Materials Science and Engineering Commons^™

Methods For Determining The Infrared Complex Refractive Indices N(Λ) And K(Λ) From Organic Solid Powders: Comparison Of A Sucrose Single Crystal And A Pressed Pellet, Michael O. Yokosuk, Danielle L. Saunders, Charles Tom Resch, Jeremy D. Erickson, Charmayne E. Lonergan, Sarah D. Burton, Mark E. Bowden, Kelly A. Peterson, Timothy J. Johnson, Tanya L. Myers

Materials Science and Engineering Faculty Research & Creative Works

There exists a need to measure optical constants n and k for many materials, especially organic solids in the infrared spectral region, but at present, there are only two established methods for making such measurements: single-angle (SA) reflectance and infrared spectroscopic ellipsometry (IRSE). the former derives the n/k vectors via measurement of the change in the amplitude of light reflected from the sample and then uses the Kramers-Kronig transform, while the latter measures the change in polarization of the reflected light from the sample to derive n/k. Here we make a direct comparison between the n/k vectors derived from SA …

Advanced Microstructural Characterization Of Functionally Graded Dental Ceramic Material For Materials-Informed Finishing, Angani Vigneswaran

Theses and Dissertations--Manufacturing Systems Engineering

Yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) has gained popularity as the choice of material for dental prosthetics. Ivoclar Vivadent’s IPS e.max ZirCAD Prime dental ceramic incorporates a unique gradient technology that varies the yttria content over the thickness of the material. The top layer is composed of 5Y-TZP which is desired for its optical properties while the bottom layer is composed of a much stronger 3Y-TZP. In between the two layers, 5Y-TZP and 3Y-TZP are mixed to form a transition layer. Varying the amount of yttria allows for more esthetically pleasing translucency in the visible areas of the restoration without compromising …

Xps Study Of Calcium Lanthanum Sulfide Ceramics, Brian E. Butkus

Graduate Thesis and Dissertation 2023-2024

Long wave infrared (LWIR) optics that transmit in the 8 to 14 m wavelength range and, additionally, can withstand severe physical and thermal stresses are needed for advanced remote sensing, guidance and communication-based applications. However, most non-oxide transparent LWIR optics do not have the wider transmission range, nor the hardness and resistance to thermal shock needed for extreme environments. Because of these limitations, research is circling back to a promising material, calcium lanthanum sulfide (CLS), that could meet LWIR needs for extreme environments.

In this thesis, we will demonstrate the abilities of x-ray photoelectron spectroscopy (XPS) as a technique for …

Intragranular Tungsten-Titanium Carbide Composite Ceramics Via Gas-Solid Displacement Reactions, Ryan Daniel Dempsey

Doctoral Dissertations

"Research presented herein details the synthesis and characterization of nanocomposite ceramics featuring novel heterogeneous microstructures of potential interest in a variety of electrical and structural applications. Specifically, W-TiCy composite ceramics featuring tungsten nanoprecipitates located primarily within TiCy grains have been produced via sintering of intragranular nanocomposite powders produced via reaction processing-based techniques. This dissertation details the thermodynamic basis and applied kinetics of a processing scheme for fabricating nanocomposite ceramics whose morphological heterogeneity reflects that originally developed in the powder state. The first study in this series overviews the motivation for applying metallothermic displacement reactions, conducted through gaseous intermediates, to solid …

Effect Of Mechanical Activation On Carbothermal Synthesis And Densification Of Zrc, Nina Obradović, Lun Feng, Suzana Filipović, Miljana Mirković, Darko Kosanović, Jelena Rogan, William Fahrenholtz

Materials Science and Engineering Faculty Research & Creative Works

Zirconium carbide ceramics were prepared by carbothermal reduction of ZrO₂ and C that were mixed by high-energy ball milling. Powders were milled for times from 0 to 120 min in air. As milling time increased, the surface area of the powders increased, indicating significant particle size reduction. Milled powders were reacted at 1600 °C and then densified by spark plasma sintering at 2000 °C, which was sufficient to convert the starting powders to zirconium carbide. Unmilled powders did not reach full density. Milled powders reached full density, but ZrO₂ impurities were found for specimens prepared from powders milled …

High Temperature Confocal Scanning Laser Microscopy Analysis Of Dead-Burned Magnesia Aggregates, Tyler Richards, Viraj Athavale, Jeffrey D. Smith, Ronald J. O'Malley

Materials Science and Engineering Faculty Research & Creative Works

Dead-Burned Magnesia is a Commonly Used Material in the Manufacturing of Refractories for the Steelmaking Industry. Aggregates of Dead-Burned Magnesia Contain Secondary Phases Due to the Impurities within the Magnesite Rock Used in its Production. While These Phases Can Aid in Sintering Magnesia, They May Have Some Impact on the High-Temperature Performance of the Refractory Product. High-Temperature Confocal Scanning Laser Microscopy Was Utilized to Observe the Behavior of Dead-Burned Magnesia Aggregates at Elevated Temperatures (Up to 1550°C). Liquid Formation Was Detected Even at Temperatures Below 1350°C. in Some Cases, This Liquid Quickly Exuded from the Aggregate Surface. This Liquid Phase …

Development Of Interatomic Potential Of High Entropy Diborides With Artificial Intelligence Approach To Simulate The Thermo-Mechanical Properties, Nur Aziz Octoviawan

Graduate Theses/Dissertations

The interatomic potentials designed for binary/high entropy diborides and ultra-high temperature composites (UHTC) have been developed through the implementation of deep neural network (DNN) algorithms. These algorithms employed two different approaches and corresponding codes; 1) strictly local & invariant scalar-based descriptors as implemented in the DEEPMD code and 2) equivariant tensor-based descriptors as included in the ALLEGRO code. The samples for training and validation sets of the forces, energy, and virial data were obtained from the ab-initio molecular dynamics (AIMD) simulations and Density Functional Theory (DFT) calculations, including the simulation data from the ultra-high temperature region (> 2000K). The study …

Effects Of Confinement On Ionic Liquids And Deep Eutectic Solvents For The Design Of Catalytic Systems, Electrochemical Devices, And Separations, Andrew Drake

Theses and Dissertations--Chemical and Materials Engineering

Confinement of ionic liquids (ILs) and deep eutectic solvents (DESs) within mesoporous materials such as silica helps to control the local environment within the pores for applications such as catalysis, electrochemistry, and absorption. Silica thin films with 2.5 and 8 nm pores and micron-sized silica particles with pore diameters of 5.4 and 9 nm were synthesized to study the effect of nanoconfinement on ILs 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF₆]), 1-butyl-3-methylimidazolium chloride ([BMIM][Cl]), and DESs reline and ethaline (choline chloride and urea or ethylene glycol). Silica thin films with vertically aligned, well ordered, and accessible pores were synthesized via the evaporation-induced …

System Analysis Of An Internal Combustion Engine (Ice) – Solid Oxide Fuel Cell (Sofc) Hybrid Cycle, Jose Javier Colon Rodriguez

Graduate Theses, Dissertations, and Problem Reports (ETD)

Due to the intermittent nature of renewable energy and the rigid operation of existing coal plants, the need for flexible power generation technology is eminent. Hybrid energy systems have shown potential for flexible, grid following dynamics while maintaining higher efficiencies. The work below focuses on the performance analysis of a proposed 100 kW pressurized Internal Combustion Engine (ICE) and Solid Oxide Fuel Cell (SOFC) hybrid system. The un-utilized fuel from the SOFC stack provided the chemical energy to operate the engine. A turbocharger was used to deliver the necessary air flow for both the stack and engine. An external reformer …

Thermal And Electrical Properties Of Spark Plasma Sintered (Ti,Cr)B2 Ceramics, Steven M. Smith, Lun Feng, William Fahrenholtz, Gregory E. Hilmas, Laura Silvestroni

Materials Science and Engineering Faculty Research & Creative Works

Thermal and electrical properties were measured for TiB₂ ceramics containing varying CrB₂ contents up to 33 mol%. The room-temperature thermal diffusivity decreased with increasing Cr content from 0.330 ± 0.003 cm²/s for pure TiB₂ to 0.060 ± 0.003 cm²/s for (Ti_0.66Cr_0.33)B2. The amount of anisotropy in the coefficients of thermal expansion increased with increasing Cr content and the c-axis had the greatest dependence on Cr addition, with an increase of more than 25% in the thermal expansion for 33 mol% CrB₂ compared to TiB₂, whereas the …

Manganese-Based A-Site High-Entropy Perovskite Oxides For Solar Thermochemical Hydrogen Production, Cijie Liu

Graduate Theses, Dissertations, and Problem Reports (ETD)

Non-stoichiometric perovskite oxides have been studied as a new family of redox oxides for solar thermochemical hydrogen (STCH) production owing to their favourable thermodynamic properties. However, conventional perovskite oxides suffer from limited phase stability and kinetic properties, and poor cyclability. Here, we report a strategy of introducing A-site multi-principal-component mixing to develop a high-entropy perovskite oxide, (La_1/6Pr_1/6Nd_1/6Gd_1/6Sr_1/6Ba_1/6)MnO₃ (LPNGSB_Mn), which shows desirable thermodynamic and kinetics properties as well as excellent phase stability and cycling durability. LPNGSB_Mn exhibits enhanced hydrogen production (~77.5 mmol moloxide^–1) compared to (La …

Development Of High Kinetic Inductance Superconducting Nanowire Devices On High Permittivity Strontium Titanate Substrates, Jamie Timmons

UNF Graduate Theses and Dissertations

This thesis involves the fabrication and characterization of devices made from two different superconducting materials: yttrium barium copper oxide (YBCO), a high-TC complex oxide, and niobium nitride (NbN), a low-TC transition metal nitride. Both types of devices are fabricated on strontium titanate substrates, which provides a good lattice match to YBCO and also an extremely large permittivity at low temperature. We demonstrate that wet etching of YBCO thin films via bromine can be a viable microfrabriation technique for the material. Using approximately 35 nm thick epitaxially grown YBCO on an STO substrate, we were able to fabricate YBCO “microwires” with …

Solid-State Electrolytes For Long Duration Molten Sodium Batteries, Ryan C. Hill

Theses and Dissertations--Chemical and Materials Engineering

Rechargeable batteries have become a staple of modern society, driving the development and expansion of portable electronics and electric vehicles. The long lifetime and high energy density provided by batteries have made them excellent candidates for use in the emerging field of long duration, grid-scale energy storage. However, traditional battery chemistries, such as Li-ion, are not an ideal solution for grid-scale storage, due to high-cost raw materials that are often sourced from volatile markets. Sodium-based batteries are a promising alternative for long duration storage, owing to the domestic abundance of raw materials and energy densities that nearly rival that of …

Boosting Snr Of Cascaded Fbgs In A Sapphire Fiber Through A Rapid Heat Treatment, Farhan Mumtaz, Hanok Tekle, Bohong Zhang, Jeffrey D. Smith, Ronald J. O'Malley, Rex Gerald, Jie Huang

PSMRC Faculty Research

This Letter reports the performance of femtosecond (fs) laser-written distributed fiber Bragg gratings (FBGs) under high-temperature conditions up to 1600°C and explores the impact of rapid heat treatment on signal-to-noise ratio (SNR) enhancement. FBGs are essential for reliable optical sensing in extreme temperature environments. Comprehensive tests demonstrate the remarkable performance and resilience of FBGs at temperatures up to 1600°C, confirming their suitability for deployment in such conditions. The study also reveals significant fringe visibility improvements of up to ∼10 dB on a 1-m-long sapphire optical fiber through rapid heat treatment, representing a first-time achievement to the best of our knowledge. …

Mechanical Properties Of Zrb2 Ceramics Determined By Two Laboratories, Jeffrey J. Swab, Jecee Jarman, William Fahrenholtz, Jeremy Lee Watts

Materials Science and Engineering Faculty Research & Creative Works

The mechanical properties for zirconium diboride (ZrB2) were measured at two laboratories and compared. Two billets of ZrB2 were prepared by hot-pressing commercial powder. The relative densities of the billets were >99% and with an average grain size of 5.9 ± 4.5 µm. Both laboratories prepared American Society for Testing and Materials (ASTM) C1161 B-bars for strength and ASTM C1421 bars with notch configuration A for fracture toughness. Specimens were machined by diamond grinding at the Army Research Laboratory (ARL) and electrical discharge machining (EDM) at Missouri S&T. Strength bars tested at Missouri S&T were polished to a.25 μm finish …

Oxidation Behavior Of Nb-Coated Zirconium Diboride, Jan E. Förster, William Fahrenholtz, Gregory E. Hilmas, Ravisankar Naraparaju

Materials Science and Engineering Faculty Research & Creative Works

Metallic Nb-Coatings Were Deposited on Top of ZrB₂ by Means of Magnetron Sputtering to Improve its Oxidation Resistance. High Temperature Oxidation Tests Have Revealed that the Metallic Nb-Coatings Lead to the Formation of a Dense Solid and Protective Reaction Zone in Addition to a More Stable B₂O₃ Liquid Solution at the Surface. Compared to Baseline ZrB₂, a Reduction in the Oxidation Kinetics, as Well as the Thickness of the Porous Zirconia Layer by 71%, Has Been Achieved with the Help of Nb-Coatings. a Liquid Phase Sintering by Molten Nb₂O₅ Mechanism Was …

High Temperature Dielectric Properties Of Calcium Zirconate, Alan Devoe, Hung Trinh, Fatih Dogan

Materials Science and Engineering Faculty Research & Creative Works

The electrical properties of dense, high purity CaZrO3 discs, sintered at 1380°C with and without added ZrO2, were investigated up to 950°C. Dielectric constant, loss tangent, and electrical conductivity were measured from 25 to 725°C, and the real and imaginary impedances were measured between 800 and 950°C by impedance spectroscopy techniques. Dielectric constant increased by 8% above 300°C and loss tangent increased from.1% at 25°C to ∼2% above 300°C. Activation energy of electrical conductivity determined between 300°C and 950°C by alternative current (AC) and direct current (DC) measurements. These results indicate that CaZrO3 could be a useful dielectric material for …

Final-Stage Densification Kinetics Of Direct Current–Sintered Zrb2, Austin D. Stanfield, Steven M. Smith, Suzana Filipović, Nina Obradović, Vladimir Buljak, Gregory E. Hilmas, William Fahrenholtz

Materials Science and Engineering Faculty Research & Creative Works

Final-stage sintering was analyzed for nominally phase pure zirconium diboride synthesized by borothermal reduction of high-purity ZrO₂. Analysis was conducted on ZrB₂ ceramics with relative densities greater than 90% using the Nabarro–Herring stress–directed vacancy diffusion model. Temperatures of 1900°C or above and an applied uniaxial pressure of 50 MPa were required to fully densify ZrB₂ ceramics by direct current sintering. Ram travel data were collected and used to determine the relative density of the specimens during sintering. Specimens sintered between 1900 and 2100°C achieved relative densities greater than 97%, whereas specimens sintered below 1900°C failed to …

The Effect Of Crystal Anisotropy On Fracture Toughness And Strength Of Zrb2 Microcantilevers, Tamás Csanádi, Ahmad Azizpour, Marek Vojtko, William Fahrenholtz

Materials Science and Engineering Faculty Research & Creative Works

The influence of crystal anisotropy on the micromechanical properties of ceramic grains plays an important role in the design of the macromechanical performance of bulk polycrystalline samples. To this end, the effect of crystal orientation on fracture toughness and strength was investigated by microcantilever bending experiments combined with finite element method (FEM) simulations in grains of a polycrystalline ZrB2 sample. The sample was prepared by hot pressing and the crystal orientations were determined by electron backscatter diffraction after careful surface preparation. The bending tests were carried out on notched and unnotched microcantilevers cut from specific grains along the prismatic (⊥ …

Strength Retention Of Single-Phase High-Entropy Diboride Ceramics Up To 2000°C, Lun Feng, William Fahrenholtz, Gregory E. Hilmas, Yue Zhou, Jincheng Bai

Materials Science and Engineering Faculty Research & Creative Works

The mechanical properties of single-phase (Hf_0.2,Nb_0.2,Ta_0.2,Ti_0.2,Zr_0.2)B₂ ceramics with high purity were investigated. The resulting ceramics had relative density greater than 99%, and an average grain size of 4.3 ± 1.6 μm. At room temperature (RT), the Vickers hardness was 25.2 ± 0.6 GPa at a load of 0.49 N, Young's modulus was 551 ± 7 GPa, fracture toughness was 4.5 ± 0.4 MPa m1/2, and flexural strength was 507 ± 10 MPa. Flexural strength increased by more than 50% from 507 ± 10 MPa at RT to 776 ± …

Thermal And Electrical Properties Of Spark Plasma Sintered (Ti,Cr)B2 Ceramics, Steven M. Smith, Lun Feng, William Fahrenholtz, Gregory E. Hilmas, Laura Silvestroni

Materials Science and Engineering Faculty Research & Creative Works

Thermal and electrical properties were measured for TiB2 ceramics containing varying CrB2 contents up to 33 mol%. The room-temperature thermal diffusivity decreased with increasing Cr content from 0.330 ± 0.003 cm2/s for pure TiB2 to 0.060 ± 0.003 cm2/s for (Ti0.66Cr0.33)B2. The amount of anisotropy in the coefficients of thermal expansion increased with increasing Cr content and the c-axis had the greatest dependence on Cr addition, with an increase of more than 25% in the thermal expansion for 33 mol% CrB2 compared to TiB2, whereas the a-axis only increased by about 8%. The electrical conductivity was the lowest for (Ti0.66Cr0.33)B2 …

Boro/Carbothermal Reduction Co-Synthesis Of Dual-Phase High-Entropy Boride-Carbide Ceramics, Lun Feng, William Fahrenholtz, Gregory E. Hilmas, Stefano Curtarolo

Materials Science and Engineering Faculty Research & Creative Works

Dense, dual-phase (Cr,Hf,Nb,Ta,Ti,Zr)B₂-(Cr,Hf,Nb,Ta,Ti,Zr)C ceramics were synthesized by boro/carbothermal reduction of oxides and densified by spark plasma sintering. The high-entropy carbide content was about 14.5 wt%. Grain growth was suppressed by the pinning effect of the two-phase ceramic, which resulted in average grain sizes of 2.7 ± 1.3 µm for the high-entropy boride phase and 1.6 ± 0.7 µm for the high-entropy carbide phase. Vickers hardness values increased from 25.2 ± 1.1 GPa for an indentation load of 9.81 N to 38.9 ± 2.5 GPa for an indentation load of 0.49 N due to the indentation size effect. Boro/carbothermal …

Thermal And Electrical Properties Of Spark Plasma Sintered (Ti,Cr)B2 Ceramics, Steven M. Smith, Lun Feng, William Fahrenholtz, Gregory E. Hilmas, Laura Silvestroni

Mathematics and Statistics Faculty Research & Creative Works

Thermal and electrical properties were measured for TiB2 ceramics containing varying CrB2 contents up to 33 mol%. The room-temperature thermal diffusivity decreased with increasing Cr content from 0.330 ± 0.003 cm2/s for pure TiB2 to 0.060 ± 0.003 cm2/s for (Ti0.66Cr0.33)B2. The amount of anisotropy in the coefficients of thermal expansion increased with increasing Cr content and the c-axis had the greatest dependence on Cr addition, with an increase of more than 25% in the thermal expansion for 33 mol% CrB2 compared to TiB2, whereas the a-axis only increased by about 8%. The electrical conductivity was the lowest for (Ti0.66Cr0.33)B2 …

Cascaded Sapphire Fiber Bragg Gratings Inscribed By Femtosecond Laser For Molten Steel Studies, Dinesh Reddy Alla, Deva Prasad Neelakandan, Farhan Mumtaz, Rex E. Gerald, Laura Bartlett, Ronald J. O'Malley, Jeffrey D. Smith, Jie Huang

Electrical and Computer Engineering Faculty Research & Creative Works

This research reports a distributed fiber optic high-temperature sensing system tailored for applications in the steel industry and various other sectors. Recent advancements in optical sensor technology have led to the exploration of sapphire crystal fibers as a solution for sensing in harsh environments. Utilizing a femtosecond (fs) laser, cascaded fiber Bragg gratings (FBGs) were meticulously fabricated within a multimode sapphire optical fiber. These FBGs endowed the system with distributed sensing capabilities and underwent rigorous testing under extreme temperatures, reaching up to 1,800 °C. The study delves into the investigation of the FBG reflection spectrum, facilitated by the development of …

Modified Reactive Sputter Deposition Of Titanium Nitride Thin Films Via Hipims With Kick-Pulse And Improvement Of The Structure-Zone Model, Andrew Miceli

UNF Graduate Theses and Dissertations

Direct current (DC) and radio frequency (RF) sputtering methods have been commonplace in industry for several decades and widely studied in literature. Hard films of nitrides, such as titanium nitride (TiN), have been deposited using reactive DC sputtering onto cutting tools and medical devices extensively as well. For these applications, the films require excellent adhesion, high density, and high hardness. High-Power Impulse Magnetron Sputtering (HIPIMS) has emerged over the last several years as a method to produce films with increased density and mechanical properties. Process-structure-property relationships for reactive HIPIMS are not yet well developed. Additionally, conventional HIPIMS suffers from relatively …

Assembly Of Ceramic Particles In Aqueous Suspensions Induced By High-Frequency Ac Electric Field, James E. John Iv

Mechanical & Aerospace Engineering Theses & Dissertations

Ceramic materials processed using colloidal methods have been the focus of a great deal of research aimed at tailoring the final structure and microstructure of the finished ceramic sample. To this end, various external field effects have been investigated to modify the suspension microstructure without manipulating the ceramic particles directly. In a previous work in the field of ice templating it has been shown that AC electric fields are able to produce microstructural changes in ice templated ceramics that have significantly improved the final mechanical properties. However, the mechanisms for this process are still not well understood in ceramics.

To …

Material Characterization And Comparison Of Sol-Gel Deposited And Rf Magnetron Deposited Lead Zirconate Titanate Thin Films, Katherine Lynne Miles

Mechanical Engineering ETDs

Lead zirconate titanate (PZT) has been a material of interest for sensor, actuator, and transducer applications in microelectromechanical systems (MEMS). This is due to their favorable piezoelectric, pyroelectric and ferroelectric properties. While various methods are available to deposit PZT thin films, radio frequency (RF) magnetron sputtering was selected to provide high quality PZT films with the added capability of batch processing. These sputter deposited PZT films were characterized to determine their internal film stress, Young’s modulus, composition, and structure. After characterization, the sputtered PZT samples were poled using corona poling and direct poling methods. As a means of comparison, commercially …

An Experimental Study Of Norton And Thule Cooking Pot Performance, Caelie Marshall Butler

Dissertations and Theses

Ceramic technology was adopted by hunter-gatherers of the Paleo-Inuit Norton tradition in the Western Arctic between 2800 and 2500 years B.P., corresponding with an increase in the use of aquatic resources. Pottery production and use continued until approximately 1,500 BP, and resumed during the Neo-Inuit Birnirk and Thule periods, approximately 1,350 years BP. The technical characteristics of Norton and Thule ceramics suggest they performed differently when used for cooking, with Norton ceramics best suited for cooking using direct or suspended heat, and Thule ceramics best suited for indirect heat. Prior experimental archaeological research has focused on Thule ceramics, with limited …

Study Of Asymptotic Velocity In The Bondi–Hoyle Accretion Flows In The Domain Of Kerr And 4-D Einstein–Gauss–Bonnet Gravities, Orhan Donmez, Fatih Dogan, Tuba Sahin

Materials Science and Engineering Faculty Research & Creative Works

Understanding the physical structures of the accreted matter very close to a black hole in quasars and active galactic nucleus (AGN) is an important milestone to constrain the activities occurring in their centers. In this paper, we numerically investigate the effects of the asymptotic velocities on the physical structures of the accretion disk around the Kerr and Einstein–Gauss–Bonnet (EGB) rapidly rotating black holes. The Bondi–Hoyle accretion is considered with a falling gas towards the black hole in an upstream region of the computational domain. Shock cones are naturally formed in the downstream part of the flow around both black holes. …

Developing Positive Thermal Coefficient (Ptc) Heaters For Solar Electric Cooking, Katarina Ivana Brekalo, Andrew Shepherd

Physics

Positive Thermal Coefficients, PTCs, are materials that abruptly change in resistance in response to changes in temperature. The purpose of this experiment is to explore the viability of using the switching type ceramic PTC thermistor as a replacement for current resistive heaters. These types of PTCs have a nonlinear change in resistance with increases in temperature. This device will be used as a temperature-controlling heating element intended to power an Insulated Solar Electric Cooker (ISEC). The ISEC is designed to cook meals throughout the day for impacted communities as an alternative cooking method that doesn’t require biofuel as an energy …