Suspensions of cobalt spinel (Co3O4) powders were rf plasma sprayed to form electrocatalytically active anode layers. Stable cobalt oxide suspensions of low viscosity exceeding 50 wt% solid phase have been processed. A spheroidization study revealed the formation of large spherical powder particles (- 30 + 80 µm). Cobalt oxide coatings were produced by rf suspension plasma spraying. The porosity was controlled by optimizing spray distance and reactor pressure. The main disadvantage of the thermal plasma processing of cobalt spinel is that the decomposition of the spinel phase into CoO could not be prevented, not even with the application of an 80% oxygen plasma. However, with a relatively low power oxygen plasma post-treatment, the deposited CoO layers can be oxidized to Co3O4, greatly improving the electrochemical performance of the anode layers.

Ultra-fine hydroxyapatite powders were successfully synthesized using radio frequency (RF) suspension plasma spraying (SPS). This novel technique utilises the inherent characteristics of the RF plasma to axially feed and spheroidise a liquid suspension to produce spherical ultra-fine HA powders. This offers an alternative approach over conventional D.C. and flame spheroidising techniques which are better suited for solid feed stocks. Rietveld analysis was subsequently applied using Rietquan Quantitative Analysis software package to determine the amount of decomposed phases and amorphous content of the as-sprayed powder. This was also compared against quantitative XRD analysis employing internal and external standards. However, pure phases needed for calibration is scarce and amorphous calcium phosphate (ACP) is virtually impossible to isolate. In addition, the long and laborious task of obtaining calibration curves makes this technique unpopular. Nevertheless, conventional quantitative phase analysis (QPA) was carried out, using relative peak height ratios of HA and the phase involved, but the calculated decomposition only shows relative trends for a particular parameter variation. Determining the actual phase content is critical because of possible variations in biological responses when used as coatings and inserts in restorative orthopaedic implants. Varying tissue responses can arise from decomposed phases such as α and β-tricalcium phosphate (TCP) and tetra-calcium phosphate (TTCP) as well as ACP which generally have higher solubility as compared to crystalline. QPA via the Rietveld method provides a powerful tool that offers the user simultaneous quantitative phase determination of multiphase systems containing amorphous content. Unlike XRD QPA, the amorphous content could be indirectly calculated using crystalline alumina standard. XRD QPA results showed that decomposition generally rose with plate power without considering the amorphous content. With Rietveld QPA, the results showed an initial rise in decomposition before decreasing at higher plate powers. The amorphous phase content was calculated at different plate powers and concentration of suspension with the aid of alumina as an external standard. Results showed that the amorphous content increased substantially at higher powers. This study demonstrates the ability of Rietveld analysis to completely quantify all associated amorphous and crystalline phases within a multiphase system for any thermally treated material.

Ultra-fine hydroxyapatite (HA) powders were produced with radio frequency (RF) suspension plasma spraying (SPS). This novel technique utilizes the inherent properties of the RF plasma enabling axial feeding of the suspension into the plasma producing spherical ultra-fine HA powders. These powders were examined by XRD and Rietveld analysis using the Rietquan 2.3 Quantitative Analysis software package. The aim of the analysis was to determine the various amounts of decomposed phases and amorphous content after SPS of HA. Results showed that the amount of decomposed phases rose up to a plate power of 15 kW there after decreasing at higher plate powers. The amorphous phase however kept increasing with plate power reaching about 35 wt.% in the powders sprayed at 21 kW. These trends have led to the belief that the phase content and hence, the characteristics of the powders are controlled mainly by the competitive processes of decomposition and melting and evaporation within the plasma. The morphology of the powders was also observed through TEM and changes in molecular structure were investigated by FTIR. DSC was carried out to observe the crystallisation of amorphous calcium phosphate into HA.

Homogenous mixtures of Ce 0.8 Gd 0.2 O 1.9 (GDC) and La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3 (LSCF6428) nanopowders were successfully synthesized using radio frequency (RF) induction plasma by axial injection of a solution. Two kinds of powders with different mass ratio of GDC/LSCF, such as 3/7 and 6/4, were obtained. The crystallinity and morphological features of the powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The particles are almost globular in shape with a diameter lower than 100nm and the BET specific areas around 20m 2 /g. In addition, suspensions, made with the composite nanopowders and ethanol, were used to deposit some cathode coatings using suspension plasma spray method. Several initial results of the coatings are also presented. The coatings are homogeneous and porous with cauliflower structures.

Ceria (CeO2) based electrolytes have been considered for use in solid oxide fuel cells (SOFC) for more than 20 years. There are however some limitations to this usage that this study has tried to address, indeed the study objective has been that of synthesizing and thermal spraying thin layers (50 - 100 µm) of doped CeO2 by the technique of suspension plasma spraying, using radio frequency (RF) plasma technology. Various dopant combinations and concentrations have been selected for this work in order to increase the useful partial oxygen pressure range for satisfactory ionic conductivity development, thereby increasing the anionic conductivity and preventing CeO2 reduction in fuel cell service. Ceria possesses the fluorite crystal structure at low temperatures but does not have enough oxygen vacancies to be a good ionic conductor. In ceria the cerium have 4+ oxidation state within the fluorite structure, and by substituting a certain amount of Ce4+ ions by trivalent dopant ions, oxygen vacancies are induced into the structure. Recent studies have demonstrated that at low temperatures doped ceria seems to be a better electrolyte than doped zirconia. Also, it seems that dopants with ionic radii close to Ce4+ ions give rise to better ionic conductivities. The doped ceria conductivity increases with the dopant concentration because more oxygen vacancies are created, but at higher concentrations vacancy ordering occurs which results in decreased ionic conductivity.

Suspension Plasma Spraying (SPS) is a thermal spray process based on a suspension of fine (<10 μm) or even ultrafine (<100 nm) powders which is axially fed into the induction plasma through an atomization probe. The atomization of the suspension results in microdroplets (20 μm in size). They are flash dried in the plasma, melted and finally can impact a substrate to build a coating or be cooled down and collected as a spheroidized powder. The large industrial potential of this technology results first from the use of fine powder or even sol-gel which is one of the starting step for many ceramic processes, and second from the various side benefits of the liquid phase in the SPS. Indeed, the liquid phase can be simply a carrier for ultrafine powder, or a protection against oxidation in the case of metals, or a protection for health in the case of whiskers, for instance. It can also take a part in chemical reactions when the liquid phase is a solution of chloride, nitrates... or it can be an organic liquid for the synthesis of carbide, where CO is a strong reducer. Furthermore the liquid phase can also release some energy because of its combustion at the very end of the process. It can also change the local atmosphere surrounding the in flight droplets in the plasma where it is possible to use H 2 O 2 as a carrier in order to increase the oxygen partial pressure around sensitive to oxygen decomposition materials. The applications of SPS are in the powder synthesis (in R&D or production), in the spraying of metals, ceramics or composites directly synthesized, or in production of very reactive with air materials. Applications of SPS will be presented for hydroxyapatite (HA) and NiAlMo. Induction plasma SPS coatings and/or powders properties will be discussed as a function of the SPS process variables.

Perovskite-type LaMnO 3 powders and coatings have been prepared by a novel technique, the reactive suspension plasma spraying (SPS) using an inductively coupled plasma of about 40 kW plate power and an oxygen plasma sheath gas. Suitable precursor mixtures were found on the basis of solid state reactions, solubility and the phases obtained during the spray process. Best results were achieved by spraying a suspension of fine MnO 2 powder in a saturated ethanol solution of LaCl 3 with a 1:1 molar ratio of La and Mn. Low reactor pressure was helpful in order to diminish the amount of corrosive chlorine compounds in the reactor. As-sprayed coatings and collected powders showed perovskite contents of 70-90%. After a post-treatment with an 80% oxygen plasma an almost pure LaMnO 3 deposit was achieved in the center of the incident plasma jet.

This work is aimed at acquiring knowledge on successive deposition of alumina and nickel coatings on a metallic substrate using an RF plasma torch. The composition and morphology of various Ni/Al 2 O 3 steam reforming catalysts, prepared by plasma spraying of precursor nickel suspensions, are studied in this work. As Ni/γ-Al 2 O 3 is a well known reforming catalyst it was decided to study the deposition of a particular catalytic formulation on a metallic substrate. The purpose of this study was to find the means of building 2D monolithic catalysts by plasma deposition. Since 2D monolithic catalysts are non-porous, their specific areas available for hosting the catalytic reactions are low. Thus, It is essential to have very good dispersion of the active catalytic sites. Such dispersion is only possible only if the deposit can take place at the nanometer scale. The suspension plasma spraying is assessed for its ability to produce such structures. This method permits the formation of nanocrystalline structures within a few seconds. The main difficulty is the control of the various spraying parameters in order to obtain satisfactory deposition. The Ni/γ-Al 2 O 3 catalysts so obtained are characterized by scanning electron microscopy, field electron microscopy and X-Ray diffraction.

LaMnO 3 powders and coatings have been prepared by reactive suspension plasma spraying (SPS) of MnO 2 powders and LaCl 3 solutions. A 40 kW inductively coupled plasma with an oxygen plasma sheath gas has been used. Water and ethanol have been tested as the liquid phase in the SPS process. High perovskite content (70-90%) has been achieved for both powders and coatings when spraying a suspension of fine MnO 2 powder in a saturated ethanol solution of LaCl3 with a 1:1 molar ratio of La and Mn. Materials obtained by a 1100 °C oven treatment have been used as reference during the study. The reactor pressure was varied from 30 to 80 kPa. Low pressure was found to be necessary to suppress the formation of undesired phases in the powders and coatings obtained. A plasma post treatment of the coatings results in an increase of the perovskite content.

Fine (median size 6 μm and 0.3 μm) cobalt spinel (Co 3 O 4 ) powders were processed suspended in a suitable liquid phase. Suspensions exceeding 50 wt.% solid phase content were successfully injected into an inductively coupled plasma. Spheroidized powders with large particle size (up to 80 μm) were prepared, and cobalt oxide coatings were produced by this novel RF-SPS method. The microstructural features of the coatings can be controlled by parameter optimization similarly to plasma spraying of dry powders. Numerous variations of the physical and chemical conditions of the process were performed in an attempt to overcome the main disadvantage of the process, i.e. the decomposition of the spinel phase to CoO. So far, the spinel phase could be reestablished only by a post-treatment of the deposited coatings with atomic oxygen in the RF plasma.

Recently we successfully developed a new suspension plasma spray (SPS) system by using a twin-cathode plasma spray gun. The system consists of three plasma torches (central main torch with cathode nozzle and anode, and two sub-torches on the sides with anode nozzle and cathode). The system is characterized by using only argon (Ar) as the plasma gas and low input power, which makes it a gas and power consumption SPS system, compared to the other available SPS systems. This study will discuss the unique features of the axial injection spraying and its effect on the coating formation by the new system. The axial injection showed a significant potential during suspension feeding. It keeps the liquid suspension on the plasma core zone; therefore, the liquid encountered the highest heat and momentum transfers. This enhances the precious control of the coating microstructure through controlling of the droplet size and splat size. It was possible to control the droplet size and therefore the coating microstructure through axial injection and controlling the solid load content on the suspensions. Furthermore, gas atomization control and adjustment showed a strong potential on controlling the mist distribution on the plasma plume and coating formation during axial injection suspension plasma spraying.

DC plasma spraying with its products has gained a high technical importance. With the availability of technically reliable high-frequency plasma torches whose basic development can be traced back to about 40 years ago, some of the disadvantages of the DC spray method are no longer existing or can be avoided to a great extent. This paper describes the principle, construction, and function of high-frequency plasma torches in which the plasma is generated by induction and metallic electrodes are not required (as is the case with conventional DC plasma torches). Typical examples of HF plasma spray application are discussed. Paper includes a German-language abstract.

This paper investigates the problem of complete evaporation of zirconium oxide powders that are injected into a thermal RF plasma. Particle trajectories and evaporation are studied using optical emission spectroscopy and laser Doppler anemometry. Model calculations are compared with the results of process diagnostics. It is observed that axial emission profiles confirm the influence of the particle size on the evaporation behavior. Paper includes a German-language abstract.

In this work, optical emission spectroscopy is used to study plasma-liquid precursor interactions in a plasma spray process. A mapping of the plasma jet is performed with a bundle of seven optical fibers while injecting various liquid precursors. Two suspensions containing a titania (TiO 2 ) powder in different solvents and one solution containing titanium butoxide are analyzed. For each precursor, the evolution of both temperature and spectral line intensities along the plasma jet are observed. Comparing these results brings a new understanding of the precursor decomposition inside the plasma, while the noted contrasts between water and ethanol as solvent, and between the use of a powder and that of an alkoxide as a source of titanium, help to assess the effect of these parameters on the plasma spray process.

In this investigation, two complex perovskite powders, Ba(MgTa)O and Ta(AlMgT)O, are deposited by atmospheric plasma spraying and evaluated for use as thermal barrier layers. Process parameters are optimized to provide sufficient melting without causing the formation of secondary phases. Deposited coatings are assessed based on composition, morphology, porosity, and thermal cycling lifetime. It is shown that the nature of the starting powders has a significant effect on the lifetime and performance of perovskite-based thermal barrier coatings.

This paper reports on the synthesis of SiC material through the decomposition of silanes in a thermal high frequency (HF) plasma. The process is based on thermal plasma technology for chemical deposition from the gas phase and on suspension plasma spray technology, in which a liquid or suspension is injected axially and atomized in the plasma flame. The liquid silane then decomposes, and forms SiC with some gaseous by-products such as HCl. Various plasma parameters were varied, for example the plasma power level, the plasma gas composition, the chamber pressure, and the silane composition. The paper also presents first investigations into the elementary and phase composition as well as the morphology of the powders and coatings. Paper includes a German-language abstract.

This paper describes the properties and behaviors of alumina and titania coatings that have recently been produced using suspension spraying techniques. It examines coating microstructures and phase compositions are shows how they are influenced by different operating parameters and interactions. A selection of new experimental results obtained by the authors is also presented. In the case of Al 2 O 3 , the goal was to retain a high ratio of the thermodynamically stable α-phase. In the case of TiO 2 , the spraying process was optimized to preserve the anatase phase in order to obtain photocatalytically active layers.

Thermal plasma spraying is a suitable technique for hydroxyapatite [HA, Ca 10 (P0 4 ) 6 (OH) 2 ] coating preparation. Suspension Plasma Spraying (SPS) is a newly developed process based on a suspension of fine (<10 μm) or even ultrafine (<100 μm) powders, axially fed into the RF plasma through an atomization probe. The atomization of the suspension results in microdroplets (20 μm in size). They are flash dried, melted and finally impacted onto the substrate to solidify and build the coating. The aqueous suspension of HA is chemically synthesized. Our experiments included variations of the plasma gas composition (Ar/O 2 , Ar/H 2 ), the plasma deposition reactor pressure. Characterizations techniques (e.g. X-ray diffraction, scanning electron microscope and transmission electron microscope) were applied to resultant SPS HA coatings which possessed good crystallinity and about 3% weight α-TCP and lime. The texture examination has shown that preferential crystal orientation followed the (001) Miller's plane family. SPS by RF induction plasma has proved to be a reliable process for the production of thick (200 μm) HA coatings with high deposition rate (>150 μm/min).

This paper reviews various powder treatments and particle alteration processes and evaluates their effect on the microstructure and properties of thermal spray coatings. It discusses the benefits and drawbacks of thermal plasma treatments for powders, the use of self-propagating high-temperature synthesis (SHS), and different ways nanopowders are produced and sprayed. It covers several spraying methods and a wide range of materials, including ceramics, metals and alloys, cermets, and composites. It also covers mechanical alloying and powder milling processes and addresses the potential risks of inhaling nanopowders.

Hybrid aerosol deposition (HAD) is a new coating method to deposit homogeneous nano-structured ceramic coatings. An accurate evaluation of the fabricated coating properties is required. In this study, α-Al 2 O 3 fine powder was sprayed by HAD. The obtained coatings were dense and uniform with a nanocrystalline structure. An X-ray diffraction measurement revealed that the fabricated HAD Al 2 O 3 coatings mainly consisted of α-Al 2 O 3 phase. The hardness and Young's modulus of the HAD Al 2 O 3 coatings were evaluated by a micro-Vickers method and a nanoindentation method using the Weibull distribution. The hardness of HAD Al 2 O 3 coatings measured by micro-Vickers was ~1400 HV (~15 GPa). The variation of mechanical properties of HAD coatings measured by the nanoindentation method was extremely small compared to those of plasma-sprayed coatings, which also indicates that HAD coatings contain less pores and cracks than plasma-sprayed coatings.