Spelling suggestions: "subject:"stabilized zirconium""
11 |
Electrophoretic deposition of yttria-stabilized zirconia for application in thermal barrier coatingsGuo, Fangwei January 2012 (has links)
Electrophoretic deposition (EPD) has been used to produce the yttria-stabilized zirconia (YSZ) coatings on metal substrates. Sintering of YSZ with and without doping has been carried out at 1150 °C for 2hrs. The properties of these coatings have been examined in light of thermal barrier applications. For EPD, the green density increases with an initial increase in the HCl concentration and the EPD time. This suggests that particle packing was influenced by a time dependent re-arrangement, in addition to the initial suspension dispersion state. The green density peaks at a electrical conductivity of around 10×10-4 S/m achieved by an 0.5 mM HCl addition for the 20 g/l suspensions with the EPD time of around 8 ~10 minute. For sintered coatings, the HCl concentration had a marked effect on the neck size to grain size ratio of the 8 mol% yttria-stabilized zirconia (8YSZ) coatings. The presence of ZrCl4 and ZrOCl2, and a high concentration of oxygen vacancies at the grain boundaries are believed to promote neck growth in the early stage of sintering at 1150 °C. During sintering of 3 mol% and 8 mol% yttria-stabilized zirconia (3YSZ and 8YSZ) at 1150 ºC for 2hrs, the densification rate substantially increased with a small amount of Fe2O3 addition (0.5 mol%) to the 3YSZ/8YSZ deposits. A more pronounced graingrowth was present in the Fe2O3 doped 8YSZ deposits. The increased Zr4+ diffusion coefficient is mainly responsible to the rapid densification rate of the Fe2O3 doped 3YSZ/8YSZ deposits. A small grain growth observed in the Fe2O3 doped 3YSZ deposits is attributed to the Fe3+ segregation at grain boundary. A small amount of CeO2 doping was found to substantially inhibit the densification rate of the doped 3YSZ deposits with a minor grain growth. Fe2O3 doping reduced the thermal conductivities of 3YSZ/8YSZ. It is found that Rayleigh-type phonon scattering due to the mass difference alone is inadequate to explain the thermal conductivity of Fe2O3 doped YSZ systems. The lattice strain effects due to the ionic radius difference could more effectively reduce thermal conductivity of the Fe2O3-doped 3YSZ. A decrease in the growth rate of the TGO scale with the increasing Fe2O3 additions was observed for the oxidized FeCrAlY metal substrates with the Fe2O3-doped 3YSZ coating, which was found to be attributed to the early formation of the stable and dense α-Al2O3 phase due to the presence of Fe3+ ions.
|
12 |
Electrochemical Promotion of Gold Nanoparticles Supported on Yttria-Stabilized ZirconiaKim, Jong Min January 2011 (has links)
The feasibility of highly dispersed gold nanocatalyst supported on yttria-stabilized zirconia (YSZ) for the model reactions of C2H4 and CO oxidation is demonstrated for the first time. Gold nanoparticles are synthesized on YSZ powder by chemical reduction of the precursor salt in the mixture of ethanol, water and polyvinylpyrrolidone (PVP). Resulting metal loading of the catalysts are 1 wt.% with average particle sizes ranging from 6 to 9 nm. Results of CO and C2H4 oxidation display catalytic activity at 65 0C and 25 0C for CO and C2H4 oxidation, respectively. The catalytic properties of the catalysts are different due to their average particle size. Electrochemical Promotion of Catalysis (EPOC) of C2H4 oxidation is demonstrated. Application of constant potential difference between two electrodes in the bipolar electrochemical cell led to increase in C2H4 conversion. A proposed mechanism explains the bipolar EPOC phenomenon through formation of O2- flux across the electrochemical cell, resulting in the change of Work Function of gold nanoparticles placed in between the electrodes and is electronically isolated.
|
13 |
Solid-State Yttria-Stabilized Zirconia Electrochemical Sensors for Extreme EnvironmentsPeters, Travis L. 23 October 2019 (has links)
No description available.
|
14 |
Investigations in the Mechanism of Carbothermal Reduction of Yttria Stabilized Zirconia for Ultra-high Temperature Ceramics Application and Its Influence on Yttria Contained in ItSondhi, Anchal 05 1900 (has links)
Zirconium carbide (ZrC) is a high modulus ceramic with an ultra-high melting temperature and, consequently, is capable of withstanding extreme environments. Carbon-carbon composites (CCCs) are important structural materials in future hypersonic aircraft; however, these materials may be susceptible to degradation when exposed to elevated temperatures during extreme velocities. At speeds of exceeding Mach 5, intense heating of leading edges of the aircraft triggers rapid oxidation of carbon in CCCs resulting in degradation of the structure and probable failure. Environmental/thermal barrier coatings (EBC/TBC) are employed to protect airfoil structures from extreme conditions. Yttria stabilized zirconia (YSZ) is a well-known EBC/TBC material currently used to protect metallic turbine blades and other aerospace structures. In this work, 3 mol% YSZ has been studied as a potential EBC/TBC on CCCs. However, YSZ is an oxygen conductor and may not sufficiently slow the oxidation of the underlying CCC. Under appropriate conditions, ZrC can form at the interface between CCC and YSZ. Because ZrC is a poor oxygen ion conductor in addition to its stability at high temperatures, it can reduce the oxygen transport to the CCC and thus increase the service lifetime of the structure. This dissertation investigates the thermodynamics and kinetics of the YSZ/ZrC/CCC system and the resulting structural changes across multiple size scales. A series of experiments were conducted to understand the mechanisms and species involved in the carbothermal reduction of ZrO2 to form ZrC. 3 mol% YSZ and graphite powders were uniaxially pressed into pellets and reacted in a graphite (C) furnace. Rietveld x-ray diffraction phase quantification determined that greater fractions of ZrC were formed when carbon was the majority mobile species. These results were validated by modeling the process thermochemically and were confirmed with additional experiments. Measurements were conducted to examine the effect of carbothermal reduction on the bond lengths in YSZ and ZrC. Subsequent extended x-ray absorption fine structure (EXAFS) measurements and calculations showed Zr-O, Zr-C and Zr-Zr bond lengths to be unchanged after carbothermal reduction. Energy dispersive spectroscopy (EDS) line scan and mapping were carried out on carbothermaly reduced 3 mol% YSZ and 10 mol% YSZ powders. Results revealed Y2O3 stabilizer forming agglomerates with a very low solubility in ZrC.
|
15 |
Processing of Cubic Stabilized Zirconia Electrolyte Membranes For Electrolyte-Supported Single Cell Solid Oxide Fuel Cells Using Tape CastingCoronado Rodriguez, Arturo 01 January 2018 (has links)
Electrochemical conversion devices are a developing technology that prove to be a viable and more efficient alternative to current environmentally friendly generation devices. As such, constant research has been done in the last few decades to increase their applications and reliability. One of these systems, and the focus of this research, is the single cell Solid Oxide Fuel Cell (SOFC). These systems are a developing technology which main caveat is the need of high operating temperatures and costs. As such, most multidisciplinary research has been focused on researching materials and/or processes that help mitigate the costs or lower the operating temperature. The research presented in this paper focused on the manufacturing of a cubic stabilized zirconia (CSZ) electrolyte thin membrane for a single cell SOFC through tape casting. Thus, the process was divided into slurry preparation, tape casting, further processing, and analysis of samples. First the tape was produced reaching optimal viscosity (between 500 to 6000 cP) and minimizing impurities. Then, the slurry was poured into the doctor's blade with a 200 micrometers gap and allowed to dry. Samples were punched from the green tape with a diameter of 28 inches. Afterwards, these samples were pressed and sintered with a force of 218016 N and temperature of 1550 degrees celsius, respectively. These steps are done to maximize density and grain growth and minimize porosity. Lastly, the tape went further analysis and it was stated that further research should be done to determine this tape viability for stationary SOFC application.
|
16 |
Fabrication and Optimization of Yttria Stabilized Zirconia Thinfilms towards the Development of Electrochemical Gas SensorKiruba, M S January 2016 (has links) (PDF)
Yttria stabilized Zirconia (8YSZ) is an extensively used solid electrolyte, which finds applications in electrochemical sensors, solid oxide fuel cells and gate oxide in MOSFETs. Recent studies report that YSZ thin films are better performers than their bulk counterparts, in terms of ionic conductivity even at moderate temperatures. YSZ thin films also attract attention with the scope of device miniaturization. However, most of the studies available in the literature on YSZ thin films focus mainly on their electrical characterization. In this work, YSZ thin films were deposited, characterized and possible use of sensors were evaluated.
In the present work, 8 mol% yttria stabilized zirconia thin films were deposited using RF magnetron reactive sputtering under different deposition conditions. Films with thicknesses ranging from few tens to few hundreds of nanometres were deposited. The deposited films were subjected to morphological, structural, compositional and electrical characterizations. Deposition and annealing conditions were optimized to obtain dense, stoichiometric and crystalline YSZ thin films. The ionic conductivity of 200 nm nanocrystal line thin film was found to be two orders of magnitude higher than the bulk. The ionic conductivity increased with the decrease in film thickness.
Compositional analyses of a set of YSZ thin films revealed free surface yttrium segregation. The free surface segregation of dopants can locally alter the surface chemistry and influence the oxygen transfer kinetics across the electrode-electrolyte interface. Although number of reports are available on the segregation characteristics in YSZ bulk, no reports are available on yttria segregation in YSZ thin film. Hence, this work reports detailed investigations on the free surface yttria segregation in YSZ thin films using angle resolved X-ray photoelectron spectroscopy (XPS). Influence of annealing temperature, film thickness, annealing time, and purity on the segregation concentration was determined. It was found that the most important factor that determines the segregation was found to be the target purity. The segregation depth profile analysis showed that the segregation layer depth was proportional to segregation concentration. Free surface segregation reduced the ionic conductivity of the YSZ thin films roughly about a factor. However, segregation did not affect the film’s morphology, grain size, crystallinity and activation energy. The difference in ionic conductivity observed in the segregated and clean YSZ films suggests that dopant free surface segregation could also be one of the reasons for the variable ionic conductivity reported in the literature.
For using YSZ in miniaturized devices, micro-structuring of YSZ is important. It has been reported that the wet etching techniques available for YSZ were not repeatable and do not etch annealed YSZ samples. Reactive ion etching (RIE) is better suited for YSZ patterning due to its capability to offer high resolution, easy control and tenable anisotropic/isotropic pattern transfer for batch processing. Although reports are available on the dry etching of zirconia and yttria thin films, no studies were reported on the dry etching of YSZ thin films. In this work, inductively coupled reactive ion etching (ICP-RIE) using fluorine and chlorine chemistries were employed to etch YSZ thin films. Optimized etching conditions were identified by varying different process parameters like, type of gas, gas flow rate, RF power, ICP power, chamber pressure and carrier wafer in the ICP-RIE process. Optimized conditions were chosen by examining the etch depth, composition analyses before
and after etch using XPS, selectivity towards SiO2 (which is the most common buffer layer) and surface roughness. Etch chemistries involved in a particular plasma (SF6, Cl2 and BCl3) were discussed with the help of surface composition and etch thicknesses. The results showed that etching YSZ with BCl3 plasma at optimized conditions yielded best results through oxygen-scavenging mechanism. A maximum etch rate of 53 nm/min was obtained in BCl3 plasma using PECVD Si3N4 carrier wafer at an ICP power of 1500 W, RF power of 100 W, chamber pressure of 5 mTorr with 30 sccm BCl3 flow.
Sensing devices were designed by employing YSZ thin film as solid electrolyte and nickel oxide and gold thin film as sensing and reference electrodes, respectively to evaluate the possible use of YSZ thin film in miniaturized NO2 sensor. The electrodes were deposited in inter-digitated pattern. Two types of electrodes were designed with different number of fingers in symmetric and asymmetric configurations. The NO2 sensing was performed in the concentration range of 25 to 2000 ppm at three different temperatures, 673, 773 and 873 K in mixed potential and impedance metric modes. The mixed potential type measurements were carried out only for asymmetric cell in two different electrode configurations. The impedance metric type measurements were carried out for both symmetric and asymmetric cells in two different electrode configurations. Preliminary NO2 sensing experiments in both the types of measurements revealed that in devices with electrodes having more fingers were better in performance.
In mixed potential type sensors, sensitivity was measured as the amount of voltage generated when the sensor was exposed to a test gas. The generated voltage was found to be proportional to the logarithm of NO2 concentration in the entire measurement range (50 to 2000 ppm) with the regression fitting parameter, adj.R2 around 0.97 to 0.99 in all the cases. A maximum potential of 271 mV was measured with 2000 ppm NO2 at 873 K. The response and recovery times of the sensors were sensitive to the operating temperature.
In impedance metric mode, the sensitivities were measured as the variation in the low frequency phase angle (∆ φ) when the gas concentration is changed. The frequency range of the measurement was from 0.01 Hz to100 kHz. The response time in the impedance metric sensors was comparable to that of mixed potential sensors. But the recovery time in impedance metric sensors was much was slower than the mixed potential type for all the concentrations. The sensors showed linear response only in a narrow range of 50 to 500 ppm with regression fitting value, R2 around 0.98 in all the cases. Above 500 ppm, the sensitivity value was observed to be saturated. From the gas sensing studies performed on the miniaturized sensors, it was found that the mixed potential type sensing mode is better than the impedance metric type in YSZ thin film based devices. However detailed interference gas studies were needed before drawing any conclusion.
In summary, the studies presented in the work have contributed to the understanding of free surface yttria segregation behaviour in YSZ thin films. Micromachining conditions were optimized for both pristine and annealed YSZ thin films. Suitability of YSZ thin film based miniaturized NO2 gas sensor was evaluated.
|
17 |
Scandia And Ceria Stabilized Zirconia Based Electrolytes And Anodes For Intermediate Temperature Solid Oxide Fuel Cells: Manufacturing And PropertiesChen, Yan 01 January 2013 (has links)
Mesoscale optical phenomena occur when light interacts with a number of different types of materials, such as biological and chemical systems and fabricated nanostructures. As a framework, mesoscale optics unifies the interpretations of the interaction of light with complex media when the outcome depends significantly upon the scale of the interaction. Most importantly, it guides the process of designing an optical sensing technique by focusing on the nature and amount of information that can be extracted from a measurement. Different aspects of mesoscale optics are addressed in this dissertation which led to the solution of a number of problems in complex media. Dynamical and structural information from complex fluids—such as colloidal suspensions and biological fluids—was obtained by controlling the size of the interaction volume with low coherence interferometry. With this information, material properties such as particle sizes, optical transport coefficients, and viscoelastic characteristics of polymer solutions and blood were determined in natural, realistic conditions that are inaccessible to conventional techniques. The same framework also enabled the development of new, scale-dependent models for several important physical and biological systems. These models were then used to explain the results of some unique measurements. For example, the transport of light in disordered photonic lattices was interpreted as a scale-dependent, diffusive process to explain the anomalous behavior of photon path length distributions through these complex structures. In addition, it was demonstrated how specialized optical measurements and models at the mesoscale enable solutions to fundamental problems in cell biology. Specifically, it was found for the first time that the nature of cell motility changes markedly with the curvature of the substrate that the cells iv move on. This particular work addresses increasingly important questions concerning the nature of cellular responses to external forces and the mechanical properties of their local environment. Besides sensing of properties and modeling behaviors of complex systems, mesoscale optics encompasses the control of material systems as a result of the light-matter interaction. Specific modifications to a material’s structure can occur due to not only an exchange of energy between radiation and a material, but also due to a transfer of momentum. Based on the mechanical action of multiply scattered light on colloidal particles, an optically-controlled active medium that did not require specially tailored particles was demonstrated for the first time. The coupling between the particles and the random electromagnetic field affords new possibilities for controlling mesoscale systems and observing nonequilibrium thermodynamic phenomena
|
18 |
Etude sur fusion laser sélective de matériau céramique Zircone Yttriée / Study on Selective Laser Melting of ceramic material Yttria Stabilized ZirconiaLiu, Qi 05 November 2013 (has links)
La fusion sélective par laser est un procédé de la technologie de fabrication rapide de plus en plus utilisé dans l’industrie automobile, aéronautique, médicale, etc. Selon le principe de la fabrication rapide, la pièce est fabriquée couche par couche en fusionnant et soudant les particules fines par laser. Actuellement, les principaux matériaux utilisés sont les métaux métalliques ou les polymères. Le faible ou modeste point de fusion de ces matériaux conduit à une mise en œuvre par laser relativement facile. Cependant, en raison de leur point de fusion élevé, de la forte résistance à haute température et de la faible conductivité thermique, l’utilisation de matériaux céramiques est limitée dans la technologie de fusion laser sélective. Cette étude explore la fusion laser sélective de zircone stabilisée par yttrine avec un laser à fibre de longueur d’onde d’environ 1 µm. L’influence de différentes puissances de laser et de différentes vitesses de balayage sur la microstructure et la déformation de l’échantillon a été étudiée, et la densité relative et la microdureté ont été mesurées. Notamment, l’effet de différentes températures de préchauffage sur la microstructure sera étudié. En même temps, la structure cristalline céramique et la transformation des phases pendant le procédé de prototypage rapide ont été analysées. Les résultats expérimentaux montrent qu’il est possible de fondre complètement de la poudre YSZ avec un laser à fibre NIR, et avec l’optimisation des paramètres de fabrication, la densité relative de l’échantillon peut atteindre 91 %. Il est inévitable de voir se former des fissures et des pores dans les pièces fabriquées du fait de l’hétérogénéité de la distribution de l’énergie du laser. Cette distribution de l’énergie peut être améliorée grâce à l’optimisation des paramètres ; les longueurs de fissure peuvent être contrôlées et maîtrisées par un préchauffage du lit de poudre. Notamment, à haute température (1500°C, 2000°C et 2500°C) de préchauffage, la fissure verticale continue devient désordonnée et courte. Une transformation de la structure monoclinique et cubique en structure tétragonale s’est produite pendant le processus de fabrication. / Selective laser melting is a rapid manufacturing process coming from the rapid prototyping technology, which is widely used in the automotive, aeronautical, medical industry etc. According to the principle of rapid manufacturing, the piece is manufactured layer by layer through the laser sintering or melting the fine powder. Currently, the main powder materials used are metal or polymer materials. The low melting point of these materials facilitates the melting process. However, duo to the high melting point, strong strength at high temperature and low thermal conductivity the application of ceramic materials is limited in the technology of selective laser melting. In this study, selective laser melting of the ceramic yttria stabilized zirconia by a 1μm wavelength fiber laser was explored. The influence of different laser powers and different scanning velocities on the microstructure and the deformation were analyzed, then the micro-hardness and relative density were measured. In particular, the effect of different preheat temperatures on microstructure was investigated. At the same time, the crystal structure and phase transformation during the fabrication were analyzed. Experimental results show that YSZ powder can be completely melted by the near IR fiber laser. With the optimization of the manufacturing parameters, the relative density of sample could reach 91 %. The forming of cracks and pores in the manufactured parts is rarely avoid due to the heterogeneity of distribution of energy. The energy distribution could be improved by optimizing the parameters and the crack lengths can be controlled by preheating the powder bed. In particular, the high temperature (1500 ℃, 2000 ℃ and 2500 ℃) lead the continuous vertical crack becomes messy and short. The transformation of monoclinic and cubic crystal to tetragonal crystal can be observed during the fabrication.
|
19 |
Elaboration et maitrise de la structure d'une cellule de pile à combustible à base de zircone scandiée. / Fabrication and control of the structure of a fuel cell based on scandia-stabilized zirconiaReynier, Thibault 08 November 2012 (has links)
Dans le domaine des piles SOFC, un des principaux objectifs actuels est la réduction de latempérature de fonctionnement des cellules en deçà de 700°C, afin de garantir une plusgrande durabilité des systèmes électrochimiques et des matériaux de cellules. En outre, leprocédé d’élaboration d’une cellule complète comprend actuellement deux voire trois étapesde frittage; une seule opération de frittage pourrait conduire à une diminution conséquente ducoût de production de la cellule. Le but de ce travail de thèse est d’apporter une contribution àces deux problématiques en proposant un procédé d’élaboration d’une cellule de pile àcombustible SOFC en une seule opération dite de cofrittage et avec une sélection dematériaux à hautes performances électrochimiques.Cette thèse a été abordée selon trois thématiques principales : mécanique, microstructurale etélectrochimique.Après la caractérisation du comportement en frittage des matériaux retenus pour l’étude, uncycle de frittage conduisant à une microstructure d’électrolyte acceptable (porosité fermée) aété sélectionné. Le cofrittage a ensuite été étudié selon un aspect mécanique. Les phénomènesde courbure engendrés par le cofrittage ont été expliquées à l’aide d’une modélisationanalytique et confrontées à des observations in situ. Le travail s’est ensuite orienté dans uneapproche microstructurale avec l’optimisation de la microstructure de la cathode en utilisantune modélisation numérique basée sur la méthode des éléments discrets. Les composants de lacellule complète ont finalement été caractérisés par spectroscopie d’impédanceélectrochimique afin d’optimiser leurs performances. Enfin, une cellule complète exempt defissure a été réalisée par cofrittage et ses performances électrochimiques ont été estimées. / In the field of SOFCs, a major objective is the reduction of the cell operating temperaturebelow 700°C, in order to ensure greater durability of electrochemical systems and cellmaterials. In addition, the fabrication process of a complete cell currently includes two orthree stages of sintering. Thus one sintering process could lead to a consequent decrease in theproduction cost of the cell. The purpose of this thesis is to contribute to these two issues byproposing a method for manufacturing a SOFC fuel cell in a single operation called cofiringand with a selection of high electrochemical performance materials.This thesis is addressed in three main areas: mechanical, microstructural and electrochemical.After sintering behavior characterization of the selected materials, a sintering cycle leading toan acceptable electrolyte microstructure (closed porosity) was selected. The cofiring was thenapproached by a mechanical aspect. The curvature Phenomena caused by of cofiring wereexplained using an analytical model and compared with in situ observations. The work is thencontinued with a microstructural approach. The optimization of the cathode microstructurewas done using a numerical modeling based on the discrete element method. Cell componentswere finally characterized by electrochemical impedance spectroscopy to optimize theirperformances. Finally, a free crack complete cell was obtained by co-sintering process and herelectrochemical performance was estimated.
|
20 |
Zircônia CO-dopada por compensação de cargas nos sistemas (ZrO2)1-(x+y)(InO1,5)x(MOz)y com MOz = TaO2,5, NbO2,5, MoO3 ou WO3, como revestimento para barreira térmicaPiva, Roger Honorato 30 September 2016 (has links)
Submitted by Alison Vanceto (alison-vanceto@hotmail.com) on 2016-10-25T10:51:21Z
No. of bitstreams: 1
TeseRHP.pdf: 8778601 bytes, checksum: eb4553a13387041c0fd36d153b524c3c (MD5) / Approved for entry into archive by Marina Freitas (marinapf@ufscar.br) on 2016-11-08T19:10:09Z (GMT) No. of bitstreams: 1
TeseRHP.pdf: 8778601 bytes, checksum: eb4553a13387041c0fd36d153b524c3c (MD5) / Approved for entry into archive by Marina Freitas (marinapf@ufscar.br) on 2016-11-08T19:10:15Z (GMT) No. of bitstreams: 1
TeseRHP.pdf: 8778601 bytes, checksum: eb4553a13387041c0fd36d153b524c3c (MD5) / Made available in DSpace on 2016-11-08T19:10:21Z (GMT). No. of bitstreams: 1
TeseRHP.pdf: 8778601 bytes, checksum: eb4553a13387041c0fd36d153b524c3c (MD5)
Previous issue date: 2016-09-30 / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / InO1.5-stabilized zirconia (InSZ) is a potential hot corrosion resistant thermal
barrier coating (TBC). However, the thermal instability prevents real applications
of InSZ-based TBC. This thesis investigates the hypothesis of co-doping
using the charge compensation to improve the phase stability of InSZ. Four
co-doping systems were synthesized by coprecipitation and studied:
(ZrO2)1-(x+y)(InO1.5)x(MOz)y with MOz = TaO2.5, NbO2.5, MoO3, or WO3. After
synthesis, 9 mol% of InO1.5 plus the charge-compensating oxides was sufficient
to stabilize the tetragonal phase. Specific surface area up to 106.1 m2.g-1 and
crystallite size ~11 nm were achieved using ethanol washing followed by
azeotropic distillation as dehydration technique in the precipitates. In these
powders, initial thermal stability analysis indicated instability of the tetragonal
phase, with extension of the t→m transformation less detrimental in the InMoSZ
system. Further increase in the concentration of InO1.5:MoO3 results in
monophasic samples with retention of cubic phase in the InMoSZ. Cubic
InMoSZ exhibited hardness and thermal expansion coefficient of 13.5% and 9%
higher than those of InSZ, respectively. However, thermal treatments at
T ≥ 1200 °C showed that the InMoSZ is also passive to destabilization of the
high temperature cubic polymorph. Although the cubic InMoSZ was the most
promising system found in this thesis, the stability results do not support its
application as TBC for temperatures ≥ 1000 ºC. A deep evaluation of the phase
transformations between 1000 to 1200 °C indicated that the instability of the
proposed systems is due to a progressive c→t→m destabilization of the
polymorphs. This c→t→m transformation is directly associated with the
reduction of the InO1.5 stabilizer in solid solution by volatilization as In2O during
heat treatment. At temperatures ≤ 800 ºC, the c→t phase transformation do not
occurs, then, InSZ-based TBC is stable in these conditions. / A zircônia estabilizada com InO1,5 (InSZ) é um material com potencial aplicação
como revestimentos para barreira térmica (TBC) resistentes à corrosão.
Contudo, a instabilidade de fases impede aplicações industriais da InSZ. Esta
tese investiga a ação da co-dopagem por compensação de cargas como uma
estratégia para aumentar a estabilidade de fases da InSZ. Quatro sistemas de
co-dopagem foram sintetizados por co-precipitação e estudados:
(ZrO2)1-(x+y)(InO1,5)x(MOz)y com MOz = TaO2,5, NbO2,5, MoO3 ou WO3. Após a
síntese, 9 %mol de InO1,5 somado a concentração de óxidos compensadores
de carga foi suficiente para estabilização da fase tetragonal. Área superficial
específica de até 106,1 m2.g‒1 e tamanho de cristalitos de ~11 nm foram
obtidos utilizando a lavagem com etanol seguida por destilação azeotrópica
como técnica de desidratação dos precipitados. Para estes pós, testes de
estabilidade térmica indicaram instabilidade da fase tetragonal, com extensão
de transformação t→m menos detrimental no sistema InMoSZ. Aumentando
gradativamente a concentração de InO1,5-MoO3 na InMoSZ resulta em
amostras monofásicas com retenção da fase cúbica. A InMoSZ cúbica exibiu
dureza e coeficiente de expansão térmica até 13,5% e 9% superiores aos
valores da InSZ, respectivamente. No entanto, tratamentos em temperaturas ≥
1200 ºC indicaram que a InMoSZ é também suscetível a desestabilização da
fase cúbica. Embora a InMoSZ cúbica tenha sido o sistema mais promissor
obtido nesta tese, os resultados de estabilidade indicam que sua aplicação
como TBC não é possível em temperaturas ≥ 1000 ºC. Uma avaliação
detalhada das fases formadas após os tratamentos entre 1000 a 1200 ºC
demonstrou que a instabilidade dos sistemas estudados é decorrente de uma
transformação progressiva tipo c→t→m. A origem da transformação c→t→m é
associada a redução da concentração do estabilizador InO1,5 em solução sólida
por volatilização como In2O durante os testes de estabilidade térmica. Em
temperaturas ≤ 800 ºC, a transformação c→m não ocorre, neste caso, TBCs
baseadas em InSZ são estáveis termicamente para aplicações industriais.
|
Page generated in 0.062 seconds