temperature gradients and grain size uniformity across the part. The model aids in developing tooling to manipulate localize current density in specific regions to produce uniform 100 mm discs of ZrB₂ and Si₃N₄.
TWO-DIMENSIONAL SIGNAL PROCESSING IN RADON SPACE (OPTICAL SIGNAL, IMAGE PROCESSING, FOURIER TRANSFORMS).Barrett, Harrison H.; EASTON, ROGER LEE, JR. (The University of Arizona., 1986)This dissertation considers a method for processing two-dimensional (2-D) signals (e.g. imagery) by transformation to a coordinate space where the 2-D operation separates into orthogonal 1-D operations. After processing, the 2-D output is reconstructed by a second coordinate transformation. This approach is based on the Radon transform, which maps a two-dimensional Cartesian representation of a signal into a series of one-dimensional signals by line-integral projection. The mathematical principles of this transformation are well-known as the basis for medical computed tomography. This approach can process signals more rapidly than conventional digital processing and more flexibly and precisely than optical techniques. A new formulation of the Radon transform is introduced that employs a new transformation--the central-slice transform--to symmetrize the operations between the Cartesian and Radon representations of the signal and to aid in analyzing operations that may be susceptible to solution in this manner. It is well-known that 2-D Fourier transforms and convolutions can be performed by 1-D operations after Radon transformation, as proven by the central-slice and filter theorems. Demonstrations of these operations via Radon transforms are described. An optical system has been constructed to derive the line-integral projections of 2-D transmissive or reflective input data. Fourier transforms of the projections are derived by a surface-acoustic-wave chirp Fourier transformer, and filtering is performed in a surface-acoustic-wave convolver. Reconstruction of the processed 2-D signal is performed optically. The system can process 2-D imagery at approximately 5 frames/second, though rates to 30 frames/second are achievable if a faster image rotator is added. Other signal processing operations in Radon space are demonstrated, including Labeyrie stellar speckle interferometry, the Hartley transform, and the joint coordinate-frequency representations such as the Wigner distribution function. Other operations worthy of further study include derivation of the 2-D cepstrum, and several spectrum estimation algorithms.