EBC Development and Behaviour Analysis for High Temperature CMC Components

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An efficient route to aqueous phase synthesis of nanocrystalline γ-Al2O3 with high porosity: From stable boehmite colloids to large pore mesoporous alumina

In this paper we emphasise the important role of Pluronic F127 on the porosity of mesoporous alumina prepared from boehmite colloids. By focusing on the F127/boehmite interactions we show how the concepts of interface science may help to predict and improve the textural characteristics of mesoporous alumina. By varying the synthetic parameters, in particular the copolymer content, we show that the porosity of c-Al2O3 can be enhanced by 400% and the average pore diameter can be expanded from 5 to 14 nm. These results are discussed in terms of interactions between the Pluronic F127 and boehmite colloids, and are correlated to the critical micelle concentration (CMC) of the copolymer. The textural characteristics of the mesoporous alumina can be further improved either by introducing hydrocarbons in the preformed boehmite/copolymer sols or by concentrating the sols. In comparison with as-synthesised alumina, those prepared with F127 showed improved thermal stability. Furthermore, boehmite/copolymer sols were stable for all surfactant concentrations investigated and can give high quality coatings suitable for catalytic applications

Reinforced sol–gel thermal barrier coatings and their cyclic oxidation life

Cyclic oxidation life enhancement of sol–gel thermal barrier coatings is obtained via the reinforcement of the controlled micro-crack network that forms during the initial sintering of the deposit. Two different sol–gel methods are used to fill in the process-induced cracks, namely dipcoating and spray-coating. Filling parameters, for instance the number of passes or the viscosity of the sol are adjusted, using various techniques such as profilometry and microstructural analysis, to optimise crack filling. Cyclic oxidation tests are implemented at both 1100C and 1150C to investigate the efficiency of the various reinforcement procedures developed and address the influence of the specific microstructure on the oxidation behaviour

Renforcement et fonctionnalisation de barrières thermiques aéronautiques élaborées par voie sol-gel : comportement en oxydation cyclique et diagnostic thermique

Les principaux objectifs de cette thèse sont d'une part d'améliorer la tenue en oxydation cyclique des barrières thermiques élaborées par la voie sol-gel (BTSG) et d'autre part de réaliser des diagnostics thermiques afin d'évaluer les températures opérant dans de tels systèmes. Tout d'abord, l'identification des mécanismes d'endommagement en oxydation cyclique de BTSG a été réalisée. Ainsi, la dégradation des BTSG est initiée par la création d'un réseau de microfissures, qui se développe pour mener à l'écaillage localisé de cellules de revêtement. A partir de ces résultats, des voies d'optimisation du protocole d'élaboration des BTSG ont été proposées : l'étude du frittage sur la pré-fissuration des revêtements, ainsi que le renfort du revêtement par le colmatage des fissures. Pour évaluer les performances de ces BTSG renforcées en termes de durée de vie, elles ont ensuite été testées en oxydation cyclique. Par ailleurs, le pronostic de la durée de vie de ses systèmes nécessite une connaissance précise de la température dans l'épaisseur du revêtement. Ainsi, la méthode de thermométrie par phosphorescence a été utilisée sur des BTSG, montrant les possibilités de la technique pour de tels systèmes.The main objectives of this PhD work are on the one hand to improve the performance in cyclic oxidation of thermal barrier coating synthesized by sol-gel route (BTSG) and on the other hand to realize thermal diagnosis to evaluate the temperature used in these systems. Firstly, the identification of damage mechanisms in cyclic oxidation of BTSG has been realized. Thus, the BTSG degradation is initiated by the creation of micro-cracks network, which develops to lead to localised spallation of coating cells. From these results, optimisation route of BTSG elaboration process has been proposed : sintering study on the coating pre-cracking and the coating reinforcement with the filling oft the cracks. To evaluate the efficiency of this reinforced BTSG, in lifetime terms, they are tested in cyclic oxidation. Furthermore, the lifetime prediction of these systems require an accurate knowledge of temperature in the thickness of the coating. Thus, the phosphor thermometry method has been used on BTSG, showing the technique possibilities for these systems

Characterisation of thermal barrier sensor coatings synthesised by sol–gel route

Further improvements in the efficiency of gas turbines are recognised to come from increases in turbine entry temperatures. Accurate temperature measurements are crucial to achieve these increases whilst maintaining reliability and economic component life. The combination of phosphor thermometry and thermal barrier coating (TBC) technology has led to the development of functional temperature sensor coatings which have several advantages over conventional temperature measurement techniques. Developments in sol–gel processing indicate that this method could be used for the production, or particularly, the repair of TBCs in the future. This paper demonstrates, for the first time, that sol–gel processing can be used to make sensor TBCs. The optimum concentration of SmO1.5 was 2 wt.% in YSZ to achieve the brightest phosphorescence emission. Above this concentration the overall intensity of the emission reduces and the transitions from 4F3/2 were suppressed. Furthermore, a similar suppression of these transitions was observed when the product of the sol–gel was heat treated to 1100 ◦C. This was concluded to be due to a higher degree of crystallinity allowing a greater interaction between the dopant ions. The dependence of the phosphorescence spectrum on heat treatment temperature provides the first indication that YSZ produced through sol–gel could be used to detect historic temperatures. An evaluation of the subsurface measurement and temperature capabilities has shown that the phosphorescence can be detected from relatively thin layers, 20 µm, even under 50 µm of undoped YSZ coating. Although the temperature detection range, 400–700 ◦C, is too low for advanced TBCs the material could be used in low temperature regimes or for health monitoring purposes

Processing, repairing and cyclic oxidation behaviour of sol–gel thermal barrier coatings

Sol–gel Thermal Barriers Coatings (TBCs) are manufactured using the dip-coating technique optimised in terms of process parameters including sol formulation, rate of withdrawing and heat treatment. The specific mechanisms of sol–gel TBCs, deposited on either NiAl or NiPtAl bond-coated superalloy substrates, are described. The possibility to reinforce and stabilise the crack network formed during the heat treatment or the first oxidation cycles using supplementary dip-coatings and appropriate process parameters is investigated. It is shown that implementing this technique that can be further regarded as an attractive way for repairing TBCs, significantly improves the cyclic oxidation behaviour of the multi-materials systems

Advances in the deposition of ceramics by soft chemistry process : example of rare- earth silicate coatings

The dip-coating process consists in immersing a sample to be coated in the liquid medium and then removing it at a controlled speed in order to obtain a film of regular thickness, as shown in Figure 1a). Dip-coating technique is now used in many industrial fields (biomedical, transportation, optics…). It is a very simple, and easy process to implement for the deposition and shaping of different natures of coatings (ceramic, metallic and polymer). In the case of ceramic coatings, after the dip-coating operation, the layers undergo a sintering post-treatment leading to the consolidation and/or the densification of the deposit. The corresponding mechanisms need a rigorous control of many parameters. The parameters involved in the dip-coating process are related to the medium and to the process. Concerning the medium, the dispersion medium nature, the particles concentration, viscosity, and stability are the main ones. The stability of the suspension is a first-order parameter and a preliminary formulation work has been carried out to cope with it. Moreover, parameters relative to the fabrication process such as the number of layers and the thermal profile (intermediary and final temperatures), will also be key factors to be taken into account in the formation of homogeneous and reproducible coatings by dip-coating.This work highlights the influence of these various parameters in the case of rare earth silicates based coatings. The various experiments were carried out in correlation to the coatings quality and microstructure. Homogeneous and conformal ceramic coatings of few tens of micrometers thick, as shown in Figure 1b), were obtained. A multi-layers deposit in a sol loaded at 40% mass generally allows to reach the desired thickness. With these experiments relationship between dip-coating parameters and coatings microstructure and morphology can be established. Please click Additional Files below to see the full abstract

Sol–gel thermal barrier coatings: Optimization of the manufacturing route and durability under cyclic oxidation

A new promising and versatile process based on the sol–gel transformation has been developed to deposit yttria-stabilised thermal barrier coatings. The non-oriented microstructure with randomly structured pore network, resulting from the soft chemical process, is expected to show satisfactory thermo-mechanical behaviour when the TBC is cyclically oxidized. First stage of the research consists of optimizing the processing route to generate homogeneous microstructure and controlled surface roughness. The objective is to reduce, as much as possible, the size and depth of the surface cracks network inherent to the process. Indeed, the durability of the TBC when cyclically oxidized strongly depends on the sharpness of those cracks that concentrate thermo-mechanical stresses and generate detrimental propagation resulting in spallation. Cyclic oxidation tests are performed using a cyclic oxidation rig instrumented with CCD cameras to monitor in a real time basis the mechanism of crack propagation and spallation. The impact of various parameters either directly related to the processing route, e.g. the intimate microstructure of the TBC and the TBC thickness, or to the thermal loading, e.g. the oxidation temperature and the cumulated hot time, on the durability of the TBC is investigate

CO\u3csub\u3e2\u3c/sub\u3e-Fixing One-Carbon Metabolism in a Cellulose-Degrading Bacterium \u3cem\u3eClostridium thermocellum\u3c/em\u3e

Clostridium thermocellum can ferment cellulosic biomass to formate and other end products, including CO2. This organism lacks formate dehydrogenase (Fdh), which catalyzes the reduction of CO2 to formate. However, feeding the bacterium 13C-bicarbonate and cellobiose followed by NMR analysis showed the production of 13C-formate in C. thermocellum culture, indicating the presence of an uncharacterized pathway capable of converting CO2 to formate. Combining genomic and experimental data, we demonstrated that the conversion of CO2 to formate serves as a CO2 entry point into the reductive one-carbon (C1) metabolism, and internalizes CO2 via two biochemical reactions: the reversed pyruvate: ferredoxin oxidoreductase (rPFOR), which incorporates CO2 using acetyl-CoA as a substrate and generates pyruvate, and pyruvate- formate lyase (PFL) converting pyruvate to formate and acetyl-CoA. We analyzed the labeling patterns of proteinogenic amino acids in individual deletions of all five putative PFOR mutants and in a PFL deletion mutant. We identified two enzymes acting as rPFOR, confirmed the dual activities of rPFOR and PFL crucial for CO2 uptake, and provided physical evidence of a distinct in vivo “rPFOR-PFL shunt” to reduce CO2 to formate while circumventing the lack of Fdh. Such a pathway precedes CO2 fixation via the reductive C1 metabolic pathway in C. thermocellum. These findings demonstrated the metabolic versatility of C. thermocellum, which is thought of as primarily a cellulosic heterotroph but is shown here to be endowed with the ability to fix CO2 as well