This work focuses on the processing and deposit by suspension plasma spraying (SPS) of ZrO 2 -based ceramic materials for Thermal Barrier Coatings (TBC's) applications. The system of interest is ZrO 2 -16mol%Y 2 O 3 -16mol%Ta 2 O 5 (16YTZ). This ceramic has been reported to keep a non-transformable tetragonal phase (t'-phase), suitable to overcome the thermodynamic limits of the mostly used conventional 7-8wt.% yttria stabilized zirconia (YSZ). The research consists into evaluate the t'-phase stability and performance of the 16YTZ SPS coating. Synthesis of 16YTZ and, the evolution of the resulting microstructure in the dense ceramic and in the coating are a central part of the study. Sintering behavior in dense ceramics prepared from both precursor derived and milled powders is evaluated. Microstructural characterization by XRD, SEM and RAMAN spectroscopy of the as-deposited ceramic coating is presented and discussed.

In this study, the in-situ technique was used to observe crack formation and growth in multilayer suspension plasma spray (SPS) thermal barrier coatings (TBCs). Utilizing synchronized three-point bending (3PB) and scanning electron microscopy (SEM), coupled with digital image correlation (DIC), we provide real-time insights into strain field dynamics around cracking zones. Bending-driven failure was induced in both single and composite-layer SPS coatings to investigate the crack behavior in these columnar-structured multilayer TBCs. The real-time observations showed that columnar gaps can facilitate crack initiation and propagation from the coatings' free surface. The composite-layer SPS coating exhibits lower susceptibility to vertical cracking than the single-layer SPS coating, possibly due to the presence of a gadolinium zirconate (GZ) dense layer at the coating's free surface that enhances the bonding strength within the coating's columnar structure. The splat structure of the bond coat (BC) layer contributes to the crack path deflection, thereby potentially improving the SPS coating' fracture toughness by dissipating the energy required for crack propagation. Moreover, it was revealed that grit particles at the BC/substrate interface seem to promote crack branching near the interface, localized coating delamination, and serve as nucleation sites for crack development. Hence, optimizing the grit-blasting process of the substrate before BC layer deposition is crucial for minimizing the possibility of crack formation under operational conditions, contributing to enhanced durability and prolonged lifespan. This study underscores the critical role of in-situ observation in unravelling the complex failure mechanisms of multi-layered coatings, paving the way for the design of advanced coatings with enhanced structural complexity and improved performance for more extreme environments.

Suspension plasma spraying (SPS) is increasingly studied to produce finely structured coatings with dense and columnar microstructures for promising thermal barrier coatings especially in aerospace application. However, this process involves many parameters and complex phenomena with large spans of time and space scales in many physical mechanisms, like droplet break-up, liquid droplet evaporation, and various physical phenomena occurring within the suspension droplet, making it difficult to master. Especially, understanding the interactions of liquid drop submitted to plasma with the submicronic suspended particles is essential for material process optimization and control. For SPS understanding, a meaningful modelling of suspension treatment requires a prior analysis of these physical mechanisms and their characteristic times. This study details the different phenomena, their significance and characteristic timescales as well as the selection of the main governing forces acting between the different continuous and discrete phases (plasma, liquid, submicronic particles). We explore associated mechanisms: droplet breakup, carrier liquid evaporation, convective mixing and submicronic particle diffusion within the droplets. These mechanisms involve mass and heat transfer, that should condition particle agglomeration morphology before melting.

Due to their promising photocatalytic properties under visible light irradiation, thermally sprayed ZnO-TiO 2 coatings are of interest as substitute for TiO 2 for various industrial applications, like hydrogen production via water splitting or the reduction of organic pollutants in water. Suspension spraying is an effective method to produce coatings in the binary ZnO-TiO 2 system to form Zn 2 TiO 4 in-situ during the spraying process. Aqueous suspensions containing fine dispersed ZnO and TiO 2 particles are mixed at tailored composition and sprayed using the SHVOF and SPS spraying processes. Coatings with homogeneous distribution of elements and different surface structures and phase compositions are obtained. The phase composition is analyzed via XRD. UV-Vis spectroscopy measurements and photocatalytic tests of Rhodamin B degradation are performed. The potential to use appropriate binary suspension feedstock to produce ZnO-TiO 2 -Zn 2 TiO 4 coatings with different microstructures and photocatalytic properties is presented.

In the study, Axial Suspension Plasma Spray (SPS) was used to produce a range of columnar microstructures from Yttria Stabilized Zirconia (YSZ) suspension after an extensive experimental design. The optimized microstructure was applied to a multi-layer GZ/YSZ system, in which both layers were sprayed with SPS. In addition to SPS, a new GZ coating using Axial Solution Precursor Plasma Spray (SPPS) was developed and deposited on top of the SPS GZ coating. The durability in the furnace cycling test (FCT), as well as the consequences of CMAS infiltration into the columnar coatings was extensively studied on different microstructures. Preliminary CMAS test on the SPS coatings infiltrated them completely, leading to delamination. To minimize the detrimental effect of CMAS on the underlying SPS, the dense solution precursor GZ layer was aimed to act as a sealant to protect the underlying columnar SPS-GZ layer from molten CMAS infiltration.

Additive Manufacturing (AM) processes offer geometrical freedom to design complex shaped parts that cannot be manufactured with conventional processes. This leads to new applications including aerospace propulsion systems where the Ni-superalloy based material has to withstand high operating temperatures. In this contribution suspension plasma sprayed YSZ TBC coating was applied on the spike contour of an additively manufactured aerospike engine demonstrator. The engine was designed for a hydrogen peroxide / kerosene 6 kN thrust at 2.0 MPa chamber pressure and was manufactured from nickel-based superalloy Inconel 718 powder using the laser powder bed fusion process (LPBF). Due to the novelty of the application of suspension sprayed YSZ thermal protection coatings on additively manufactured Inconel 718 components, extensive tests were necessary to characterize the interaction between the coating and the component.

Additive Manufacturing (AM) processes offer geometrical freedom to design complex shaped parts that cannot be manufactured with conventional processes. This leads to new applications including aerospace propulsion systems where the Ni-superalloy based material has to withstand high operating temperatures. In this contribution, the influence of heat treatment and surface conditioning of the additively manufactured Inconel 718 substrates on the thermocycling performance of suspension sprayed YSZ coatings was investigated. The different surface conditions included as-built, sandblasted and milled substrate surfaces with and without heat treatment. YSZ coatings were applied using suspension plasma spraying (SPS) with commercial available suspensions. Thermal cycling tests (FCT) at 1100°C, 1300 °C, and 1500 °C were applied to coating systems until failure occurred. The microstructures of the samples were characterized before and after thermal cycling. The performance of the coatings was mainly influenced by the coating morphology and FCT test conditions and less by the state of the AM substrates. Columnar-like YSZ SPS sprayed coatings on AM Inconel 718 substrates seemed to be a promising candidate for rocket engine applications.

Deposition of protective dense environmental barrier layers is a promising solution to improve the reliability and environmental durability of the next-generation turbines and other industrial applications. In this context, spraying of fine particles could enhance the formation of fine dense coating microstructures with improved properties. In AIST we are focusing on the spraying of the fine particles via different spraying technologies including suspension plasma spraying, as well as deposition of the fine solid particles directly by aerosol deposition (AD) and plasma-assisted aerosol deposition (so-called Hybrid Aerosol Deposition; HAD. The HAD is a new coating window to spray the fine ceramic particles via the implementation of a low-power rf-plasma source to assist the aerosol deposition at room temperature. This study introduced the feasibility of utilization of HAD as an outstanding technology for deposition of dense ceramic coatings on different substrate materials and 3D deposition capability. Highly dense and well-adhered Al 2 O 3 coatings without obvious observable cracks and bulk-like properties were successfully fabricated on different substrate materials of SUS 304, Aluminium, Al 2 O 3 and glass, via HAD of fine particles. The substrate material and its hardness significantly influenced the first deposition step, which determined the coating adhesion and properties. Furthermore, homogeneously uniform, dense, and crack-free coating with a strong adhesion has been fabricated successfully on cylindrical substrates with 6.3 mm diameter. During HAD spraying the plasma activated the surface of the particles without reaching to the molten state, then the activated particles impact and stuck with the substrate by room temperature impact consolidation mechanism. Therefore, the fabricated coatings had the same crystal structure as the starting feedstock powder, and the activated surface act as glue and improved the deposition efficiency and 3D capabilities. Herein, the deposition phenomena of HAD makes it as a promising candidate technology for development of environmental and sealing layers of highly dense microstructure, with the targeted crystalline phase structure, without stoichiometric composition nor phase transformation and improved deposition efficiency on multi-shape components in different fields such as environmental, thermal barrier coatings (TBCs), environmental barrier coatings (EBCs) and gas turbine applications.

The porous architecture of coatings has a significant influence on the coating performances and thus should be properly designed for the intended applications. For simulating the coating properties, it is necessary to determine the numerical representation of the coating microstructure. In this study, YSZ coatings were manufactured by suspension plasma spray (SPS). Afterwards, the porous architecture of as-prepared coatings was investigated by the combination of three techniques, imaging analysis, Ultra Small Angle X-ray Scattering (USAXS), and X-ray transmission. A microstructural model for reconstructing the porous architecture of the SPS coating was subsequently computed according to the collected experimental results. Finally, the coating thermal properties were simulated based on the model and were compared with the experimental results.

Thermal spray is a versatile process that produces high-quality coatings possessing diverse properties such as superhydrophobicity, wear resistance, corrosion resistance, dielectric properties etc. Conventionally, powder feedstock is used in thermal spray, and this process is commercialised in numerous industrial processes. However, liquid feedstock based thermal spray is still in its development phases, due to limited information available on process parameters. Various parameters such as plasma/fuel gas, plasma current, feedrate, feeding angle, type of feedstock (suspension or solution precursor), feedstock concentration, feedstock viscosity, solvent, etc. significantly influence the thermal and kinetic energy exchange between plasma/flame and feedstock material. Suspension plasma spray (SPS) and suspension high velocity oxy-fuel spray (SHVOF), once optimised, can give rise to coatings with multiscale features. An in-depth understanding of the complex interaction between feedstock solution/suspension chemical-physical properties and plasma/flame jet characteristics is essential to understand its specific impact on coating properties and their application. This paper presents comparisons between two different TiO2 coatings, deposited by SPS and S-HVOF, and obtained by varying some of the fundamental spray deposition parameters. The surface morphology and cross-sections of the as-deposited coatings were compared through SEM/EDX. Further, surface wetting properties were analysed through measuring the static and dynamic contact angles.

The focus of this study is the formation of a solid solution and metallic nickel in the cobalt-nickel mixed oxide coatings during suspension plasma spray (SPS) deposition. The (Co,Ni)O solid solution is a potential material for inert anode applications in aluminum production. SPS coatings and in-flight collected particles are studied to gain further insight into the melting and mixing phenomena of the NiO and CoO powders as well as phase formation in the deposited coatings. Moreover, the role of suspension feedstock particle sizes on the microstructure of coatings is discussed. SEM, EDS and X-ray diffraction studies helped better understanding the formation of different crystalline phases within the as-sprayed coatings. It was found that the formation of metallic nickel is possible in the coatings. The results support the importance of substrate temperature on the formation of metallic Ni, so that keeping the substrate at low temperature results in an increase of the Ni content in the coatings. In this study, possible causes for the formation of metallic Ni during spraying are discussed.

The aim of this work is to better understand the build-up of thermal barrier coatings (TBC) on microtextured substrates, particularly the influence of geometry on the behavior of plasma jets in substrate boundary layers. Coatings produced by suspension plasma spraying served as an experimental reference for numerical analysis, which involved advanced turbulent flow and volumetric heat source modeling along with the use of commercial fluid flow software. Geometric and numerical models were used to simulate the generation of plasma inside the torch and the resulting plasma flow with its highly nonlinear thermophysical characteristics. This work opens the possibility of predicting feedstock particle movement and deposition, which is essential in understanding coating build-up mechanisms in general and the flow of fine particles on substrate surfaces in particular.

In suspension spraying, the two most frequently used solvents are water and ethanol. In this study, we test a potential alternative, a high-molecular weight solvent. Two organic solvents are compared: ethanol (serving as a benchmark, suspension formulated at 10 wt.% solid load) and di-propylene glycol methyl ether (two suspensions at 10 wt.% and 20 wt.%). Submicron alpha-alumina powder is used as a model material to formulate the suspensions. It is shown that ethanol- and ether-based-feedstock coatings are fully comparable in terms of their microstructure, porosity content, surface roughness, and hardness. However, the ether-based coatings exhibit slightly higher levels of α-Al2O3 phase than their ethanol-based counterpart (17 wt.% vs. 6 wt.%). The use of 20 wt.% solid load in the ether solvent leads to a twofold increase in the deposition rate while, as opposed to ethanol, successfully retaining a dense microstructure. Ether also costs less than ethanol and is safer to handle.

This study investigates the effect of composition on the antibacterial and antiviral properties of hydroxyapatite/titania composite coatings deposited by suspension plasma spraying. Hydroxyapatite is a bioceramic material used as a plasma-sprayed coating to promote osseointegration of femoral stems. TiO2 has promising photocatalytic activity and good efficiency in destroying bacteria, viral species, and parasites. Prior to coating, substrates were grit blasted, ultrasonically cleaned, and heated to enhance adhesion strength. The microstructure of the resulting coatings was then characterized using XRD and Raman spectroscopy. Test results indicated that SPS transformed Ti2O3 into TiO2 with mixed phases. Ti4O7 and Ti3O5 phases were also identified, which show photocatalytic activity due to oxygen vacancies. Antibacterial and antiviral tests were conducted as well.

This study investigates the co-deposition of aluminum and chromium oxides from solution precursor feedstocks with the aim of maximizing the α-alumina content. A hybrid water-stabilized plasma torch was used to spray the feedstock materials and the deposition principles were studied. The chemical composition of the deposits corresponded to the formulation of the feedstocks, indicating a uniform deposition of both materials. It was found that α-phase content can be increased in the coatings by increasing the Cr-forming precursor in the solution.

The agglomeration process plays an important role in suspension plasma spraying (SPS), affecting the state of particles prior to impact and consequently the mechanical properties of the coated substrate. This paper presents the results of an investigation on the agglomeration of submicron YSZ particles sprayed from a water suspension. The shape and surface morphology of transient and final agglomerate structures was studied by injecting YSZ suspensions with a nebulizer into an inductively coupled plasma torch. It was found that particle agglomeration occurs in successive stages identified as cup or doughnut shaped agglomerates, polycrystalline particles, and amorphous or partially molten particles.

In this work, numerical models are developed and used to simulate magneto-hydrodynamic fields inside a dc plasma torch during suspension plasma spraying and their influence on arc attachment. A Reynolds stress model is used to simulate turbulent plasma flow and a discrete phase model simulates the effects of arc fluctuation on suspension droplets in the plasma jet. Submicron yttria-stabilized zirconia particles, suspended in ethanol, are modeled as multicomponent droplets and the KHRT model is used to simulate their breakup. The results show that particles are significantly affected by plasma arc fluctuations and that fine particles near the centerline of the torch are hotter and experience better penetration into the plasma jet.

This study compares the performance of different measurement methods for characterizing particles during thermal spraying. The accuracy of double-point and single-point measurements is assessed in the context of HVOF and suspension plasma spraying (SPS) where in-flight particle temperature and velocity are recorded for different powders and suspensions. The results are evaluated by analyzing splats and correlating their size and shape to in-flight particle temperature measurements. It is shown that particle diagnostic systems based on single-point measurements are well suited for SPS and HVOF processes.

This study investigates the effect of suspension plasma spraying (SPS) parameters on inner diameter coatings produced from yttria suspensions, one in water and one in ethanol. Thermal spray trials were conducted at different spray distances, transverse speeds, and spray angles, with and without a water shroud. The coatings obtained were then examined in order to assess the influence of each parameter and the effect of water cooling on substrate temperature, porosity, vertical cracking, nodule formation, surface roughness, and deposition rate. Key findings and correlations are presented in the paper along with recommended practices and potential improvement pathways.

Strontium zirconate is a candidate material for thermal barrier coatings due to its high melting point, good sintering resistance, and high TCE. One drawback, however, is a phase transition that occurs below 1200 °C , although rare-earth element doping offers a way to suppress it. In this study, SrZrO 3 doped with two rare earth oxides, ytterbia and gadolinia, is deposited by solution precursor plasma spraying and the layers obtained are evaluated before and after heat treatment. The coatings are characterized by two phases, SrZrO 3 and t-ZrO 2 , with interpass boundary structure, nano and microscale porosity, and through-thickness vertical cracks. XRD analysis after heat treatment at 1400 °C for 360 h shows that the two phases are very stable due to the doping of rare-earth elements, which is also shown to reduce thermal conductivity in the as-sprayed deposits by nearly 35%.