20 research outputs found

    Nucleation and growth mechanisms of trivalent chromium conversion coatings on 2024-T3 aluminium alloy

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    Nucleation and growth mechanisms of trivalent chromium conversion coatings on 2024 aluminium alloy (AA 2024) were studied. Nucleation of 25 nm diameter nodules was observed on the ridges of the scalloped structure of degreased and desmutted AA 2024 after very short time of conversion treatment corresponding to the formation of a 12 nm thick precursor layer. Then, the composition of this layer evolved and concomitantly a chromium and zirconium outer layer deposited on top of it. Rather long-lasting anticorrosive properties were measured even for conversion coatings formed after short exposure to the conversion bath, except for the precursor layer

    Synthesis of yttria by aqueous sol-gel route to develop anti-CMAS coatings for the protection of EBPVD thermal barriers

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    Anti-CMAS yttria coatings have been prepared by sol-gel routes. Yttria powders with controlled morphology are prepared via auto-combustion of yttrium precursors in a polymerized matrix. The influence of key parameters of the water-based sols is assessed. Indeed, the pH of the initial sol and the temperature of thermal treatment play a major role in the morphology and grain size of yttria powders. To prevent infiltration of CMAS, yttria powders are proposed to be synthesized at pH=1 of the aqueous sol, with drying of the sol and heating at 900 °C. After optimization of the synthesis and deposition conditions via sol-gel route, yttria-based coatings with high specific surface area are obtained. They promote the interaction with melt CMAS and consequently limit the degradation of the thermal barrier coatings situated underneath. It was proved that anti-CMAS yttria coating is effective against the infiltration of CMAS at 1250 °C for 15 min and even 1 h

    Dense on Porous Solid LATP Electrolyte System: Preparation and Conductivity Measurement

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    A dense membrane of lithium aluminum titanium phosphate Li1+xAlxTi2-x(PO4)3, x=0.3 (LATP) is deposited on a porous LATP substrate via wet chemistry. In the polymerized complex process, phosphate precursors with different active groups and steric hindrance are selected to tune precursor’s reactivity. Rheological studies and microstructural observations lead to the selection of an LATP powder slurry charged with lithium, aluminum, titanium, and phosphate ion precursors. The optimized formulation is impregnated into a porous LATP substrate. After thermal treatment, dense LATP membranes on top of a porous LATP substrate are obtained with conductivities as high as 3 x 10-4 S/cm for the dense part, the porous part acting as a mechanical support. An original Van der Pauw impedance setup is validated for the measurement of the ionic conductivity of such dense/ porous systems

    Lithium conducting solid electrolyte Li1.3Al0.3Ti1.7(PO4)3 obtained via solution chemistry

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    NaSICON-type lithium conductor Li1.3Al0.3Ti1.7(PO4)3 (LATP) is synthesized with controlled grain size and composition using solution chemistry. After thermal treatment at 850 C, sub-micronic crystallized powders with high purity are obtained. They are converted into ceramic through Spark Plasma Sintering at 850–1000 C. By varying the processing parameters, pellet with conductivities up to 1.6 * 10−4 S/cm with density of 97% of the theoretical density have been obtained. XRD, FEG-SEM, ac-impedance and Vickers indentation were used to characterize the products. The influence of sintering parameters on pellet composition, microstructure and conductivity is discussed in addition to the analysis of the mechanical behavior of the grains interfaces

    Synthesis of yttria by aqueous sol-gel route to develop anti-CMAS coatings for the protection of EBPVD thermal barriers

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    Anti-CMAS yttria coatings have been prepared by sol-gel routes. Yttria powders with controlled morphology are prepared via auto-combustion of yttrium precursors in a polymerized matrix. The influence of key parameters of the water-based sols is assessed. Indeed, the pH of the initial sol and the temperature of thermal treatment play a major role in the morphology and grain size of yttria powders. To prevent infiltration of CMAS, yttria powders are proposed to be synthesized at pH=1 of the aqueous sol, with drying of the sol and heating at 900 °C. After optimization of the synthesis and deposition conditions via sol-gel route, yttria-based coatings with high specific surface area are obtained. They promote the interaction with melt CMAS and consequently limit the degradation of the thermal barrier coatings situated underneath. It was proved that anti-CMAS yttria coating is effective against the infiltration of CMAS at 1250 °C for 15 min and even 1 h

    Influence of the alloy microstructure and surface state on the protective properties of trivalent chromium coatings grown on a 2024 aluminium alloy

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    The protective properties of trivalent chromium process (TCP) coatings grown on a 2024-T3 aluminium alloy were studied on the basis of electrochemical measurements performed both in sulphate and chloride solutions and neutral salt spray tests. The influence of the alloy microstructure and surface state was studied: two batches, each one characterized by its own coarse intermetallic particle distribution, and two surface states, i.e. laminated and polished, were considered. Results showed that in 0.1 M Na2SO4, the protective properties of the TCP coatings decreased when the roughness of the initial surface increased. Furthermore, improved protective properties were observed for a TCP coating grown on a surface containing a lower amount of Al-Cu-Mg IMCs in the initial microstructure. The most plausible explanation is that a fast kinetics of coating growth, either associated to strong initial roughness or a great surface copper coverage, was detrimental for the protective properties of the coatings. In more aggressive solutions, i.e. 0.5 M NaCl solution or for neutral salt spray tests, the differences are not significant. The findings are highly relevant for industrial applications: the results showed that variations in batches, for a same type of alloy, or in initial surface state should not be detrimental for the corrosion resistance of the TCP coated samples. However, the conversion process had to be adapted for different types of alloys, characterized by their own microstructure

    Optimized sol–gel thermal barrier coatings for long-term cyclic oxidation life

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    New promising thermal barrier coatings (TBCs) processed by the sol–gel route are deposited onto NiPtAl bond coated superalloy substrates usingthe dip and/or spray coating technique. In this study, the optimization of the process, including an appropriate heat treatment prone to densifythe yttria-stabilized-zirconia (YSZ) top-coat and leading to the sintering and the development of a resulting crack network, is investigated. Inparticular, relevant information on internal strain evolution during the heat treatment are obtained using in situ synchrotron X-rays diffraction andconfirm a stabilization of the TBC through the occurrence of the micro-cracks that beneficially releases the in-plane sintering stress. Such TBCs aresubsequently reinforced using additional material brought within the cracks using sol–gel spray coating. The effect of various process parameters,such as the pre-oxidation of the bond-coat, on the sol gel TBCs consolidation and their cyclic oxidation resistance enhancement, is presented.Reinforced sol–gel TBCs are successfully oxidized up to more than one thousand 1 h-cycles at 1100◦C, without any detrimental spallation

    Functionalized superhydrophobic coatings with micro-/nanostructured ZnO particles in a sol–gel matrix

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    Among the methods to create superhydrophobic surfaces by wet chemistry, one of the strategies consists in coating the substrate with a hydrophobic polymer with specific morphology. Such elaborated surfaces are largely developed and can present complex architectures but are generally fragile. Ceramic-based coatings show better durability. In this work, a new route associating inorganic and polymeric parts is used. Surfaces with superhydrophobic properties are prepared with a mixture of zinc oxide (ZnO) particles in a hybrid organic inorganic matrix prepared via sol–gel route. ZnO particles were synthesized by the inorganic polycondensation route and exhibit an appropriate micro-/nanostructure for superhydrophobicity. Sol–gel matrix is obtained by the alkoxide route with aluminum-tri-secbutoxide (ASB) and (3-glycidoxypropyl)trimethoxysilane (GPTMS). A step of octadecylphosphonic acid (ODP) functionalization on ZnO particles and on film surfaces was employed to considerably improve hydrophobic properties. This new route enables to obtain superhydrophobic coatings that exhibitwater contact angles superior to 150°. These coatings show a homogeneous and smooth coverage on aluminum alloy substrate. Results attest the significance of the synergy for superhydrophobic coatings: a micro-/nanostructured surface and an intrinsic hydrophobic property of the material. The durability of the coatings has also been demonstrated with only a slight decrease in hydrophobicity after erosion

    Photolithographic processing of silver loaded dielectric coatings based on preformed colloidal TiO2nanoparticles dispersed in a mesoporous silica binder

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    Titanium dioxide is a well known photocatalyst for reactions involving surface trapped photogenerated carriers. Noble metal photo-reduction may be used for the processing of silver/TiO 2 nanocomposite coatings that may exhibit interesting optical and electrical properties. We present here results of our investigations performed on an original system consisting of preformed colloidal TiO 2 nanoparticles homogeneously dispersed within a mesoporous silica host matrix. Light irradiation of samples immerged in an aqueous silver salt solution leads to the homogeneous deposition of silver islands in the vicinity of the TiO 2 particles and throughout the film thickness. The silver volume fraction is directly controlled by the irradiation dose up to a value of about 16 vol.%. Films exhibit tunable plasmonic properties that correspond to silver nanoparticles in interaction, and a percolation threshold is observed at 8–10 vol.%, leading to films with a conductivity of about 40 S cm −1 . The major interest of this method lies in the high silver reduction quantum efficiency (about 50%) and the possibility to modulate optical and electronic properties by light irradiation while the low temperature of processing permits the photolithographic deposition of metallic patterns on organic flexible substrates

    Apparent Interfacial Toughness of Undoped and Photoluminescent Eu3+-Doped Yttria-Stabilized Zirconia Thermal Barrier Coatings

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    Most photoluminescence methods for the diagnostic of thermal barrier coatings (TBC) rely on the functionalization of yttria-stabilized zirconia (YSZ) with trivalent lanthanide ions. It consists in determining temperature and detecting preventively damages within the volume of the TBC prior to ceramic topcoat spallation. The latter depends on the interfacial toughness, which is an important factor to address thermal barrier coating’s performance and durability. In this paper, the influence of the addition of rare earth elements (Eu3+) on the interfacial toughness of TBC deposited by atmospheric plasma spray is investigated. Two types of coatings are deposited and investigated: (1) Type I: coating deposited using Eu3+-doped YSZ powder (2 mol.%), (2) Type II: coating deposited using undoped YSZ powder. Both types of coatings are heat-treated at 1100 °C under isothermal conditions using different oxidation exposure times: 100, 300 and 800 h. The morphology of the interface between the topcoat (TBC) and the bond coat is analyzed by scanning electron microscopy. The apparent interfacial toughness is investigated using indentation. It is shown that the interfacial apparent toughness decreases as the oxidation exposure time increases. Concomitantly, the thickness of the thermally grown oxide (TGO) layer between the bond coat and the topcoat increases. Results show as well that the partial substitution of Y3+ ions by a low amount of Eu3+ ions (2 mol.%) does not have influence on the microstructure and the interfacial toughness of the YSZ coatings. In addition, energy dispersive spectrometry reveals that there is no diffusion of Eu3+ into the TGO layer. It is therefore concluded that the use of Eu3+ for damage diagnostic based on photoluminescence methods will not induce any kind of degradation of the properties of TBCs
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