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.

Molten calcium-magnesium-aluminum-silicate (CMAS) particles cause significant degradation of thermal barrier coatings (TBCs) in aero-engines. One way to protect TBCs against CMAS attack is through the application of a sacrificial topcoat. In this work, Al 2 O 3 coatings were deposited on top of EB-PVD 7wt% YSZ layers via suspension thermal spraying using an aqueous Al 2 O 3 suspension. Spray parameters were varied in order to obtain Al 2 O 3 layers with two different microstructures and porosity levels. The coating systems were evaluated by means of CMAS infiltration testing at 1250 °C. It was found that the porosity and morphology of Al 2 O 3 strongly influence CMAS infiltration and the formation of reaction products and that CMAS mitigation is a function of coating morphology and the speed at which Al 2 O 3 reacts with CMAS deposits.

Solution precursor plasma spraying (SPPS) was used to deposit barium magnesium tantalate thermal barrier coatings on titanium alloy substrates. The suspension was axially fed into an inductively-coupled RF plasma torch with a 25-mm converging nozzle. By selecting an atomization probe with a bimodal distribution of droplet size and adjusting the precursor feed rate and spraying distance, it was possible to tune the coating microstructure from dense splat-like layers to columns with intracolumnar porosity of 4.3% and intercolumnar porosity of 10%. The deposition rate achieved is suitable for commercial use.

This study compares the performance of an ordinary plasma spray gun with that of recently developed gun designed for spraying feedstock suspensions on inner diameter surfaces. To evaluate the guns, yttrium oxide was deposited on 304 stainless steel while varying supply pressure, spraying distance, and gun traverse speed. Different methods of delivering suspension spray material to the gun were also investigated. Although Y 2 O 3 inner-diameter coatings were successfully formed, hardness and cross-sectional porosity need improvement. Based on the findings, it may be necessary to increase substrate temperature, readjust spraying parameters, and optimize feedstock materials.

YSZ coatings were deposited by suspension plasma spraying and a parametric study was performed with different process parameters. Afterward, the porosity of the as-prepared coatings was investigated by SEM imaging and X-ray transmission and a multivariate analysis of the collected data was carried out. The results show that total porosity correlates negatively with suspension mass load, but positively with original powder size, spray step, substrate roughness, and spray distance, which was found to have the greatest impact. A porosity prediction model was also developed and its practical use is discussed.

In this work, CeO 2 -G d2 O 3 co-stabilized ZrO 2 (CGZ) thermal barrier coatings are deposited by solution precursor plasma spraying and the microstructure, phase stability, thermophysical properties, and thermal cycling behaviors of the resulting coatings are investigated and discussed in comparison to conventional 8YSZ coatings.

In this study, hydroxyapatite, titania, and HA-TiO 2 composite layers are deposited by suspension plasma spraying on titanium substrates and assessed by means of SEM and XRD analysis, Raman spectroscopy, and acoustic emission testing. The coatings exhibited dense microstructures with low porosity and good interfacial bond strength. The main phase in the HA and composite coatings was found to be similar to the peak of the feedstock powder. In the composite and titania coatings, besides rutile and anatase, a significant percentage of thermally stable Ti 3 O 5 was observed, which is favorable for photocatalytic performance.