Preparation and characterization of Pr0.6Sr0.4FeO3-δ-Ce0.9Pr0.1O2-δ nanofiber structured composite cathode for IT-SOFCs

In this work, Pr_0.6Sr_0.4FeO_3-δ -Ce_0.9Pr_0.1O_2-δ (PSFO-CPO) nanofibers were synthesized by a one-step electrospin technique for use in intermediate-temperature solid oxide fuel cell (IT-SOFC) applications. PSFO-CPO nanofibers were produced with a diameter of about 100nm and lengths exceeding tens of microns. The thermal expansion coefficient (TEC) matches with standard GDC electrolytes and the resulting conductivity also satisfies the needs of IT-SOFCs cathodes. EIS analysis of the nanofiber structured electrode gives a polarization resistance of 0.072Ωcm² at 800°C, smaller than that from the powdered cathode with the same composition. The excellent electrochemical performance can be attributed to the well-constructed microstructure of the nanofiber structured cathode, which promotes surface oxygen diffusion and charge transfer processes. All the results imply that the one-step electrospin method is a facile and practical way of improving the cathode properties and that PSFO-CPO is a promising cathode material for IT-SOFCs.

Synthesis and characterization of hybrids derived from vermiculite chloropropyl and aliphatic diamines

ALVES, Ana Paula de Melo et al. Synthesis and characterization of hybrids derived from vermiculite chloropropyl and aliphatic diamines. Journal of Thermal Analysis and Calorimetry, v.87, n. 3, p.771–774, 2007.

Synthesis and characterization of lanthanum- and yttrium-doped Fe2O3 pigments

MELO, D. M. A. et al. Synthesis and charactezarion of lanthanum and yttrium doped Fe2O3 pigments. Cerâmica, São Paulo, v. 53, p. 79-82, 2007.

Thermal degradation studies on Edible Oil during Deep Fat Frying Process

Deep fat frying process is one of the widely followed cooking practices throughout the world. Cooking oils serve as a medium for frying food for transferring heat and makes fried food tasty and palatable. Frying process is a most complex process involving numerous physicochemical changes which are complicated to understand. Frying leads to thermal degradation of oil through thermo-oxidation, hydrolysis, and polymerization. Hydrolysis results in formation of free fatty acids whereas oxidation process produces hydroperoxides and small molecular carbonyl compounds. This whole process leads to the formation of polar compounds and degradation of antioxidants that further degrades frying oil. Eventually, through mass transfer process these degradation products accumulate into fried food and reduce the nutritional quality of both oil and food. Thus, the frying process is of research interest calls for detailed systematic study which is chosen for the present study. The primary objective of this study is to understand the mechanism of degradation and characterization ofdegraded products which helps in arriving at the limits for frying oil utilization in terms of number of frying cycles. The mechanistic studies and the knowledge on the degraded products help to understand the way to retard the deterioration of oil for stability and enhancement of frying cycles. The study also explores the formation of the predominant polar compounds and their structural elucidation through mass spectrometry. Oxidation of oil is another important factor that ignites the degradation phenomena. One of the best ways to increase thermal stability of any oil is addition of potent antioxidants. But, most of the natural and synthetic antioxidants are unstable and ineffective at frying temperatures. Therefore, it is necessary to screen alternative antioxidants for their activity in the refined oils which are devoid of any added antioxidants. In this context, this study discussed the efficacy of several natural and synthetic antioxidants to retard the formation of polar compounds and thermooxidation during prolonged frying conditions. Similarly, the advantage of blending of two different oils to improve the thermal stability was explored. The present study brings out the total picture on the type of degradation products formed during frying and the ways of retarding the determination to improve upon the stability of the oil and enhancement of frying cycles.

Ultrasonic Spectral Analysis for Nuclear Fuel Characterization

Ceramic materials have been widely used for various purposes in many different industries due to certain characteristics, such as high melting point and high resistance to corrosion. Concerning the areas of applications, automobile, aeronautics, naval and even nuclear, the characteristics of these materials should be strictly controlled. In the nuclear area, ceramics are of great importance once they are the nuclear fuel pellets and must have, among other features, a well controlled porosity due to mechanical strength and thermal conductivity required by the application. Generally, the techniques used to characterize nuclear fuel are destructive and require costly equipment and facilities. This paper aims to present a nondestructive technique for ceramic characterization using ultrasound. This technique differs from other ultrasonic techniques because it uses ultrasonic pulse in frequency domain instead of time domain, associating the characteristics of the analyzed material with its frequency spectrum. In the present work, 40 Alumina (Al2O3) ceramic pellets with porosities ranging from 5% to 37%, in absolute terms measured by Archimedes technique, were tested. It can be observed that the frequency spectrum of each pellet varies according to its respective porosity and microstructure, allowing a fast and non-destructive association of the same characteristics with the same spectra pellets.

Development of a Rational Characterization Method for Iowa Fly Ash, HR-286, Annual Progress Report 2, 1987

The following report summarizes research activities on the project for the period December 1, 1986 to November 30, 1987. Research efforts for the second year deviated slightly from those described in the project proposal. By the end of the second year of testing, it was possible to begin evaluating how power plant operating conditions influenced the chemical and physical properties of fly ash obtained from one of the monitored power plants (Ottumwa Generating Station, OGS). Hence, several of the tasks initially assigned to the third year of the project (specifically tasks D, E, and F) were initiated during the second year of the project. Manpower constraints were balanced by delaying full scale implementation of the quantitative X-ray diffraction and differential thermal analysis tasks until the beginning of the third year of the project. Such changes should have little bearing on the outcome of the overall project.

Pulling Back the Veil: The Characterization and Habitability of Enshrouded Worlds

Thesis (Ph.D.)--University of Washington, 2016-08

Development and characterization of Poly(L-lactic acid) (PLLA) platforms for bone tissue engineering

The development of scaffolds based on biomaterials is a promising strategy for Tissue Engineering and cellular regeneration. This work focuses on Bone Tissue Engineering, the aim is to develop electrically tailored biomaterials with different crystalline and electric features, and study their impacts onto cell biological behavior, so as to predict the materials output in the enhancement of bone tissue regeneration. It is accepted that bone exhibits piezoelectricity, a property that has been proved to be involved in bone growth/repair mechanism regulation. In addition electrical stimulations have been proved to influence bone growth and repair. Piezoelectric materials are therefore widely investigated for a potential use in bone tissue engineering. The main goal is the development of novel strategies to produce and employ piezoelectric biomaterials, with detailed knowledge of mechanisms involved in cell-material interaction. In the current work, poly (L-lactic) acid (PLLA), a synthetic semi-crystalline polymer, exhibiting biodegradibility, biocompatibility and piezoelectricity is studied and proposed as a promoter of enhanced tissue regeneration. PLLA has already been approved for implantation in human body by the Food and Drug Administration (FDA), and at the moment it is being used in several clinical strategies. The present study consists of first preparing films with different degrees of crystallinity and characterizing these PLLA films, in terms of surface and structural properties, and subsequently assessing the behavior of cells in terms of viability, proliferation, morphology and mineralization for each PLLA configuration. PLLA films were prepared using the solvent cast technique and submitted to different thermal treatments in order to obtain different degrees of crystallinity. Those platforms were then electrically poled, positively and negatively, by corona discharge in order to tailor their electrical properties. The cellular assays were conducted by using two different osteoblast cell lines grown directly onto the PLLA films:Human osteoblast Hob, a primary cell culture and Human osteosarcoma MG-63 cell line. This thesis gives also a comprehensive introduction to the area of Bone Tissue Engineering and provides a review of the work done in this field in the past until today, in that same field, including the one related with bone’s piezoelectricity. Then the experimental part deals with the effects of the crystallinity degrees and of the polarization in terms of surface properties and cellular bio assays. Three different degrees of crystallinity, and three different polarization conditions were prepared; which results in 9 different configurations under investigation.

Synthesis and characterization of hybrids derived from vermiculite chloropropyl and aliphatic diamines

ALVES, Ana Paula de Melo et al. Synthesis and characterization of hybrids derived from vermiculite chloropropyl and aliphatic diamines. Journal of Thermal Analysis and Calorimetry, v.87, n. 3, p.771–774, 2007.

Synthesis and characterization of lanthanum- and yttrium-doped Fe2O3 pigments

MELO, D. M. A. et al. Synthesis and charactezarion of lanthanum and yttrium doped Fe2O3 pigments. Cerâmica, São Paulo, v. 53, p. 79-82, 2007.

Controlling Nanostructures for in-situ TEM Characterization

Low dimensional nanostructures, such as nanotubes and 2D sheets, have unique and promising material properties both from a fundamental science and an application standpoint. Theoretical modelling and calculations predict previously unobserved phenomena that experimental scientists often struggle to reproduce because of the difficulty in controlling and characterizing the small structures under real-world constraints. The goal of this dissertation is to controlling these structures so that nanostructures can be characterized in-situ in transmission electron microscopes (TEM) allowing for direct observation of the actual physical responses of the materials to different stimuli. Of most interest to this work are the thermal and electrical properties of carbon nanotubes, boron nitride nanotubes, and graphene. The first topic of the dissertation is using surfactants for aqueous processing to fabricate, store, and deposit the nanostructures. More specifically, thorough characterization of a new surfactant, ammonium laurate (AL), is provided and shows that this new surfactant outperforms the standard surfactant for these materials, sodium dodecyl sulfate (SDS), in almost all tested metrics. New experimental set-ups have been developed by combining specialized in-situ TEM holders with innovative device fabrication. For example, electrical characterization of graphene was performed by using an STM-TEM holder and depositing graphene from aqueous solutions onto lithographically patterned, electron transparent silicon nitride membranes. These experiments produce exciting information about the interaction between graphene and metal probes and the substrate that it rests on. Then, by adding indium to the backside of the membrane and employing the electron thermal microscopy (EThM) technique, the same type of graphene samples could be characterized for thermal transport with high spatial resolution. It is found that reduced graphene oxide sheets deposited onto a silicon nitride membrane and displaying high levels of wrinkling have higher than expected electrical and thermal conduction properties. We are clearly able to visualize the ability of graphene to spread heat away from an electronic hot spot and into the substrate.

Characterization of Non-linear Polymer Properties to Predict Process Induced Warpage and Residual Stress of Electronic Packages

Nonlinear thermo-mechanical properties of advanced polymers are crucial to accurate prediction of the process induced warpage and residual stress of electronics packages. The Fiber Bragg grating (FBG) sensor based method is advanced and implemented to determine temperature and time dependent nonlinear properties. The FBG sensor is embedded in the center of the cylindrical specimen, which deforms together with the specimen. The strains of the specimen at different loading conditions are monitored by the FBG sensor. Two main sources of the warpage are considered: curing induced warpage and coefficient of thermal expansion (CTE) mismatch induced warpage. The effective chemical shrinkage and the equilibrium modulus are needed for the curing induced warpage prediction. Considering various polymeric materials used in microelectronic packages, unique curing setups and procedures are developed for elastomers (extremely low modulus, medium viscosity, room temperature curing), underfill materials (medium modulus, low viscosity, high temperature curing), and epoxy molding compound (EMC: high modulus, high viscosity, high temperature pressure curing), most notably, (1) zero-constraint mold for elastomers; (2) a two-stage curing procedure for underfill materials and (3) an air-cylinder based novel setup for EMC. For the CTE mismatch induced warpage, the temperature dependent CTE and the comprehensive viscoelastic properties are measured. The cured cylindrical specimen with a FBG sensor embedded in the center is further used for viscoelastic property measurements. A uni-axial compressive loading is applied to the specimen to measure the time dependent Young’s modulus. The test is repeated from room temperature to the reflow temperature to capture the time-temperature dependent Young’s modulus. A separate high pressure system is developed for the bulk modulus measurement. The time temperature dependent bulk modulus is measured at the same temperatures as the Young’s modulus. The master curve of the Young’s modulus and bulk modulus of the EMC is created and a single set of the shift factors is determined from the time temperature superposition. The supplementary experiments are conducted to verify the validity of the assumptions associated with the linear viscoelasticity. The measured time-temperature dependent properties are further verified by a shadow moiré and Twyman/Green test.

Thermal activation, long-range ordering, and topological frustration of artificial spin ice

Frustrated systems, typically characterized by competing interactions that cannot all be simultaneously satisfied, are ubiquitous in nature and display many rich phenomena and novel physics. Artificial spin ices (ASIs), arrays of lithographically patterned Ising-like single-domain magnetic nanostructures, are highly tunable systems that have proven to be a novel method for studying the effects of frustration and associated properties. The strength and nature of the frustrated interactions between individual magnets are readily tuned by design and the exact microstate of the system can be determined by a variety of characterization techniques. Recently, thermal activation of ASI systems has been demonstrated, introducing the spontaneous reversal of individual magnets and allowing for new explorations of novel phase transitions and phenomena using these systems. In this work, we introduce a new, robust material with favorable magnetic properties for studying thermally active ASI and use it to investigate a variety of ASI geometries. We reproduce previously reported perfect ground-state ordering in the square geometry and present studies of the kagome lattice showing the highest yet degree of ordering observed in this fully frustrated system. We consider theoretical predictions of long-range order in ASI and use both our experimental studies and kinetic Monte Carlo simulations to evaluate these predictions. Next, we introduce controlled topological defects into our square ASI samples and observe a new, extended frustration effect of the system. When we introduce a dislocation into the lattice, we still see large domains of ground-state order, but, in every sample, a domain wall containing higher energy spin arrangements originates from the dislocation, resolving a discontinuity in the ground-state order parameter. Locally, the magnets are unfrustrated, but frustration of the lattice persists due to its topology. We demonstrate the first direct imaging of spin configurations resulting from topological frustration in any system and make predictions on how dislocations could affect properties in numerous materials systems.

Characterization of nanoparticle mediated laser transfection by femtosecond laser pulses for applications in molecular medicine

Background: In molecular medicine, the manipulation of cells is prerequisite to evaluate genes as therapeutic targets or to transfect cells to develop cell therapeutic strategies. To achieve these purposes it is essential that given transfection techniques are capable of handling high cell numbers in reasonable time spans. To fulfill this demand, an alternative nanoparticle mediated laser transfection method is presented herein. The fs-laser excitation of cell-adhered gold nanoparticles evokes localized membrane permeabilization and enables an inflow of extracellular molecules into cells. Results: The parameters for an efficient and gentle cell manipulation are evaluated in detail. Efficiencies of 90% with a cell viability of 93% were achieved for siRNA transfection. The proof for a molecular medical approach is demonstrated by highly efficient knock down of the oncogene HMGA2 in a rapidly proliferating prostate carcinoma in vitro model using siRNA. Additionally, investigations concerning the initial perforation mechanism are conducted. Next to theoretical simulations, the laser induced effects are experimentally investigated by spectrometric and microscopic analysis. The results indicate that near field effects are the initial mechanism of membrane permeabilization. Conclusion: This methodical approach combined with an automated setup, allows a high throughput targeting of several 100,000 cells within seconds, providing an excellent tool for in vitro applications in molecular medicine. NIR fs lasers are characterized by specific advantages when compared to lasers employing longer (ps/ns) pulses in the visible regime. The NIR fs pulses generate low thermal impact while allowing high penetration depths into tissue. Therefore fs lasers could be used for prospective in vivo applications.

Slot Film Cooling: A Comprehensive Experimental Characterization

When components of a propulsion system are exposed to elevated flow temperatures there is a risk for catastrophic failure if the components are not properly protected from the thermal loads. Among several strategies, slot film cooling is one of the most commonly used, yet poorly understood active cooling techniques. Tangential injection of a relatively cool fluid layer protects the surface(s) in question, but the turbulent mixing between the hot mainstream and cooler film along with the presence of the wall presents an inherently complex problem where kinematics, thermal transport and multimodal heat transfer are coupled. Furthermore, new propulsion designs rely heavily on CFD analysis to verify their viability. These CFD models require validation of their results, and the current literature does not provide a comprehensive data set for film cooling that meets all the demands for proper validation, namely a comprehensive (kinematic, thermal and boundary condition data) data set obtained over a wide range of conditions. This body of work aims at solving the fundamental issue of validation by providing high quality comprehensive film cooling data (kinematics, thermal mixing, heat transfer). 3 distinct velocity ratios (VR=uc/u∞) are examined corresponding to wall-wake (VR~0.5), min-shear (VR ~ 1.0), and wall-jet (VR~2.0) type flows at injection, while the temperature ratio TR= T∞/Tc is approximately 1.5 for all cases. Turbulence intensities at injection are 2-4% for the mainstream (urms/u∞, vrms/u∞,), and on the order of 8-10% for the coolant (urms/uc, vrms/uc,). A special emphasis is placed on inlet characterization, since inlet data in the literature is often incomplete or is of relatively low quality for CFD development. The data reveals that min-shear injection provides the best performance, followed by the wall-jet. The wall-wake case is comparably poor in performance. The comprehensive data suggests that this relative performance is due to the mixing strength of each case, as well as the location of regions of strong mixing with respect to the wall. Kinematic and thermal data show that strong mixing occurs in the wall-jet away from the wall (y/s>1), while strong mixing in the wall-wake occurs much closer to the wall (y/s<1). Min-shear cases exhibit noticeably weaker mixing confined to about y/s=1. Additionally to these general observations, the experimental data obtained in this work is analyzed to reveal scaling laws for the inlets, near-wall scaling, detecting and characterizing coherent structures in the flow as well as to provide data reduction strategies for comparison to CFD models (RANS and LES).