Various alumina-based materials are applied to achieve different electrical insulation properties based on the variation of the material specific relative permittivity. Thermally sprayed mullite (Al 2 O 3 · SiO 2 ) can form an amorphous phase due to the high cooling rates of the process. The formation of amorphous phases causes a change in the capacitive behaviour of the coatings. The tendency to form amorphous areas can be influenced by the composition of the feedstock material or coating parameters. On the one hand, mullite coatings based on two different Al 2 O 3 to SiO 2 ratios are investigated. On the other hand, a parameter variation is used to achieve various particle temperatures during the process. The coatings are investigated via X-ray diffraction and DSC for phase formation, electron microscopy for coating structure and impedance spectroscopy for measuring the AC-resistance. The conducted variation of the feedstock material as well as the parameters causes differences in the XRD and DSC measurements correlating with a difference in the amounts of amorphous phases. For the capacitive behaviour, coatings applied with hydrogen as process gas showed decreased AC-resistance values. The chemical composition of the feedstock material indicates that the AC-resistance decreases with increasing amounts of SiO 2 . In summary, mullite has promising insulation properties which can be modified by the feedstock material composition as well as the coating parameters. For future application, mullite is a promising candidate for increasing the electrical insulation properties in conditions under high electrical and mechanical demands.

Ba(Mg 1/3 Ta 2/3 )O 3 (BMT), a high melting point refractory oxide, is envisioned as a thermal barrier coating material. In this study, six chemical reagents combinations are investigated as BMT coating precursors: one BMT powder suspension and five Ta 2 O 5 suspensions in nitrate solutions or acetate solutions. A hybrid suspension / sol plasma spray process is designed to axially inject these precursors into a RF thermal plasma torch to synthesize BMT and to deposit nanostructured coatings. X-ray photoelectron spectroscopy (XPS) was used to evaluate the element evaporation during plasma spraying. Thermogravimetric analysis and differential thermal analysis (TG/DTA) are applied to investigate the BMT formation. Parameters such as precursor chemistry and proportion, plasma power, spray distance and substrate preheating are studied with regards to the coating phase structure. The results indicate that the combination of twice the Mg stoichiometric amount with a power of 50 kW shows the best results when using nanocrystalline Ta 2 O 5 as Ta precursor. When choosing nitrates as Ba and Mg precursors, predominant crystalized BMT can be obtained at lower plasma power (45 kW) when compared to acetates (50 kW). BaTa 2 O 6 , Ba 3 Ta 5 O 15 , Ba 4 Ta 2 O 9 , Mg 4 Ta 2 O 9 are the main secondary phases during BMT preparation process. Because of the complicated acetate decomposition, the coating deposition rate from nitrate precursors is higher than that from acetate ones.

Environmental barrier coatings (EBC) are currently being investigated to protect ceramic matrix composite (CMC) turbine engine components in water-vapor rich combustion environments. Dense, crack-free, uniform and well-adhered coatings are demanded for this purpose. This paper represents an assessment of different thermal spray techniques for deposition of Yb 2 Si 2 O 7 and silicon (Si) EBC layers. Plasma spraying of refractory silicates is known to be complicated by undesired glass transition due to rapid solidification as well as evaporation of Si-bearing species during spraying. Plasma spraying of low-density Si also requires careful optimizations as it tends to oxidize during spraying, particularly at atmospheric conditions. Bearing these problems in mind, the Yb 2 Si 2 O 7 coatings were deposited by atmospheric plasma spraying (APS), high-velocity oxygen-fuel spraying (HVOF), and plasma-spray physical vapor deposition (PS-PVD) techniques. As-sprayed microstructure, amorphous content and phase composition of the coatings were analyzed. Based on the findings, the advantages and disadvantages of each method over other techniques are discussed with respect to process parameters and material properties.

This work evaluates the potential of using a plasma spray process to introduce SiC into zirconia diboride ceramic coatings. Controlling the spraying of the ultra-refractory compound ZrB 2 is the first challenge as it represents the matrix in which SiC particles will reside. To that end, the experiments focus on spraying parameters that influence the plasma jet and the nature of the precursor feedstock. The results show that ZrB 2 coatings containing controlled amounts of SiC can be obtained through high-energy suspension plasma spraying. The ZrB 2 -SiC coatings will be evaluated in a high-temperature oxidative environment in future work.

Molybdenum disilicide (MoSi 2 ) has been applied as protective coating material on various substrates fabricated by different methods due to its good oxidation resistance at elevated temperature, relatively low density and coefficient of thermal expansion and high thermal conductivity. In this work, MoSi 2 coatings were fabricated by low pressure plasma spraying technology (LPPS). Their morphology, composition and microstructure characteristics were intensively investigated by SEM, XRD, EDS and TEM. The oxidation behaviors of MoSi 2 coatings were also explored. The results showed that the MoSi 2 coating was compact with porosity less than 5%. Its microstructure exhibited typical lamellar character. The MoSi 2 coating was made up of grains with irregular shapes and different sizes of 0.1-0.2 µm. It was mainly composed of tetragonal and hexagonal MoSi 2 phases. A small amount of tetragonal Mo 5 Si 3 phase formed and randomly distributed in the matrix of MoSi 2 . The MoSi 2 coating exhibited excellent oxidation-resistant behavior at 1773K, which resulted from the continuous dense glassy SiO 2 film formed on its surface.

Compositionally graded mullite/ZrO 2 coatings, have been tested as environmental barrier coatings (EBCs) for protection against water vapor corrosion of Si-based ceramic components intended for application in turbine engines. Four and five layered systems were engineered by plasma spraying over SiC substrates consisting of a Si bond coat layer, 2 or 3 mullite/ZrO 2 composite graded layers as middle layers and a nanostructured YSZ topcoat. These coatings were heat treated at 1300 °C in both stationary and thermal cycling conditions in a controlled water vapor environment. The effect of these ageing conditions on the coatings was comparatively investigated. Crystallization of the composite coatings and sintering of the YSZ topcoat was perceived. A reduction of SiO 2 content was detected in the composite layers before aging. The porosity of the coating did not change appreciably with the ageing tests and only the evolution of the pre-existing cracks and the growing of a thermally grown oxide layer can be highlighted as the major effect of the ageing tests.

The ongoing development of environmental barrier coatings (EBCs) offers the prospect to implement the full potential of silicon-based ceramics for high temperature structural applications. The current state-of-the-art EBC system comprises a Si bond coat, a mullite (3Al 2 O 3 ·2SiO 2 ) interlayer and a (1-x)BaO·xSrO·Al 2 O 3 ·2SiO 2 , 0 ≤ x ≤ 1 (BSAS) crack-resistant and water vapour attack resistant top coat. In this study, the influence of water vapour corrosion on the structural and mechanical properties of plasma-sprayed Si/Mullite/BSAS architectures was assessed by furnace thermal cycle testing (e.g., 100 cycles, 2h/cycle at 1300°C). Commercially available mullite and BSAS powders were used to produce crystalline coatings by air plasma spraying. Fully crystalline mullite and celsian BSAS coatings were engineered under controlled conditions on silicon coated, sintered α-SiC Hexoloy substrates. The overall performance at high-temperature of these functionally graded EBCs is discussed and correlated to their microstructural characteristics.

The dense refractory is applied for the high-temperature glass melting equipment. Furthermore, platinum or its alloy-clad refractory bricks are utilized to melt high quality glass in fields of optical and display glasses. From the viewpoint of the resource saving of rare metal, the decreasing of Pt-consumption is very serious problem for glass manufacturing. The platinum thermal spray coating is effective alternative technology to solve this problem for platinum cladding. A Pt-spray coated ceramics is difficult to get reliability due to the large difference of thermal expansion between the ceramic and the metal. In this study, we have investigated the bond strength of the platinum coat on the dense refractories which was textured by the mechanical process. As a result, the bond strength between the ceramic and the metal is 3-5 MPa. It is almost the same as the thermal spray ceramics coating on the metal. Furthermore, in case of the ceramics substrate that contains the glass phase, the bond strength between the ceramic and the metal increased to 14-17 MPa after 1773 K heat treatment.

Plasma sprayed ceramic coatings are widely used for thermal barrier coating applications. Commercially available mullite powder particles and a mixture of mechanically alloyed alumina and silica powder particles were used to deposit mullite ceramic coatings by plasma spraying. Microstructure and morphology of both powder particles as well as coatings were investigated by using scanning electron microscopy (SEM). Phase formation and degree of crystallization of coatings were analyzed and estimated by using X-ray diffraction technique. Differential thermal analysis (DTA) method was used to study the phase transformation of coatings. Results indicated that the porosity level in the coating deposited using mullite as initial powder particles was lower than that deposited using the mixed powder particles. The crystallization degree of the coating deposited using the mixed powder particles are higher than that deposited using mullite powder particles. DTA curves of coatings deposited using the mixed powders have showed some phase transformation due to the crystallization of the retained amorphous phases such as mullite and alumina in the coatings. The degree of crystallization of both as sprayed coatings was significantly increased after post deposition heat treatments.

Si-based ceramics (e.g., SiC and Si 3 N 4 ) are known as promising high-temperature structural materials in various components where metals/alloys reached their ultimate performances (e.g., advanced gas turbine engines and structural components of future hypersonic vehicles). To alleviate the thickness recess that Si-based ceramics undergo in a high-temperature environmental attack (e.g., H 2 O vapour), appropriate refractory oxides are engineered as environmental barrier coatings (EBCs). Presently, the state-of-the art EBCs comprise multilayers of silicon (Si) bond coat, mullite (Al 6 Si 2 O 13 ) intermediate layer and BaO-SrO-Al 2 O 3 -SiO 2 (BSAS) top coat. Evaluating and understanding their mechanical properties, such as, the elastic modulus (E) and the strain-stress relationship is essential for their practical application and reliable employment. It was investigated via depth-sensing indentation the role of high-temperature treatment (1300°C), performed in H 2 O vapour environment (for time intervals up to 500 h), on the mechanical behaviour of air plasma sprayed Si/mullite/BSAS layers deposited on SiC substrates. Laser-ultrasonics was employed to evaluate the E values of as-sprayed coatings and to validate the indentation results. The fully crystalline, crack-free and near crack-free as-sprayed EBCs were engineered under controlled deposition conditions. The (i) absence of phase transformation and (ii) stability of the low elastic modulus values (e.g., ~60-70 GPa) retained by the BSAS top layers even after harsh environmental exposures provides a plausible explanation for the almost crack-free coatings observed. The measured mechanical properties of the EBCs and their microstructural behaviour during the high-temperature exposure are discussed and correlated.

In this work the high temperature mechanical properties of UHTC coatings deposited by plasma spraying have been investigated; particularly the stress-strain relationship of ZrB2 based thick films has been evaluated by means of 4-point bending tests up to 1500 °C in air. Results show that at each investigated temperature (500, 1000, 1500 °C) Modulus of Rupture (MOR) values are higher than the ones obtained at room temperature; moreover at 1500°C the UHTC coatings exhibit a marked plastic behaviour, maintaining a flexural strength 25 % higher compared to RT tested samples. The coefficient of linear thermal expansion (CTE) has been evaluated up to 1500 °C: obtained data are of primary importance for substrate selection, interface design and to analyze the thermo-mechanical behaviour of coating-substrate coupled system. Finally SEM-EDS analyses have been carried out on as sprayed and tested materials in order to understand the mechanisms of reinforcement activated by high temperature exposure and to identify the microstructural modifications induced by the combination of mechanical loads and temperature in an oxidizing environment.

Large (3 x 3 x 0.05 m 3 ) refractory pieces (as the ones used for examples in smelters or incinerators) do not sustain regular glazing in a kiln, mostly due to high associated costs. Still, glass coatings could find use on such pieces due to their physical properties (durability, chemical inertia, tightness, etc.). Thermal spraying, using oxyacetylenic flame in particular, appears as a cost-effective solution permitting to circumvent the aforementioned disadvantages. This study aims at evaluating the quality of two types of coatings in terms of permeability. The first type considered coatings (resulting from a previous optimization of the spray operating parameters) sprayed directly on the substrates whereas the second one considered an additional brass underlayer manufactured by twin-wire electric arc spraying. The wettability of the glaze on the refractory substrate and on the brass underlayer was studied to comprehend the coating structural attributes (thickness, porosity, crazing, etc.) as well as their effects on the permeability. A specific measuring device was developed to assess permeability.

Mullite and mullite/ZrO 2 bi-layer systems are being considered as environment barrier coatings (EBCs) for protection of Si-based (Si 3 N 4 , SiC) substrates against water vapor corrosion for application in forthcoming turbine engines. An approach to reduce the thermal expansion mismatch between mullite and ZrO 2 layers in those coatings would be to tailor intermediate mullite/Y-ZrO 2 composite layers. The feasibility of these composite layers is studied in a comparative manner by plasma spraying both single mullite and bi-layer coatings of mullite and of mullite/ Y-ZrO 2 (75/25 vol %.) over Hexoloy SiC substrates. All feedstock materials are equally prepared using spray drying methods as the mix powders are not commercially available. Singular spraying conditions are used to assure enhanced crystallization of the mullite phase. Coatings are aged for 100 h at 1300 °C in a controlled water vapor environment. The effect of water corrosion on the exposed coatings is comparatively investigated, determining changes in crystalline phase by X-ray diffraction (XRD), the crystallization of amorphous phases is highlighted by the use of differential thermal analysis (DTA) tools and the microstructure of the polished coatings is analyzed by scanning electron microscopy (SEM).

Mullite (Al 6 Si 2 O 13 ) is the basis of efficient environmental barrier coatings (EBCs) for protecting Si-based ceramic matrix composites (CMCs) selected to replace specific hot-section metallic components in advanced gas turbines. Furthermore, YSZ-mullite multilayer architectures with compositional grading between the bond coat and YSZ top coat were envisioned as solutions to ease their coefficient of thermal expansion (CTE) mismatch induced stress. Consequently, a proper understanding of the mechanical properties such as the elastic modulus, hardness or plastic/elastic recovery work serve for an efficient design of such refractory oxide multilayers. In this work, three different mullite powder morphologies (fused and crushed, spray-dried and freeze-granulated) were employed. Using depth-sensing indentation with loads in the range 100 – 500 mN, the role of the microstructure and morphology of the powder feedstock on the mechanical behaviour of air plasma sprayed mullite bond coats deposited on SiC Hexoloy substrates was investigated. Fully crystalline as-sprayed mullite coatings were engineered under controlled deposition conditions. Mechanical properties were measured for the as-sprayed coatings as well as for coatings heat-treated at 1300°C, in water vapour environment, for periods up to 500 h. Both E and H values of the coatings are found to be highly dependent on the morphology of the starting powders.

Mullite based compositions have interest for thermal barrier coatings because they have thermal expansion coefficients close to those of silicon ceramic substrates. In this work, mullite-zirconia coatings are obtained by flame spraying and characterized based on microstructure, crystal phases, hardness, elastic modulus, and thermal conductivity. Crystallinity is improved by in-situ heating with a flame torch, which is also shown to increase hardness and elastic modulus. Thermal diffusivity measurements show that the thermal properties of mullite-zirconia coatings are relatively stable over a wide temperature range and adequate for many thermal barrier applications.

This study investigates the influence of powder morphology and spray processes on the microstructure, crystallinity, hardness, and elastic modulus of mullite coatings. Coatings produced from mullite powders and suspensions are deposited by plasma spraying while measuring in-flight particle temperature and velocity. Powder morphology and spraying conditions are correlated with measured coating properties, creating a process map for engineering mullite coatings for specific applications. It is shown that coating crystallinity, microstructure, and mechanical properties vary widely depending on powder morphology, processing, and in-flight particle characteristics.

In this study, two processing routes are used to produce mullite powders for thermal spraying and the influence of each method on particle morphology and microstructure is investigated. Different thermal treatments are performed to improve grain cohesion and powder flow and their effect on the crystal structure of the powder is assessed as well. The powders are plasma sprayed, in-flight characteristics are measured, and splats are collected and analyzed. A correlation among powder morphology, in-flight particle properties, and splat morphology is established to better understand the influence of powder processing route on coating formation.

In this study, plasma sprayed ceramic coatings with different amounts of SiC and MoSi 2 particles dispersed in a ZrB 2 matrix were produced and tested. The results show that MoSi 2 addition in ZrB 2 -SiC samples improves high-temperature oxidation resistance without affecting mechanical properties. Demonstrative components were manufactured and tested in simulated operating conditions by means of a plasma wind tunnel. Preliminary results indicate that thermal sprayed ceramics are well suited for use in space re-entry vehicles.

Zircon (ZrSiO 4 ) is a technologically important oxide ceramic material known for its high refractoriness and chemical stability. It shows excellent thermal shock resistance as a result of its very low thermal expansion coefficient and a low heat conductivity coefficient. Plasma spraying is a convenient method to produce large area coatings with high growth rates, necessary for many applications. ZrSiO 4 is among the least expensive spraying materials for refractory applications. In this study, a single-step process was used to prepare mullite/zirconia ceramic composites by plasma spraying zircon/alumina mixtures. Mixtures of ZrSiO 4 and Al 2 O 3 powders with Al 2 O 3 to SiO 2 molar ratios of 3:2 were milled for 2 h in a zirconia medium using a ball mill. The as–milled powders were dried in the furnace and sintered at 1300 and 1350 °C for 2h then crushed to a size less than 100 μm. The powders were sprayed by an atmospheric plasma spray gun (Metco 3MB) using C/C+SiC ceramic matrix composite substrates. Scanning electron microscopy (SEM) was used to analyze the microstructures of the powders and plasma coatings. The phase composition analysis of the powder showed the presence of alumina and zircon. After plasma coating, alumina, zircon, and zirconia phases were determined.

Mullite coatings (3Al 2 O 3 ·2SiO 2 ) were deposited by suspension thermal spraying of micron-sized (D50 = 1.8 µm) feedstock powders, using a high-velocity-oxy-fuel gun (HVOF) operated on propylene (DJ-2700) and hydrogen fuels (DJ-2600). The liquid carrier employed in this approach allows for controlled injection of much finer particles than in conventional thermal spraying, leading to coatings with low porosity and fine and homogeneous porosity distribution, making this process potentially suitable for creating thin layers with low gas permeability. In-flight particle states were measured for a number of spray conditions of varying fuel-to-oxygen ratios and standoff distances and related to the resulting microstructure, stoichiometry, phase composition (EDS, SEM, XRD) and hardness (VHN 300gf) of the coatings. In an attempt to retain the crystalline phase in the coatings, HVOF operating conditions were varied to limit in-flight particle melting. However, fully crystalline coatings were only obtained by gradually heating the coating during deposition to temperatures above 400°C.