Browsing by Author "Pickrell, Gary R."
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- Abrasive Blasting with Post-Process and In-Situ CharacterizationMills, Robert Jeffrey (Virginia Tech, 2014-07-25)Abrasive blasting is a common process for cleaning or roughening the surface of a material prior to the application of a coating. Although the process has been in practice for over 100 years, the lack of a comprehensive understanding of the complex interactions that exist with the process can still yield an inferior surface quality. Subsequently, parts can be rejected at one of many stages of the manufacturing process and/or fail unexpectedly upon deployment. The objective of this work is to evaluate the effect of selected input parameters on the characteristics of the blasted surface characteristics so that a more useful control strategy can be implemented. To characterize surface roughness, mechanical profilometry was used to collect average roughness parameter, Ra. Decreasing blast distance from 6” to 4” gave ΔRa = +0.22 µm and from 8” to 6” gave ΔRa = +0.22 µm. Increasing blast pressure from 42 psi to 60 psi decreased the Ra by 0.33 µm. Media pulsation reduced Ra by 0.56 µm and the use of new media reduced Ra by 0.47 µm. Although blasting under the same conditions and operator on different days led to ΔRa due to shorter blast times, there was no statistically significant variance in Ra attributed to blasting on different days. Conversely, a ΔRa = +0.46 µm was observed upon blasting samples with different cabinets. No significant ΔRa was found when switching between straight and Venturi nozzles or when using different operators. Furthermore, the feasibility of fiber optic sensing technologies was investigated as potential tools to provide real time feedback to the blast machine operator in terms of substrate temperature. Decreasing the blast distance from 6” to 4” led to ΔT = +9.2 °C, while decreasing the blast angle to 45° gave ΔT= -11.6 °C for 304 stainless steel substrates. Furthermore, increasing the blast pressure from 40 psi to 50 psi gave ΔT= +15.3 °C and changing from 50 psi to 60 psi gave ΔT= +9.9 °C. The blast distance change from 8” to 6” resulted in ΔT = +9.8 °C in thin stainless steel substrate temperature. The effects of substrate thickness or shape were evaluated, giving ΔT= +7.4 °C at 8” distance, ΔT= +20.2 °C at 60 psi pressure, and ΔT= -15.2 °C at 45° blasting when comparing thin stainless steel against 304 stainless steel (thick) temperatures. No significant ΔT in means was found when going from 6” to 8” distance on 304 stainless steel, 40 psi and 60 psi blasting of thin SS, as well as angled and perpendicular blasting of thin SS. Comparing thick 304 and thin stainless steel substrates at a 6” blast distance gave no significant ΔT.
- Acid Leaching of SHS Produced MgO/TiB2Lok, Jonathan Y. (Virginia Tech, 2006-10-10)The stoichiometric Self-propagating High-temperature Synthesis (SHS) thermite reaction involving magnesium oxide (MgO), titanium dioxide (TiO₂), and boron oxide (B₂O₃) forms titanium diboride (TiB₂) and MgO as final products. Selective acid leaching is used to remove the MgO leaving high purity TiB₂ powder. The SHS method to produce TiB₂ is attractive because of the relatively low temperature required to initiate the reaction, fast reaction time, and product purity. This study investigates the acid leaching of SHS produced MgO/TiB2 and a stoichiometric mixture of commercial MgO and TiB₂ powders. Leaching was conducted at 90° C, 60° C, and 30° C at pH levels of 4.0, 2.5, and 1.0 by introduction of concentrated aliquots of HNO₃. This method maintains a minimum pH target throughout the leaching process, thereby sustaining a dynamic concentration to remove the oxide. The optimal leaching conditions were determined to be at 90° C at a minimum pH target of 2.5 for the SHS produced product. At these conditions, conversion percentages of 83%-84% of MgO were measured with only trace amounts of TiB2 measured in the solution (less than 100 ppm). Conversion percentages for each leaching condition and dissolution mass of solid MgO and TiB₂ at each pH are also reported. Results from powder XRD confirm the removal of MgO and minimal dissolution of TiB₂, and indicate the formation of unidentified compounds. Inductively coupled plasma mass spectrometry (ICP) was used to analyze the ionic composition and extent of leaching. Scanning electron microscopy (SEM) was used to observe the particle morphology of the leached powders.
- Acoustic Waveguides and Sensors for High Temperature and Gamma Radiation EnvironmentHe, Jiaji (Virginia Tech, 2021-01-12)Sensing in harsh environments is always in great need. Although many sensors and sensing systems are reported, such as optical fiber sensors and acoustic sensors, they all have drawbacks. In this dissertation, fused quartz and sapphire acoustic waveguides and sensors are developed for high temperature and heavy gamma radiation. The periodic structure, acoustic fiber Bragg grating (AFBG), is the core sensor structure in this dissertation. To better analyze the propagation of acoustic waves, the acoustic coupled more analysis is proposed. It could solve for the reflection spectrum of the AFBG with at most 2.1% error. For the waveguide, the fused quartz "suspended core" waveguide is designed. It achieved strong acoustic energy confinement so surface perturbations no longer affected the wave propagation. Single crystal sapphire fiber features low acoustic loss, and survivability under high temperature. It is also chosen as an acoustic waveguide. AFBGs are fabricated in both waveguides. The fused quartz suspended core AFBG is shown to sense temperature up to 1000 C and to have stable reading at 700 C for 14 days. The sapphire AFBG as a temperature sensor works up to 1500 C and also provides continuous stable reading at 1100 C for 12 days. Both waveguides with AFBGs are then tested under long-term gamma radiation. Despite some fluctuations from radiation-related causes, the readings of both sensors generally remain stable. Given the experimental observations, the fused quartz AFBG waveguide and the sapphire AFBG waveguide are shown to work well in high temperature and gamma radiations.
- Adaptive Process Control for Achieving Consistent Mean Particles' States in Atmospheric Plasma Spray ProcessGuduri, Balachandar (Virginia Tech, 2022-02-08)The coatings produced by an atmospheric plasma spray process (APSP) must be of uniform quality. However, the complexity of the process and the random introduction of noise variables such as fluctuations in the powder injection rate and the arc voltage make it difficult to control the coating quality that has been shown to depend upon mean values of powder particles' temperature and speed, collectively called mean particles' states (MPSs), just before they impact the substrate. Here we use a science-based methodology to develop an adaptive controller for achieving consistent MPSs. We first identify inputs into the APSP that significantly affect the MPSs, and then formulate a relationship between these two quantities. When the MPSs deviate from their desired values, the adaptive controller based on the model reference adaptive controller (MRAC) framework is shown to successfully adjust the input parameters to correct them. The performance of the controller is tested via numerical experiments using the software, LAVA-P, that has been shown to well simulate the APSP. The developed adaptive process controller is further refined by using sigma (σ) adaptive laws and including a low-pass filter that remove high-frequency oscillations in the output. The utility of the MRAC controller to achieve desired locations of NiCrAlY and zirconia powder particles for generating a 5-layered coating is demonstrated. In this case a pure NiCrAlY layer bonds to the substrate and a pure zirconia makes the coating top. The composition of the intermediate 3 layers is combination of the two powders of different mass fractions. By increasing the number of intermediate layers, one can achieve a continuous through-the-thickness variation of the coating composition and fabricate a functionally graded coating.
- Adaptive process control for achieving consistent particles' states in atmospheric plasma spray processGuduri, B.; Cybulsky, Michael; Pickrell, Gary R.; Batra, Romesh C. (2021-02-08)The coatings produced by an atmospheric plasma spray process (APSP) must be of uniform quality. However, the complexity of the process and the random introduction of noise variables such as fluctuations in the powder injection rate and the arc voltage make it difficult to control the coating quality that has been shown to depend upon mean values of powder particles' temperature and speed, collectively called mean particles' states (MPSs), just before they impact the substrate. Here, we use a science-based methodology to develop a stable and adaptive controller for achieving consistent MPSs and thereby decrease the manufacturing cost. We first identify inputs into the APSP that significantly affect the MPSs and then formulate a relationship between these two quantities. When the MPSs deviate from their desired values, the adaptive controller is shown to successfully adjust the input parameters to correct them. The performance of the controller is tested via numerical experiments using the software, LAVA-P, that has been shown to well simulate the APSP.
- The Adhesion Strength of a Plasma Sprayed Silicon Bond Coating on a Silicon Carbide Ceramic Matrix CompositeScherbarth, Austin Daniel (Virginia Tech, 2020-10-19)Silicon-based ceramics and ceramic matrix composites (CMCs), such as silicon carbide (SiC) fiber reinforced SiC, are promising candidates for hot section components in next generation turbine engines. Environmental barrier coatings (EBCs) are essential for implementing these components as they insulate and protect the substrate from reaction with water vapor in the engine environment. EBCs are typically deposited via atmospheric plasma spraying (APS) and preparing the component surfaces through cleaning and roughening prior to coating is a vital step to ensure sufficient coating adhesion. The adhesion of a plasma sprayed coating to the underlying component is one of the most important properties as the component will not be protected if the coating is not well adhered. Surface roughening of metallic components via grit blasting is well documented and understood, but much less is known about preparing ceramic and ceramic composite surfaces for thermal spray coating. Silicon coatings are often used as a bond coating between SiC-based components and EBC top layers, but the adhesion strength of plasma sprayed Si on these substrates, Si splat formation and the factors that affect coating formation and adhesion have not been well studied. The effects of automated grit blasting process parameters on surface roughness and material loss of a reaction bonded SiC (rb SiC) composite were evaluated. Surface roughness before and after grit blasting was evaluated with a confocal laser scanning microscope. The differences and advantages of automated grit blasting compared to manual grit blasting were observed. Most notably was the level of control at high nozzle traverse speeds resulting in reduction of material loss and consistency of roughening. At high nozzle traverse speeds, the amount of material loss decreased greatly with a small effect on induced surface roughness. The degree of grit blasting induced roughness and material loss was found to be largely dependent on the nature of the composite matrix and reinforcement, as well as blast nozzle traverse speed. A statistical model was developed to predict the substrate thickness loss and induced average roughness based on nozzle traverse speed and blast pressure for automated grit blasting. Additionally, laser ablation was used to create controlled, regularly patterned surface texture on rb SiC substrates to further investigate the role of texture parameters in Si coating adhesion. Si was plasma sprayed onto rb SiC substrates to deposit both thick coatings to evaluate adhesion strength and single splats to study splat formation. Surface roughness/texture, substrate preheat temperature and mean Si particle size were varied in plasma spray coating experiments to observe their role in coating adhesion strength. Si adhesion strength was found to be related to all three factors and a statistical model was developed to predict adhesion strength based on them. Substrate preheat temperature had a significant effect on both Si adhesion strength and Si splat formation on rb SiC. Single splat formation during plasma spraying of Si on SiC was simulated with software called SimDrop. Simulations of Si droplet impact, spreading and solidification during plasma spraying on smooth and textured SiC surfaces were used to investigate the effects of relevant process parameters on splat formation. Experimentally observed Si splats on smooth substrates at different temperatures during deposition were matched with simulated splats with the same spraying parameters. A change in thermal contact resistance with changing substrate preheat temperature was confirmed by the simulation results. The role of surface texture parameters for a regularly patterned surface texture in splat formation was demonstrated through simulation. This dissertation investigates methods of roughening and preparing a SiC composite substrate for plasma spray coating, as well as factors which affect the adhesion strength and splat formation of plasma sprayed Si through experiments and simulation. The observations made provide valuable insight for understanding and optimizing the manufacturing processes utilized to deposit strongly adhered coatings onto SiC-based composites. In addition, areas of interest in this field for future study and further investigation are introduced and suggested.
- Analysis of component having engineered internal space for fluid flow(United States Patent and Trademark Office, 2019-04-30)A characteristic of a component having an engineered internal space can be analyzed by recording acoustic signals produced by fluid flow through the internal space at controlled flow rates, and determining one or more acoustic frequencies and acoustic intensities that are indicative of the characteristic of the component. A state and/or a source of the component can be predicted based on the results of such analysis.
- Analysis of Strength Variation in Glass Due to Ion ExchangeKulp, Andrew Brooks (Virginia Tech, 2012-05-21)The main goal of this project was to compare the changes in statistical variation and Weibull characteristics of the strength of glass rods as modified by heat treatment with and without an ion exchange bath. Several sample groups of 30 sodium borosilicate glass rod specimens were heat treated at various temperatures in air and in a potassium nitrate salt bath to induce an ion exchange process. All samples were then tested to failure in 4-point bending to assess the resulting Modulus of Rupture (MOR). Statistical analysis techniques and Weibull analysis were used to study the variations which occur within and between strength distributions of each sample group. A smaller sampling of test groups was subjected to fractographic analysis to study the effect of ion exchange on fracture features. The data shows that the ion exchange process caused a statistically significant increase in the strength of the glass rods. Samples which were heat treated do not show any significant changes in average strength. The fractographic analysis suggests that no changes in fracture morphology occurred as a result of ion exchange process, and that the critical flaw size population was not significantly different.
- Application of Sapphire-Fiber-Bragg-Grating-Based Multi-Point Temperature Sensor in Boilers at a Commercial Power PlantYang, Shuo; Homa, Daniel S.; Heyl, Hanna; Theis, Logan; Beach, John; Dudding, Billy; Acord, Glen; Taylor, Dwyn; Pickrell, Gary R.; Wang, Anbo (MDPI, 2019-07-21)Readily available temperature sensing in boilers is necessary to improve efficiencies, minimize downtime, and reduce toxic emissions for a power plant. The current techniques are typically deployed as a single-point measurement and are primarily used for detection and prevention of catastrophic events due to the harsh environment. In this work, a multi-point temperature sensor based on wavelength-multiplexed sapphire fiber Bragg gratings (SFBGs) were fabricated via the point-by-point method with a femtosecond laser. The sensor was packaged and calibrated in the lab, including thermally equilibrating at 1200 °C, followed by a 110-h, 1000 °C stability test. After laboratory testing, the sensor system was deployed in both a commercial coal-fired and a gas-fired boiler for 42 days and 48 days, respectively. The performance of the sensor was consistent during the entire test duration, over the course of which it measured temperatures up to 950 °C (with some excursions over 1000 °C), showing the survivability of the sensor in a field environment. The sensor has a demonstrated measurement range from room temperature to 1200 °C, but the maximum temperature limit is expected to be up to 1900 °C, based on previous work with other sapphire based temperature sensors.
- Behavior of Random Hole Optical Fibers under Gamma Ray Irradiation and Its Potential Use in Radiation Sensing ApplicationsAlfeeli, Bassam; Pickrell, Gary R.; Garland, Marc; Wang, Anbo (MDPI, 2007-05-24)Effects of radiation on sensing and data transmission components are of greatinterest in many applications including homeland security, nuclear power generation, andmilitary. A new type of microstructured optical fiber (MOF) called the random hole opticalfiber (RHOF) has been recently developed. The RHOFs can be made in many differentforms by varying the core size and the size and extent of porosity in the cladding region.The fibers used in this study possessed an outer diameter of 110 _m and a core ofapproximately 20 _m. The fiber structure contains thousands of air holes surrounding thecore with sizes ranging from less than 100 nm to a few _m. We present the first study ofthe behavior of RHOF under gamma irradiation. We also propose, for the first time to ourknowledge, an ionizing radiation sensor system based on scintillation light from ascintillator phosphor embedded within a holey optical fiber structure. The RHOF radiationresponse was compared to normal single mode and multimode commercial fibers(germanium doped core, pure silica cladding) and to those of radiation resistant fibers (puresilica core with fluorine doped cladding fibers). The comparison was done by measuringradiation-induced absorption (RIA) in all fiber samples at the 1550 nm wavelength window(1545 25 nm). The study was carried out under a high-intensity gamma ray field from a 60Co source (with an exposure rate of 4x104 rad/hr) at an Oak Ridge National Laboratory gamma ray irradiation facility. Linear behavior, at dose values less than 106 rad, was observed in all fiber samples except in the pure silica core fluorine doped cladding fiber which showed RIA saturation at 0.01 dB. RHOF samples demonstrated low RIA (0.02 and 0.005 dB) compared to standard germanium doped core pure silica cladding (SMF and MMF) fibers. Results also showed the possibility of post-fabrication treatment to improve the radiation resistance of the RHOF fibers.
- Characterization Study of Plasma Spray Attachment of Intrinsic Fabry-Perot Interferometric Sensors in Power Generation ApplicationsKrause, Amanda Rochelle (Virginia Tech, 2012-06-11)The purpose of this study is to characterize the plasma spray deposits used for attaching intrinsic Fabry-Perot interferometric fiber optic strain sensors. The deposits must maintain adhesion at elevated temperatures without distorting the sensors' signals. Two different material systems were tested and modeled, a nickel based alloy and yttria-stabilized zirconia. The material properties of the deposits and the thermal stresses in the system were evaluated to determine attachment lifetime of the sensors. The encapsulated sensors' signals were collected before and after plasma spraying and at elevated temperatures. The material properties of the deposits were evaluated by electron microscopy, energy dispersive x-ray spectroscopy, scratch testing, thermal fatigue testing, and nanoindentation. The thermal stresses were evaluated by Raman spectroscopy and from finite element analysis in COMSOL® Multiphysics®. Several of the sensors broke during encapsulation due to the plasma spray processing conditions and the signals experienced distortion at elevated temperatures. The sensors can be treated to remove this interference to allow for this deposit attachment. The nickel based alloy's ductility and lamellar microstructure allowed for non catastrophic relaxation mechanisms to relieve induced thermal stresses. The yttria stabilized zirconia failed catastrophically at elevated temperatures due its lack of compliance to mismatches in thermal expansion. A high melting point metallic deposit, similar to the nickel based alloy, is desirable for fiber optic sensor attachment due to its ductility, thermal expansion, and dominant relaxation mechanisms. The processing conditions may need to be optimized to allow for the sensors' protection during encapsulation.
- Coupled Mode Analysis for 3D Stress-Free Elastic Acoustic WaveguideHe, Jiaji; Homa, Daniel S.; Pickrell, Gary R.; Wang, Anbo (IEEE, 2019)Acoustic sensors and acoustic measurements receive much attention in various applications. Because waveguides are commonly used in sensor design, theoretical means to study acoustic propagation and interaction in waveguides are necessary. However, current methods for elastic wave coupling, including the transfer matrix method and coupled mode theory in planar 2D waveguides, are not satisfactory. In this work, a coupled mode analysis for acoustic waves in 3D stress-free elastic waveguides is proposed. Similar to the coupled mode theory in optical waveguides, the analysis is presented by the evolution of modal amplitudes. It can solve various modal conversion and scattering problems in elastic waveguides with small changes of cross sections and stress-free boundaries. To demonstrate the practicability, the coupled mode analysis is used to calculate the reflection spectrum of the newly proposed structure, the acoustic fiber Bragg grating. In a notch-based grating fabricated on a thin cylindrical waveguide, the results from coupled mode analysis are in good agreement with those from the transfer matrix method, which has been already validated experimentally. The coupled mode analysis is a promising method to solve various scattering problems.
- Crystallization of Lithium Disilicate Glass Using Variable Frequency Microwave ProcessingMahmoud, Morsi Mohamed (Virginia Tech, 2007-04-24)The lithium disilicate (LS2) glass system provides the basis for a large number of useful glass-ceramic products. Microwave processing of materials such as glass-ceramics offers unique benefits over conventional processing techniques. Variable frequency microwave (VFM) processing is an advanced processing technique developed to overcome the hot spot and the arcing problems in microwave processing. In general, two main questions are addressed in this dissertation: 1. How does microwave energy couple with a ceramic material to create heat? and, 2. Is there a "microwave effect" and if so what are the possible explanations for the existence of that effect? The results of the present study show that VFM processing was successfully used to crystallize LS2 glass at a frequency other than 2.45 GHz and without the aid of other forms of energy (hybrid heating). Crystallization of LS2 glass using VFM heating occurred in a significantly shorter time and at a lower temperature as compared to conventional heating. Furthermore, the crystallization mechanism of LS2 glass in VFM heating was not exactly the same as in conventional heating. Although LS2 crystal phase (Orthorhombic Ccc2) was developed in the VFM crystallized samples as well as in the conventionally crystallized samples as x-ray diffraction (XRD) confirmed, the structural units of SiO4 tetrahedra (Q species) in the VFM crystallized samples were slightly different than the ones in conventionally crystallized samples as the Raman spectroscopy revealed. Moreover, the observed reduction in the crystallization time and apparent temperature in addition to the different crystallization mechanism observed in the VFM process both provided experimental evidence to support the presence of the microwave effect in the LS2 crystallization process. Also, the molecular orbital model was successfully used to predict the microwave absorption in LS2 glass and glass-ceramic. This model was consistent with experiments and indicated that microwave-material interactions were highly dependent on the structure of the material. Finally, a correlation between the Fourier transform infrared reflectance spectroscopy (FTIRRS) peak intensities and the volume fraction of crystals in partially crystallized LS2 glass samples was established.
- Cure Kinetics of Two Part Epoxy Resin and the Effect on Characterization of Thermal Barrier CoatingsChang, Sunny (Virginia Tech, 2015-05-28)The aerospace industry strives to develop new methods of refining gas turbine engines by increasing power and thermal efficiencies while simultaneously reducing cost. Turbine engines operate under high temperatures and therefore thermal barrier coatings (TBCs) composed of yttria-stabilized zirconia (YSZ) play an important role in improving the performance of the components that make up the engine. Failure of the TBC could lead to catastrophic events, thus requiring consistent and accurate characterization for supplier qualification and production quality assurance. However, due to porosity and the anisotropic behavior of the coating and variability in processing of TBCs, consistent characterization has proven to be extremely challenging. One of the reoccurring issues is the inconsistency in measuring percent porosity, which stems from the difficulty in distinguishing filled pores from damaged, unfilled voids. Sample preparation of TBCs involves sectioning, mounting, grinding, polishing, and characterization. Eliminating variability in characterization begins with mounting which is a critical step to protect the surface integrity and edge retention of the coating during grinding and polishing. The curing kinetics of a slow cure two part epoxy was investigated and the TBC samples were mounted and cured at heating rates of 2, 5, and 10°C/min to 55°C and 70°C. Grinding and polishing procedures simulated industry practices followed by characterization with optical microscopy. Results showed that heating rates of 2°C/min to 55°C and 70°C have the best impregnation properties while uncontrolled or high heating rates of 10°C/min had an increase in the amount of pullouts and lack of infiltration from the epoxy. The curing kinetics of the epoxy needs to be controlled to eliminate the ambiguity of filled and unfilled pores.
- Damping Behavior in Ferroelectric Reinforced Metal Matrix CompositesPoquette, Ben David (Virginia Tech, 2005-04-29)Ferroelectric-reinforced metal matrix composites (FR-MMCs) show promise as high damping materials for structural applications. Most structural materials are valued based on their stiffness and strength; however, stiff materials typically have limited inherent ability to dampen mechanical or acoustic vibrations. The addition of ferroelectric ceramic particles may also augment the strength of the matrix, creating a multifunctional composite. In this work, the damping behavior of FR-MMCs created by the addition of barium titanate (BaTiO3) discontinuous reinforcement in a bearing bronze (Cu-10w%Sn) matrix has been studied. It has been shown that even when combined with other traditional composite mechanisms, added damping ability has been achieved due to the ferroelectric nature of the reinforcement. FR-MMCs currently represent a material system capable of exhibiting increased damping ability, as compared to the structural metal matrix alone.
- Design and Evaluation of Off-centered Core Fiber for Gas SensingSu, Xu (Virginia Tech, 2020-07-13)Gas Sensing Has Become a Very Important and Attractive Technique Because of Its Various Applications, Such as in the Increasingly Concerning Case of Environmental Issues, Automobile Emission Detection, Natural Gas Leakage Detection, Etc. It Also Has Significant Applications in Industries, Such as Safety and Health Monitoring in Underground Mines. Among Those Sensing Areas, Fiber-optic Sensors Have Drawn Considerable Attention Because of Its Small Size, Light Weight, High Sensitivity, and Remote Sensing Capability. However, Current Fiber-optic Gas Sensing Techniques Have Several Limitations on Their Potential for Multiplexed or Distributed Sensing Due to Difficulties Such as High Complexity or Large Loss. To Accomplish the Goal for Multiplexed Gas Sensing, an Off-centered Core Fiber Design Is Investigated. The Eccentric Core Can Reduce Attenuation, Keep Mechanical Strength, and Lower Fabrication Cost. To Verify the Feasibility of the Design, Fiber Field Distribution Is First Studied in Simulation, Which Will Be Discussed in Detail in Chapter 2. Then Two Fiber Samples with a Length of 10 Cm and 40 Cm Are Prepared and Placed in a Custom Methane Sensing System for Gas Absorption Testing, Which Is Detailed in Chapter 3. From Etching Analysis, Localized Surface Defects Are Found as the Main Reason for Power Loss. Performance Such as Detection Resolution and Sensitivity Are Investigated. In Chapter 4, Theoretical Evaluations Have Been Conducted for Multiplexed Sensors Performances Using the Off-centered Core Fiber to Study the Impact Fiber Parameters on Sensing System Design. The Conclusion and Summary Are Presented in Chapter 5.
- Design, Synthesis and Characterization of Porous Silica Nanoparticles and Application in Intracellular Drug DeliveryMunusamy, Prabhakaran (Virginia Tech, 2010-06-29)Nanoparticle mediated drug delivery approaches provide potential opportunities for targeting and killing of intracellular bacteria. Among them, the porous silica nanoparticles deserve special attention due to their multifunctional properties such as high drug loading, controlled drug release and targeting of organs/cells. A review of the functional requirements of an ideal drug delivery system is provided. A general comparison between different drug delivery carriers and key issues to be addressed for intracellular drug delivery is discussed. Acid catalyzed and acid-base catalyzed, sol-gel derived, silica xerogel systems were investigated for sustained release of an aminoglycosides antimicrobial against salmonella infection in a mouse model. The release of gentamicin from the inner hollow part of the carrier is delayed. Further, the higher porosity of the acid–base catalyzed silica xerogel allows for high drug loading compared to the acid catalyzed silica xerogel system. Efficacy of these particles in killing intracellular bacteria (salmonella) was determined by administering three doses of porous silica loaded gentamicin. This proved to be useful in reducing the salmonella in the liver and spleen of infected mice. Furthermore, the presence of silanol groups provides the ability to functionalize the silica xerogel system with organic groups, poly (ethylene glycol) (PEG), to further increase the hydrophilicity of the silica xerogel matrix and to modify the drug release properties. Increase in the hydrophilicity of the matrix allows for faster drug release rate. In order to facilitate controlled drug release, magnetic porous silica xerogels were fabricated by incorporating iron particles within the porous silica. The particles were fabricated using an acid-base catalyzed sol-gel technique. The in-vitro drug release studies confirm that the release rate can be changed by the magnetic field "ON-OFF" mechanism. This novel drug release methodology combined with the property of high drug loading capacity proves to be influential in treating salmonella intracellular bacteria. The potential application of any drug delivery carrier relies on the ability to deliver the requisite drug without adversely affecting the cells over the long term. We have developed silica/calcium nanocomposites and evaluated their solubility behavior. The solubility of particles was characterized by particle size measurements for different periods of time. It was found that the solubility behaviour of the silica/calcium particles was dependent on their calcium content. The results obtained demonstrate the potential to use mesoporous silica/calcium nano-composites for drug delivery applications. The significant contribution of this research to drug delivery technology is on design and development of the novel porous core-shell silica nano-structures. This new core-shell nano-structure combines all the above mentioned properties (high drug loading, magnetic field controlled drug release, and solubility). The main aim of preparing these porous core-shell particles is to have a control over the solubility and drug release property, which is a significant phenomenon, which has not been achieved in any other drug delivery systems. The shell layer acts as a capping agent which dissolves at a controllable rate. The rate at which the shell layer dissolves depends on the composition of the particles. This shell prevents the drug "leakage" from the particles before reaching the target site. The core layer drug loading and release rate was modified by application of a magnetic field. Additionally, inclusion of the calcium ions in the core layer destabilizes the silica network and allows the particles to dissolve at an appropriate rate (which can be controlled by the concentration of the calcium ions).
- Determination of Surface Free Energies and Aspect Ratio of TalcLobato, Emilio Marcus de Castro (Virginia Tech, 2004-11-12)Microcalorimetric measurements and contact angle measurements were conducted to assess the surface chemistry of the mineral talc. The contact angles were performed on both flat and powdered samples and the results were used to determine the surface free energy components and parameters (SFEC) using the acid-base theory for solids, according to the van Oss-Chaudhury-Good approach. It was found that the surface hydrophobicity of talc increases with decreasing particle size up to a limit after which hydrophilicity (polarity) increases. The increase in hydrophobicity was attributed to the increase of the delamination of the lamellar talc particles. Delamination is a comminution mechanism that preferentially exposes talc's hydrophobic basal planes, while fracture is another mechanism that breaks the lamellae, rupturing covalent bonds thus exposing more hydrophilic edge surfaces. The decrease in hydrophobicity, beyond a given particle size, could be related to the prevail of fracture over delamination during grinding which generated more hydrophilic edge surfaces. The flow microcalorymetry combined with thin layer wicking allowed the separate estimation of the SFEC at the basal plane and edge surfaces of talc. The results suggested that the basal surface of talc is monopolar basic, while the edge surface is monopolar acidic, which are in agreement with the crystal structure of the mineral. The combination of two particle size distribution techniques, which are based on different physical principles, permitted the quantitative determination of the aspect ratio of highly anisometric particles, such as talc. The same trend obtained using flow microcalorimetry was observed for the evolution of the aspect ratio as a function of particle fineness, i.e. the fracture prevails over delamination after achieving a maximum aspect ratio value of about 35. The agreement between two distinct methods was considered rather encouraging.
- Determining the Role of Porosity on the Thermal Properties of Graphite FoamMueller, Jennifer Elizabeth (Virginia Tech, 2008-07-10)Graphite foams have high bulk thermal conductivity and low density, making them an excellent material for heat exchanger applications. This research focused on the characterization of graphite foams under various processing conditions (different foaming pressures and particle additions), specifically studying the effects of porosity on the thermal properties. The characterization of the foams included measuring cell sizes, percent open porosity, number of cells per square inch, bulk density, Archimedes density, compression strength, thermal conductivity, thermal resistance, and permeability. Several relationships between the structure and properties were established, and a recommendation for the processing conditions of graphite foams for the use in heat exchangers was determined.
- Development of "Core-Suction" Technique for Fabrication of Highly Doped Fibers for Optical Amplification and Characterization of Optical Fibers for Raman AmplificationGoel, Nitin Kumar (Virginia Tech, 2005-10-11)This thesis presents a novel technique named "Core Suction" for fabricating optical fiber preforms for manufacturing highly doped fibers (HDFs) for optical amplification (Raman effect based or Erbium fiber based). The technique involves drawing the molten non-conventional core glass material into the silica cladding tube to form the preform. The developed technique is simple, inexpensive and shows great potential for fabricating preforms of highly nonlinear non-conventional multi-component glasses as the core material. Preforms were made with various core glasses such as Schott SF6, Lead-Tellurium-Germanate, Lead-Tellurium-Germanate- Neodymium -Erbium and MM2 in silica cladding tubes and then pulled into fibers. The fabricated fibers were measured for refractive index profile, loss spectrum and spontaneous Raman spectra. Elemental analysis of the fiber samples was also performed using an electron microprobe. Erbium doped fiber amplifiers (EDFAs) were setup using 30 cm, 5cm and 1 cm lengths of fabricated erbium doped fibers and their gain spectra measured. The distributed gain spectrum for an EDFA was also measured using an optical frequency domain reflectometery (OFDR) technique. Commercial dispersion compensated fiber (DCF) with very high GeO2 doping was used to setup a Raman amplifier and the gain spectrum measured. One of the needs of Raman amplification in optical fibers is to predict an accurate Raman gain, based on the fiber's refractive index profile. A method of predicting Raman gain in GeO2 doped fibers is presented and the predicted Raman gain values are compared with the measured ones in the same fibers. Raman gain issues like the dependence of the Raman gain on the GeO2 concentration, polarization dependence were taken into account for the gain calculations. An experimental setup for Raman gain measurements was made and measurement issues addressed. Polarization dependence of the Raman gain in one kilometer of polarization maintaining fiber was also measured.